Food Control 31 (2013) 359e365. Contents lists available at SciVerse ScienceDirect. Food Control. journal homepage:
|
|
- Melanie Allison
- 5 years ago
- Views:
Transcription
1 Food Control 31 (13) 359e365 Contents lists available at SciVerse ScienceDirect Food Control journal homepage: Highly sensitive and simultaneous determination of sixteen sulphonamide antibiotics, four acetyled metabolites and trimethoprim in meat by rapid resolution liquid chromatography-tandem mass spectrometry Hui Li a,b, Hanwen Sun a, *, Jingxuan Zhang b, Kun Pang b a College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science of Hebei Province, Wusi East Road 188, Baoding , China b Hebei Institute of Food Quality Supervision Inspection and Research, Shijiazhuang , China article info abstract Article history: Received 14 June 12 Received in revised form 17 September 12 Accepted 18 September 12 Keywords: Sulphonamides Acetyled metabolites Trimethoprim Solid phase extraction RRLC-MS/MS Meat A novel multiresidue analysis method is developed for highly sensitive and simultaneous determination of 16 sulphonamides (SAs), 4 acetyled metabolites, and trimethoprim in pork and mutton by rapid resolution liquid chromatography-tandem mass spectrometry (RRLC-MS/MS). The sample was extracted with acetonitrile under ultrasonication incubation, followed by solid phase extraction (SPE). The calibration curves showed good linearity with correlation coefficient (r) more than The limit of quantification (LOQ) was 0.35e1.0 mg/kg, which can ensure to detect studied drugs at the maximum residue level (MRL) of 10 mg/kg. The mean recoveries at addition level of 1.0, 5.0 and 50 mg/kg were in the range of 68.3e104% with the relative standard deviation (RSD) of 3.5e9.2%. The intra-day precision (as RSD) for six determinations at 50 mg/kg spiked level within a day was in the range of 4.2e8.9%. The method is sensitive, accurate, convenient and rapid, and can be used for the qualitatively and quantitatively determination of multiresidue of the studied drugs in meat. Ó 12 Elsevier Ltd. All rights reserved. 1. Introduction The residues of sulphonamides (SAs) in foods of animal origin are a major concern because they are harmful to the consumer s health, and could induce pathogens to develop resistance. SAs can be acetylated at the N 4 -position. N 4 -acetyl metabolite of SAs in foodproducing animals may cause the renal toxicity as a result of precipitation in the kidney (Vree & Hekster, 1985), and may affect their excretion rates due to higher plasma protein binding than the parent compound (Vree, Hekster, Nouws, & Dorrestein, 1987). Trimethoprim is another antibiotic agent, which is often coadministered with sulfamethoxazole to enhance treatment against a variety of bacterial infections. In humans and animals, it can cause changes in the bone marrow and significant effects on some organ weights. To ensure food safety for consumers, the European Community, the U.S. Food and Drug Administration (FDA), and China Agriculture Department have laid down the maximum residue level (MRL) of 100 mg/kg for SAs in foodstuffs of animal origin and 50 mg/ kg for trimethoprim in muscle, fat/skin, liver and kidney tissues of pigs (China Agriculture Ministry, 02; European Union Regulation, * Corresponding author. Tel.: þ ; fax: þ address: hanwen@hbu.edu.cn (H. Sun). 10; Food and Drug Regulation, 1991, pp. 1478e1480). Korea set an MRL of 100 mg/kg as sum of the 14 SAs in meat and milk (Korea Food Code, 08). The Japan s Positive List System presents an MRL of 50 mg/kg for sulfaquinoxaline, mg/kg for sulfamerazine, 40 mg/kg for sulfadimethoxypyrimidine, and 10 mg/kg for sulfamethazine. For other SAs the MRL takes 10 mg/kg (Ministry of Health, Labour and Welfare of Japan, 06). In order to better assess the occurrence of SAs in food, their metabolites should also be considered. These early conclusions evidenced the need for analytical methods capable to simultaneously determine parent compound as well as their metabolites at the low concentrations normally present in food. Therefore, it is urgently in need of developing rapid and effective method for the simultaneous determination of SAs residues and their metabolites in meats. High-performance liquid chromatography (HPLC) as separation and analytical technology has been used widely to detect veterinary residues in food. A series of analytical methods were reported for the determination of SAs residues in food (See Table 1). Analytical detection limits of HPLC-UV method are generally limited by significant signal interference associated with UV spectral overlaps with other food constituents. Recently, several HPLC- UV/DAD methods combined with effective extraction and cleanup were reported for the determination of residual SAs in food (Huang et al., 12; Kowalski, Plenis, Oledzka, & Konieczna, 11; Shi et al., /$ e see front matter Ó 12 Elsevier Ltd. All rights reserved.
2 360 Table 1 References for the determination of SAs, acetyled metabolites and trimethoprim in food. Analyte Matrix Extraction Cleanup Final method LOD/recovery/RSD Ref. Ref. no. 6 SAs c Shrimp, fish Ultrasonication, 1% acetic acid Molecularly imprinted LCeUV 8.4e10.9 mg/kg, 85.5e106.1%, 1.2e7.0% Shi et al., 11 1 polymers 7 SAs Milk Cloud point extraction, n-butyl LCeUV 2.23e9.79 mg/l, 67.0e105.7%, 93e8.31% Zhang et al., 11 2 alcohol 7 SAs Poultry tissue Ultrasonication, acetonitrile C18 cartridges MECC a 1.3e7.8 mg/kg, >77.2%, 9.5%, 11.2% Kowalski et al., SAs Milk, chicken Acetonitrileewater Micro-solid phase extraction LC 4.52e15.63 mg/kg, 43.11e83.81% Huang et al., 12 4 muscle 2 SAs, etc. Porcine tissues TwogramsC18, EDTA-Na 2 eoxalic Matrix solid-phase LCeDAD LOQ: 7e34 mg/kg, 80.6e99.2%, <6.1%, Yu et al., 12 5 acid dispersion 6 SAs Cattle meats Acetonitrile LCeFLD 8e15 mg/kg, 44.67e81%, <6% Mor, Kocasari, Ozdemir, 6 & Oz, 12 6 SAs Milk Water, dichloromethane PCSFC b ems 41e181 mg/kg Dost, Jones, & Davidson, SAs Milk, egg Distilled water Solid-phase extraction LCeMS 1e10 mg/kg, 76e112%, <13% Cavaliere et al., SAs Raw meat, infant Accelerated hot water extraction LCeMS/MS 2.6 mg/kg, 70e101% Gentili et al., 04 9 foods 16 SAs Poultry/meat Acetonitrile LCeMS/MS 1. 0e12.0 mg/kg, 75.4e97.3%, Pang et al., e14$09% 12 SAs Pork meat Pressurized liquid extraction, water Oasis HLB cartridge CEeMS/MS <12.5 mg/kg, 76e98%, <14%) Font et al., SAs Pork Ultrasonication, water Solid-phase microextraction LCeMS mg/kg below 15% Lu et al., SAs, etc. Fish tissue Ultrasonication, MeOH:CAN: formic LCeMS/MS 5.65e24.0 mg/kg, <% Dasenaki & Thomaidis, 13 acid 10 5 SAs Honey Acetate buffereoctanol:pentanol Hollow fiber renewal liquid LCeMS/MS 5.1e27.4 mg/kg, 80.9e103.1%, <15% Bedendo et al., membrane 18 SAs Muscles, livers, Pressurized liquid extraction with Hydrophilicelipophilic LC, LCeMS/MS 3 mg/kg, 71.1e118.3%, <13% Yu et al., kidneys acetonitrile balance cartridge 14 SAs Marine products Ultrasonication, acetonitrile C18 powder LCePDA, LCeMS/MS 3e6 mg/kg, 51.8e89.7%, 5.6e8.6% Won et al., SAs Grass, carp tissues C18-bonded silica Matrix solid-phase LCeMS/MS 0.75e3.0 mg/kg, 69.0e96.3%, 13.2% Lu et al., dispersion 6 SAs Milk, milk powder Hydrochloric acid (ph 2) 15% NaCl C18-stir bar sorptive LCeMS/MS 2.7e31.5 mg/kg, 68e115% Yu & Hu, extraction SMM, d AcSMM, e Eggs Ultrasonication saturated ammonium HPLC-DAD,30 mg/kg, >91%,within 4%. Kishida, SDM, f AcSDM g sulphate SMM, AcSMM Chicken plasma, Ultrasonication, ethanol HPLC-DAD <30 mg/kg, >90% within 4%. Kishida & Furusawa, SDM, AcSDM tissues, eggs 05 SMM, AcSMM, Milk Ultrasonication, ethanoleacetic HPLC-DAD LOQ: < mg/l, >81%, within 5% Kishida & Furusawa, 21 SDM, AcSDM Acid (97:3, v/v) 04 SDM, AcSDM Chicken meat Ultrasonication % (w/v) perchloric HPLC-DAD LOQ: 0.1 mg/kg, 84%, 6% Furusawa, acid SDA, h TMP i Broiler tissues Ethyl acetate or dichloromethane Hexaneechloroform HPLC 15e100 mg/kg SDA, e mg/kg TMP Dagorn & Delmas, in an acidic buffer SDA, TMP Swine tissues 3 ml of 0.1 M acetic acid in water SCX column HPLC-DAD LCeMS/MS 15 mg/kg SDA, mg/kg TMP De Baere et al., H. Li et al. / Food Control 31 (13) 359e365 a MECC d micellar electrokinetic capillary chromatograp. b PCSFC d packed column supercritical fluid chromatography. c SAs d sulfonamides. d SMM d sulfamonomethoxine. e AcSMM d N4-acetyl sulfamonomethoxine. f SDM d sulfadimethoxine. g AcSDM d N4-acetyl sulfadimethoxine. h SDA d sulfadiazine. i TMP d trimethoprim.
3 H. Li et al. / Food Control 31 (13) 359e ; Yu, Mun, & Hu, 12; Zhang, Duan, & Wang, 11). HPLC coupled to mass spectrometry (MS) or tandem MS (MS/MS) is the most effective method because of their high sensitivities and accuracy for compounds confirmation. A numbers of LC-MS or LC- MS/MS methods have been used for the determination of SAs residues in food (Bedendo, Jardim, & Carasek, 10; Cavaliere, Curini, Corcia, Nazzari, & Samperi, 03; Dasenaki & Thomaidis, 10; Gentili et al., 04; Lu, Chen, & Lee, 07; Lu, Shen, Dai, Zhang, & Wang, 11; Pang et al., 05; Won et al., 11; Yu & Hu, 12; Yu et al., 11 in Table 1). Since the concentration of SAs drugs commonly found in food samples is extremely low, pretreatment is necessary for their sensitive detection and quantification. Extraction and cleanup are the most challenging parts for SAs analysis in foods, which are often the critical steps in deciding the levels of detection limits of the overall methods. A series of LC-MS or LC-MS/MS methods combined with deferent cleanup technique for the determination of SAs residues in food were reported. C 18 SPE cartridges were used for cleanup of 7 SAs in poultry tissue (Kowalski et al., 11), 14 SAs in marine products (Won et al., 11), and 6 SAs in milk and milk powder (Yu & Hu, 12). Oasis HLB cartridges with reversed-phase sorbents were used for cleanup of 12 SAs in pork meat (Font, Juan-Garcia, & Pico, 07). For SAs, acetyled metabolites and trimethoprim with strong polarity and ionogenous character, positive SPE column or ion exchange SPE column should be selected for cleanup. From 11 year to date, several higher throughout methods were developed for simultaneous determination of 5e18 SAs residues in different food matrix by LC-MS or LC-MS/MS (see De Baere et al., 00; Lu et al., 11; Won et al., 11; Yu & Hu, 12; Yu et al., 11 in Table 1). However, up to date, only a few LC methods were reported for the analysis of the metabolites of SAs in food. For the analysis of acetyled metabolites, such as N 4 -acetyl sulfamonomethoxine, N 4 -acetyl sulfadimethoxine in eggs (Kishida, 07), chicken tissues (Kishida & Furusawa, 05), and milk (Kishida & Furusawa, 04) aswellasn 4 -acetyl sulfadimethoxine in chicken meat (Furusawa, 07), the sensitivity was not high enough for trace residue analysis. Thermal pinch analyses were performed by using reverse phase-hplc, with LOD ranging from to 50 mg/kg (Dagorn & Delmas, 1994), which are not low enough to fulfil the EU requirements for residue analysis. An HPLCeUV detection method for quantitative determination of sulfadiazine and trimethoprim in swine tissues was developed with LOQ of 50 and mg/kg, respectively (De Baere et al., 00). Table 1 shows that some methods reported can be used for the determination of SAs residues in food at the MRL level (100 mg/ kg). Among them, LCeMS/MS method combined with matrix solid-phase dispersion (Lu et al., 11) and pressurized liquid extraction (Yu et al., 11) have high sensitivity, which can be used for determination of SAs residues in food at the MRL level (10 mg/ kg). Recently, an isotope dilution-lc-ms/ms method for the determination of six SAs, two metabolites and trimethoprim in wastewater (Le-Minh, Stuetz, & Khan, 12). Development of selective multiresidue method for high throughput simultaneous determination of SAs, acetyled metabolites and trimethoprim in food is required. This paper develops a high sensitive approach enabling simple and rapid multiresidue analysis of 21 analytes including sixteen SAs, four acetyled metabolites, and trimethoprim. The analytes were extracted with ethyl acetate from pork and mutton samples under ultrasonic vibration, and then the extract was cleaned up through SPE, followed by LC-MS/MS detection. The evaluated LOD and LOQ values ranged from 0.1 to 0.3 mg/kg, and from 0.35 to 1.0 mg/kg in pork and mutton, respectively. These values are far lower than the MRLs set by several control authorities. 2. Materials and methods 2.1. Chemicals, reagents and solutions Seventeen SAs (purity: 99%) were purchased from DR.HIELSCHER Co. (Germany), and N 4 -acetylsulfamethazine, N 4 - acetylsulfamerazine, N 4 -acetylsulfamerazine, and N 4 -acetylsulfadiazine (purity: 98%) were purchased from Toronto Research Chemicals Inc. (Canada). Methanol, acetonitrile, ethyl acetate, and formic acid (chromatographic grade) were obtained from Alfa Aesar (Tianjin, China). Other reagents are of analytical grade. Mixed stock solution of twenty one analytes at concentrations of 1 mg/l of each compound was prepared in methanol. The stock and working standard solutions were stored at 4 C in a refrigerator. Water used in solution preparation was purified on an MYQ-sub-boiling distilling water purification system (Changsha, China) Instrument An Agilent series rapid resolution liquid chromatography-triple quadrupole tandem mass spectrometry system (Agilent, USA) was used. Data acquisition and evaluation were carried out using ChemStation software (Agilent Technologies). The following instruments were used for sample preparation and cleanup: An SPE-30 Four Chunnel Full Aut SPE instrument (Tianjin BNAJE Science and Technique Co. Ltd.), Ultrasonic cleaner (Ultrasonic Instrument Co., Kunshan, China), RE3000A rotary vacuum evaporator (Shanghai Yarong biochemical instrument factory, China), CT15RT high-speed refrigerated centrifuge (Shanghai Tianmei Com. China), T Basic homogenizer (IKACom. Germany), and Nitrogen concentrator (Organomation Com. USA). An XGJ-30 highly pure water machine (Yongcheng purification Science & Technology Co. Ltd., Beijing, China) was used Extraction and cleanup Five gram of homogenized pork and mutton samples was weighed into a 50 ml conical flask, and ml of ethyl acetate was added. The sample was homogenized with a vortex stirrer for 30 s, and then extracted by ultrasonic vibration for 10 min, followed by centrifuging at 15,000 rpm for 10 min. The supernatant was taken, and the residue was extracted again with 5 ml acetone. The supernatant obtained two times was moved in a separatory funnel with 10 g of anhydrous sodium sulphate, and filtered. Antifoaming agent isopropanol of 1 ml was added in the collected filtrate, and then concentrated in vacuo to dryness at 30 C, the residue was dissolved with 2 ml methanol, and the solution was used for cleanup further. After the AccuBONDII SCX cartridge (100 mg, 3 ml, Agilent, USA) was preconditioned by adding 5 ml of acetic acid (4%, v/v) in acetonitrile, the sample solution was passed through the cartridge at a flow rate of 1 ml/min. After sample loading, the column was washed sequentially with 5 ml methanol and 5 ml acetonitrile. The analytes were eluted with 8 ml ammonia solution/acetonitrile (1:19, v/v); the eluate was collected in a 10 ml glass flask, and then evaporated to dryness under a stream of nitrogen at 30 C. The residue was dissolved in 1 ml mobile phase (0.1% formic acid 10 mm ammonium formateeacetonitrile). The final solution was used for LC determination CLeMS/MS conditions Agilent-Plus C 18 analytical column (100 mm 2.1 mm, 1.8 mm) was used for the separation of the 21 analytes. The flow rate of the mobile phase was set at 0. ml/min. A ml volume of sample solution was injected in the column. The mobile phase consisted of
4 362 H. Li et al. / Food Control 31 (13) 359e mm ammonium formatee0.1% formic acid (A) and acetonitrile (B). Gradient elution program was as follows: B increased linearly from 5% to 35% for 0 / 7 min, retained at 35% for 5 min, decreased from 35 % to 5% for 12 / 12.1 min, then retained at 5% for 12.1 / 16 min. Matrix-matched calibration curve was measured on RRLC-MS/MS within the concentration range of 1e0 mg/kg. The electrospray ionization source and multiple reactions monitoring (MRM) were applied where the parent ions and fragment ions were monitored at Q1 and Q3, respectively. Positive ionization mode was employed. The optimization of MS parameters (precursor ions, collision energy, collision cell exit potential, and quantification and confirmation transitions) was performed by flow injection analysis for each compound dissolved in mobile phase. Table 2 shows the values of the parameters optimized and the MRM transitions selected Validation method Quantitative analysis was performed in multi-selected reaction monitoring (MRM). Identification of the 21 analytes was accomplished by comparing the retention time (within 2%) and the ratio (within %) of the two selected precursor ion-production ion transitions with those of standards. The selectivity of the method was evaluated in triplicate using pork and mutton matrices. Linearity was studied from matrix-matched calibration, spiking blank extracts at 1, 5, 50, 100, and 0 mg/kg. Calibration curve was performed in triplicate using a least-square linear regression analysis at different concentrations. The regression equations were obtained using the 5- points concentration of standard as abscissa and area of chromatogram peak as vertical coordinate. The method limit of detection (LOD) was determined as the sample concentration that produces a peak with a height three times the level of the baseline noise, and the limit of quantification (LOQ) was calculated that produced a peak with 10 times the signal-to-noise ratio. Recovery and precision were assessed by performing test on spiked samples at three concentration levels 1.0, 5.0 and 50 mg/kg. The intra-day precision (as RSD) was investigated for six determinations at 50 mg/kg spiked level within aday. 3. Results and discussion 3.1. Choice of extraction conditions SAs are sparingly soluble in water, but easily dissolved in dilute acid, dilute base, and organic solvent. So methanol, acetonitrile, ethyl acetate, and dichloromethane were selected as possible extraction solvents. The extraction recoveries of the analytes in spiked pork samples were investigated. The result showed that Table 2 MS parameters for the detection of 21 compounds. No. Compound Molecular weight Retention time (min) Quantification transition (m/z) Confirmation transition (m/z) 1 Sulacetanide / / /92 2 Sulfadiazine /156 1/156 1/108 3 Sulfapyriline /156 0/156 0/92 4 Sulfamerazine / / /172 5 Sulfamethoxazole /156 4/156 4/108 6 Sulfameter / / /108 7 Sulfisoxazole / / /113 8 Trimethoprim / / /123 9 Sulfamethoxypyridazine / / / Sulfamonomethoxine / / / Sulfadimethoxypyrimidine / / / Sulfamethazine / / / Sulfadimethoxine / / / Sulfadoxine / / / N 4 -acetylsulfadiazine / / / Sulfaphenazole / / / N 4 -acetylsulfamethoxazole / / / Sulfaquinoxaline / / / Sulfamethylthiazole / / /108 N 4 -acetylsulfamerazine / / / N 4 -acetylsulfamethazine /5 321/5 321/186 Fragment (V) Collision energy (ev)
5 H. Li et al. / Food Control 31 (13) 359e acetonitrile or ethyl acetate as an extraction solvent gave higher recoveries than the other solvents for the extraction of the 16 SAs, four acetyled metabolites, and trimethoprim in spiked pork samples. After the extraction with ethyl acetate, the extract was extracted again with acetone, the recovery increased further, preponderating over 78% for all 21 analytes, because acetone could destroy the interaction between protein and amido in SAs molecules. So ethyl acetate and acetone were selected for the extraction of the 21 analytes from the matrix Optimization of cleanup The cleanup procedure of the analyte extracts in blank pork sample spiked with 5 mg/kg for each analyte was investigated by using different SPE columns (AccuBONDII ODS-C 18, Oasis HLB and AccuBONDII SCX). The SPE columns were preconditioned by adding 5 ml of acetic acid (4%, v/v) in acetonitrile. After sample loading, the column was washed sequentially with 5 ml methanol and 5 ml acetonitrile, and the analytes were eluted with 3 ml ammonia solution/acetonitrile (1:19, v/v). Both C 18 column and HLB column with reversed-phase sorbents allowed to achieving the recoveries from 65% to 113%. SCX column with strong cation exchange sorbents can extract positively charged basic compounds. It allowed to achieving the recoveries from 81% to 109%, less interferent peaks and shortest time requirements, so that SCX column was selected in later work. acetonitrile. The result showed that the last mobile phase presented better separation effect than the others. Formic acid and ammonium formate could make the peak shapes to be sharp and symmetrical. It was observed that the recoveries of the analytes decreased notably when the ph of the mobile phase went down below 3.0. The mobile phase used in this work was a mixture solution of 10 mm ammonium formatee0.1% formic acid (A)e acetonitrile (B). The ph of the mobile phase was 3.21 and 3.72 for AeB of 95: 5 (v/v) and 65:35 (v/v), respectively. The satisfactory recoveries of the 21 analytes were achieved. The amount of acetonitrile in the mobile phase greatly affected the retentions of the 21 analytes, and acetonitrile at low concentration gave good separation of the SAs with lower molecular weight, but higher concentrations were required for the separation of the SAs with higher molecular weight. The result showed that 35% of acetonitrile in the mobile phase could not be exceeded. Good separation of the 21 SAs was obtained by using the gradient elution procedure given in Table 1 and flow rate of 0. ml/min. The total ion chromatograms of 21 standards (each ng/ml) and spiked blank matrix (0.5 mg/kg for each analyte) were observed, as shown in Fig. 1. Fig. 1 shows that the retention time of each analyte in blank matrix and standard solution is basically consistent, showing without matrix interference. Twenty one analytes including the isomers (sulfameter, sulfamethoxypyridazine and 3.3. Optimization of mobile phase The effect of different mobile phases on the separation of the 21 analytes was investigated, such as 10 mm ammonium acetatee methanol, 10 mm ammonium acetateeacetonitrile, 0.1% formic acidemethanol, and 0.1% formic acide10 mm ammonium formatee Fig. 1. TIC chromatogram of 21 analytes in standard solution of each ng/ml (above) and spiked blankpork matrixwitheach0.5 mg/kg (below).1. Sulacetanide, 2. Sulfadiazine, 3. Sulfapyriline, 4. Sulfamerazine, 5. Sulfamethoxazole, 6. Sulfameter, 7. Sulfisoxazole, 8. Trimethoprim, 9. Sulfamethoxypyridazine, 10. Sulfamonomethoxine, 11. Sulfadimethoxypyrimidine, 12. Sulfamethazine, 13. Sulfadimethoxine, 14. Sulfadoxine, 15. N 4 -acetylsulfadiazine, 16. Sulfaphenazole, 17. N 4 -acetylsulfamethoxazole, 18. Sulfaquinoxaline, 19. Sulfamethylthiazole,. N 4 -acetylsulfamerazine, 21. N 4 -acetylsulfamethazine. Fig. 2. Production process of parent ion and some fragment ions of sulfonamides, N 4 -acetyled metabolites and trimethoprim.
6 364 H. Li et al. / Food Control 31 (13) 359e365 Table 3 Analytical performance of the method. Analyte Linearity range (mg/kg) Regression equation r LOD (mg/kg) LOQ (mg/kg) Sulacetanide 1 0 y ¼ x þ Sulfapyriline 1 0 y ¼ x Sulfadiazine 1 0 y ¼ x þ Sulfamethoxazole 1 0 y ¼ xþ Sulfamerazine 1 0 y ¼ x Sulfisoxazole 1 0 y ¼ x Sulfamethylthiazole 1 0 y ¼ x þ Sulfamethazine 1 0 y ¼ x Sulfamonomethoxine 1 0 y ¼ x þ Sulfamethoxypyridazine 1 0 y ¼ x þ Sulfameter 1 0 y ¼ x Trimethoprim 1 0 y ¼ x Sulfaquinoxaline 1 0 y ¼ x Sulfadimethoxypyrimidine 1 0 y ¼ x Sulfadimethoxine 1 0 y ¼ x þ Sulfadoxine 1 0 y ¼ x þ Sulfaphenazole 1 0 y ¼ x N 4 -acetylsulfadiazine 1 0 y ¼ x N 4 -acetylsulfamethoxazole 1 0 y ¼ x N 4 -acetylsulfamerazine 1 0 y ¼ x N 4 -acetylsulfamethazine 1 0 y ¼ x þ sulfamonomethoxine; sulfadimethoxypyrimidine, sulfadimethoxine and sulfadoxine) could be baseline separated within 12 min Mass spectrum resolution Based on chemical ionization character of sulphonamides with a secondary amino group or tertiary amino groups, ESI source and positive ionization mode were selected. MRM was applied where the parent ions and fragment ions were monitored at Q1 and Q3, respectively. The parent ion [M þ H] þ with higher abundant was obtained, The selected product ions constituted the ion pair for qualitative analysis, and the ion pair with parent ions for quantification (see Table 2). Production process of the parent ions and some fragment ions is shown in Fig. 2. Typical fragment ions [MeRNH 2 ] þ (m/z ¼ 156)for most SAs were observed, except for sulfaphenazole{[c 9 N 3 H 10 ] þ (m/z 160)}. Typical fragment ions of N 4 -acetylsulfadiazine and N 4 -acetylsulfamethoxazole were [MeRNH 2 ] þ (m/z 198), and typical fragment ions of N 4 -acetylsulfamerazine and N 4 -acetyl-sulfamethazine were [M þ HeC 8 NOH 8 ] þ (m/z 172) and [MeNH 2 eso 2 ] þ (m/z 5), respectively. Typical fragment ion of trimethoprim was [Mþ2He C 2 O 2 H 6 ] þ (m/z 230) Validation study We have mainly considered the items related to the estimation of the well known performance characteristics parameters. The following criteria were considered: selectivity, sensitivity (limits of detection and quantification), and linearity of the response function, precision, and recovery. The selectivity of the method was evaluated in triplicate using pork and mutton matrices; no interference peaks were found at the retention times of the analytes studied. Linearity was studied from matrix-matched calibration, spiking blank extracts at the five concentration levels. The regression equations were obtained using the 5-points concentration of Table 4 Determination of each analyte in pork and mutton spiked at three concentration levels. Analyte Added 1.0 mg/kg Added 5.0 mg/kg Added 50.0 mg/kg Recovery (%) RSD a (%) Recovery (%) RSD a (%) Recovery (%) RSD a (%) Intra-day RSD a (%) Sulacetanide Sulfapyriline Sulfadiazine Sulfamethoxazole Sulfamerazine Sulfisoxazole Sulfamethylthiazole Sulfamethazine Sulfamonomethoxine Sulfamethoxypyridazine Sulfameter Trimethoprim Sulfaquinoxaline Sulfadimethoxypyrimidine Sulfadimethoxine Sulfadoxine Sulfaphenazole N 4 -acetylsulfadiazine N 4 -acetylsulfamethoxazole N 4 -acetylsulfamerazine N 4 -acetylsulfamethazine a n ¼ 6.
7 H. Li et al. / Food Control 31 (13) 359e standard. Table 3 shows that the good linearity was obtained for the 21 analytes with the correlation coefficient of > The LODs and LOQs of this method were listed Table 3. The LODs of 21 analytes were in the range of 0.1e0.3 mg/kg, and the LOQs were in the range from 0.35 to 1.0 mg/kg. The LOD values of the method are better than those reported by literature in Table 1, and can ensure to detect studied drugs at the MRL of 10 mg/kg. The whole procedure was applied to 10 blank samples of pork to verify the specificity of the method showing that no interference was detected around the retention times of the analytes in any of the samples analysed. Recovery and precision (Table 4) were assessed by performing test on spiked samples at three concentration levels 1.0, 5.0 and 50 mg/kg. The recovery of 21 analytes was obtained to be 68.3e104%, with RSD (n ¼ 6) of 3.5e9.2%. The intraday precision (as RSD) for six determinations at 50 mg/kg spiked level within a day was in range of 4.2e8.9% Application In this study, the applicability of this extraction method to real samples including pork and mutton was investigated at the optimized extraction conditions. No target analyte was detected in pork and mutton samples taken from different local markets. Hence, the spiked pork and mutton samples were studied. None of the commercial samples analysed yielded a positive result for the analytes. The contents of 16 SAs, 4 acetyled metabolites, and trimethoprim in pork and mutton were all below the LOQ of the proposed method. 4. Conclusion The LOD values of the proposed method are lower than those reported in the literature, it can ensure to detect studied drugs at the MRL of 10 mg/kg. The proposed methodology is relatively simple, sensitive and robust, and capable to simultaneously determine multiresidue parent compounds and their metabolites at the low concentrations normally present in food. Acknowledgements This work was supported by the Natural Science Found of Hebei Province (B ) and the Sustentation Plan of Science and Technology of Hebei Province of China (No D). References Bedendo, G. C., Jardim, I. C. S. F., & Carasek, E. (10). A simple hollow fiber renewal liquid membrane extraction method for analysis of sulfonamides in honey samples with determination by liquid chromatographyetandem mass spectrometry. Journal of Chromatography A, 1217, 6449e6454. Cavaliere, C., Curini, R., Corcia, A. d., Nazzari, M., & Samperi, R. (03). A simple and sensitive liquid chromatography mass spectrometry confirmatory method for analyzing sulfonamide antibacterials in milk and egg. Journal of Agricultureand Food Chemistry, 51, 558e566. China Agriculture Ministry. (02). Establishment of maximum residue levels of veterinary medical products in foodstuffs of animal origin. PR China, Regulation No. 235, 02. Dagorn, M., & Delmas, J. M. (1994). Methods for assay of trimethoprim and sulphadiazine in broiler tissues using liquid chromatography. Analytica Chimica Acta, 285, 353e358. Dasenaki, M. E., & Thomaidis, N. S. (10). Multi-residue determination of seventeen sulfonamides and five tetracyclines in fish tissue using a multi-stage LCeESIeMS/MS approach based on advanced mass spectrometric techniques. Analytica Chimica Acta, 672, 93e102. De Baere, S., Baert, K., Croubels, S., De Busser, J., De Wasch, K., & De Backer, P. (00). Determination and quantification of sulfadiazine and trimethoprim in swine tissues using liquid chromatography with ultraviolet and mass spectrometric detection. Analyst, 1, 409e415. Dost, K. D., Jones, C., & Davidson, G. (00). Determination of sulfonamides by packed column supercritical fluid chromatography with atmospheric pressure chemical ionisation mass spectrometric detection. Analyst, 1, 1243e1247. European Union Regulation. (10). Council regulation (EEC) No. 37/10. Font, G., Juan-Garcia, A., & Pico, Y. (07). Pressurized liquid extraction combined with capillary electrophoresisemass spectrometry as an improved methodology for the determination of sulfonamide residues in meat. Journal of Chromatography A, 1159, 233e241. Food and Drug Regulation. (1991). Canada gazette part II. Table 3, Division 15, Part B. 1. Furusawa, N. (07). Organic solvents-free technique for determining sulfadimethoxine and its metabolites in chicken meat. Journal of Chromatography A, 1172, 92e95. Gentili, A., Perret, D., Marchese, S., Sergi, M., Olmi, C., & Curini, R. (04). Accelerated solvent extraction and confirmatory analysis of sulfonamide residues in raw meat and infant foods by liquid chromatography electrospray tandem mass spectrometry. Journal of Agriculture and Food Chemistry, 52, 4614e4624. Huang, J., Liu, J., Zhang, C., Wei, J., Mei, L., Yu, S., et al. (12). Determination of sulfonamides in food samples by membrane-protected micro-solid phase extraction coupled with high performance liquid chromatography. Journal of Chromatography A, 1219, 66e74. Kishida, K. (07). Restricted-access media liquid chromatography for determination of sulfamonomethoxine, sulfadimethoxine, and their N 4 -acetyl metabolites in eggs. Food Chemistry, 101, 281e285. Kishida, K., & Furusawa, N. (04). Application of shielded column liquid chromatography for determination of sulfamonomethoxine, sulfadimethoxine, and their N 4 -acetyl metabolites in milk. Journal of Chromatography A, 1028,175e177. Kishida, K., & Furusawa, N. (05). Simultaneous determination of sulfamonomethoxine, sulfadimethoxine, and their hydroxy/n4-acetyl metabolites with gradient liquid chromatography in chicken plasma, tissues, and eggs. Talanta, 67, 54e58. Korea Food Code. (08). Korea food & drug administration. Kowalski, P., Plenis, A., Oledzka, I., & Konieczna, L. (11). Optimization and validation of the micellar electrokinetic capillary chromatographic method for simultaneous determination of sulfonamides and amphenicol-type drugs in poultry tissue. Journal of Pharmaceutical and Biomedical Analysis, 54, 160e167. Le-Minh, N., Stuetz, R. M., & Khan, S. J. (12). Determination of six sulfonamide antibiotics, two metabolites and trimethoprim in wastewater by isotope dilution liquid chromatography/tandem mass spectrometry. Talanta, 89, 407e416. Lu, K. H., Chen, C. Y., & Lee, M. R. (07). Trace determination of sulfonamides residues in meat with a combination of solid-phase microextraction and liquid chromatography-mass spectrometry. Talanta, 72, 1082e1087. Lu, Y., Shen, Q., Dai, Z., Zhang, H., & Wang, H. (11). Development of an on-line matrix solid-phase dispersion/fast liquid chromatography/tandem mass spectrometry system for the rapid and simultaneous determination of 13 sulfonamides in grass carp tissues. Journal of Chromatography A, 1218, 929e937. Ministry of Health, Labour and Welfare of Japan. (06). Introduction of the positive list system for agricultural chemical residues in foods. Department of Food Safety, Ministry of Health, Labour and Welfare, May, english/topics/foodsafety/positivelist060228/introduction.html. Mor, F., Kocasari, F. S., Ozdemir, G., & Oz, B. (12). Determination of sulphonamide residues in cattle meats by the Charm-II system and validation with high performance liquid chromatography with fluorescence detection. Food Chemistry, 134, 1645e1649. Pang, G. F., Cao, Y. Z., Zhang, J. J., Jia, G. Q., Fan, C. L., Li, X. M., et al. (05). Simultaneous determination of 16 SAs in poultry meat by high-performance liquid chromatography-tandem mass spectrometry. Chinese Journal of Analytical Chemistry, 33, 12e16. Shi, X., Meng, Y., Liua, J., Sun, A., Li, D., Yao, C., et al. (11). Group-selective molecularly imprinted polymer solid-phase extraction for the simultaneous determination of six sulfonamides in aquaculture products. Journal of Chromatography B, 879, 1071e1076. Vree, T. B., & Hekster, Y. A. (1985). Renal excretion of sulfonamides. Antibiotics & Chemotherapy, 35, 66e1. Vree, T. B., Hekster, Y. A., Nouws, J. F. M., & Dorrestein, G. M. (1987). Pharmacokinetics of sulfonamides in animals. Antibiotics and Chemotherapy, 37, 131e177. Won, S. Y., Lee, C. H., Chang, H. S., Kim, S. O., Lee, S. H., & Kim, D. S. (11). Monitoring of 14 sulfonamide antibiotic residues in marine products using HPLC-PDA and LC-MS/MS. Food Control, 22, 1101e1107. Yu, C., & Hu, B. (12). C18-coated stir bar sorptive extraction combined with high performance liquid chromatographyeelectrospray tandem mass spectrometry for the analysis of sulfonamides in milk and milk powder. Talanta, 90, 77e84. Yu, H., Mun, H., & Hu, Y. (12). Determination of fluoroquinolones, sulfonamides, and tetracyclines multiresidues simultaneously in porcine tissue by MSPD and HPLCeDAD. Journal of Pharmaceutical Analysis, 2, 76e81. Yu, H., Tao, Y., Chen, D., Wang, Y., Huang, L., Peng, D., et al. (11). Development of a high performance liquid chromatography method and a liquid chromatographyetandem mass spectrometry method with the pressurized liquid extraction for the quantification and confirmation of sulfonamides in the foods of animal origin. Journal of Chromatography B, 879, 2653e2662. Zhang, W. J., Duan, C. M., & Wang, M. L. (11). Analysis of seven sulphonamides in milk by cloud point extraction and high performance liquid chromatography. Food Chemistry, 126, 779e785.
Macrolides in Honey Using Agilent Bond Elut Plexa SPE, Poroshell 120, and LC/MS/MS
Macrolides in Honey Using Agilent Bond Elut Plexa SPE, Poroshell 120, and LC/MS/MS Application Note Food Testing and Agriculture Author Chen-Hao (Andy) Zhai and Rong-jie Fu Agilent Technologies (Shanghai)
More informationAminoglycosides in Milk Using Agilent Bond Elut Plexa SPE, Agilent Poroshell 120, and LC/Tandem MS
Aminoglycosides in Milk Using Agilent Bond Elut Plexa SPE, Agilent Poroshell 120, and LC/Tandem MS Application ote Food Testing & Agriculture Author Andy Zhai Agilent Technologies, Inc. Shanghai Co. Ltd.
More informationRapid Screening and Confirmation of Melamine Residues in Milk and Its Products by Liquid Chromatography Tandem Mass Spectrometry
Rapid Screening and Confirmation of Melamine Residues in Milk and Its Products by Liquid Chromatography Tandem Mass Spectrometry Application Note Food Authors Jianqiu Mi, Zhengxiang Zhang, Zhixu Zhang,
More informationDevelopment of monolith-based stir bar sorptive extraction and liquid. chromatography tandem mass spectrometry method for sensitive
Analytical and Bioanalytical Chemistry Electronic Supplementary Material Development of monolith-based stir bar sorptive extraction and liquid chromatography tandem mass spectrometry method for sensitive
More information16 Malachite green 17 Leucomalachite green
16 17 Leucomalachite green hydrochloride Leucomalachite green N N N + Cl - N N-[4-[[4-(dimethylamino)-phenyl] phenylmethylene]-2,5-cyclohexadien-1-ylidene ]-N-methylmethanaminium chloride C 23 H 25 ClN
More informationDetermination of Hormones in Drinking Water by LC/MS/MS Using an Agilent InfinityLab Poroshell HPH Column (EPA 539)
Determination of ormones in Drinking Water by LC/MS/MS Using an Agilent InfinityLab Poroshell P Column (EPA 539) Application Note Environmental Authors Rong-jie Fu and Chen-ao (Andy) Zhai Agilent Technologies
More informationAvailable online Journal of Chemical and Pharmaceutical Research, 2012, 4(6): Research Article
Available online www.jocpr.com Journal of Chemical and Pharmaceutical Research, 2012, 4(6):3275-3279 Research Article ISSN : 0975-7384 CODEN(USA) : JCPRC5 Development and validation of a matrix solid-phase
More informationApplication Note. Gas Chromatography/Mass Spectrometry/Food Safety. Abstract. Authors
Trace-Level Analysis of Melamine in Milk Products on Agilent 789A/5975C GC/MSD Using a ew Agilent J&W DB-5ms Ultra Inert Column and SampliQ SCX Cartridges Application ote Gas Chromatography/Mass Spectrometry/Food
More informationUltrafast Analysis of Buprenorphine and Norbuprenorphine in Urine Using the Agilent RapidFire High-Throughput Mass Spectrometry System
Ultrafast Analysis of Buprenorphine and Norbuprenorphine in Urine Using the Agilent RapidFire High-Throughput Mass Spectrometry System Application Note Authors Mohamed Youssef and Vaughn P. Miller Agilent
More informationLC/MS/MS qua ntitation of β-estradiol 17-acetate using an Agilent 6460 Triple Quadrupole LC/MS working in ESI negative ion mode
LC/MS/MS qua ntitation of β-estradiol 17-acetate using an Agilent 6460 Triple Quadrupole LC/MS working in ESI negative ion mode Application Note Authors Siji Joseph Agilent Technologies India Pvt. Ltd.
More informationLC-MS/MS Method for the Determination of Diclofenac in Human Plasma
LC-MS/MS Method for the Determination of Diclofenac in Human Plasma J. Jones, Thermo Fisher Scientific, Runcorn, Cheshire, UK Application Note 20569 Key Words SPE, SOLA, Accucore RP-MS, diclofenac, Core
More informationScreening and confirmation of sulfonamides, trimethoprim and dapsone in animal tissues using HPLC-DAD
Austrian Agency for Health and Food Safety (AGES) Screening and confirmation of sulfonamides, trimethoprim and dapsone in animal tissues using HPLC-DAD Prepared by Checked by QM-Controller Approved by
More informationQuantitative analysis of mitragynine in human urine by high performance liquid chromatography-tandem mass spectrometry
Quantitative analysis of mitragynine in human urine by high performance liquid chromatography-tandem mass spectrometry Shijun Lua, Buu N. Trana, Jamie L. Nelsenb, Kenneth M. Aldousa. Journal of Chromatography
More informationAnalysis of Illegal Dyes in Food Matrices using Automated Online Sample Preparation with LC/MS
Application Note: 56 Analysis of Illegal Dyes in Food Matrices using Automated Online Sample Preparation with LC/MS Yang Shi, Catherine Lafontaine, Matthew Berube, John Fink, François Espourteille Thermo
More informationAnalytical determination of testosterone in human serum using an Agilent Ultivo Triple Quadrupole LC/MS
Application Note Clinical Research Analytical determination of testosterone in human serum using an Agilent Ultivo Triple Quadrupole LC/MS Authors Yanan Yang 1, Victor Mandragon 2, and Peter Stone 1 1
More informationFumonisin. Fumonisin B 1 Fumonisin B 2. Fumonisin B 3. CAS No.:
Fumonisin Fumonisin B 1 Fumonisin B 2 Fumonisin B 3 Fumonisin B 1 Fumonisin B 2 H H H H H H H H NH 2 H H NH 2 H C 34 H 59 N 15 MW: 721.8 CAS No.: 116355-83-0 H C 34 H 59 N 14 MW: 705.8 CAS No.: 116355-84-1
More informationFast and Reliable Method for the Analysis of Methylmalonic Acid from Human Plasma
Fast and Reliable Method for the Analysis of Methylmalonic Acid from Human Plasma Jon Bardsley 1, James Goldberg 2 1 Thermo Fisher Scientific, Runcorn, UK; 2 Thermo Fisher Scientific, West Palm Beach,
More informationPlasma Metanephrines and 3-Methoxytyramine by LC/MS/MS Using Agilent SimpliQ WCX SPE, 1290 Infi nity LC, and 6460 Triple Quadrupole LC/MS
Plasma Metanephrines and 3-Methoxytyramine by LC/MS/MS Using Agilent SimpliQ WCX SPE, 129 Infi nity LC, and 646 Triple Quadrupole LC/MS Application Note Clinical Research Authors Linda Côté and Christophe
More informationDetermination of underivatized aflatoxins B2, B1, G2, and G1 in ground hazelnuts by immunoaffinity solid-phase extraction with HPLC-FLD detection
APPLICATION NOTE 72686 Determination of underivatized aflatoxins,, G2, and in ground hazelnuts by immunoaffinity solid-phase extraction with HPLC-FLD detection Authors Sylvia Grosse, Mauro De Pra, Frank
More informationToxicity, Teratogenic and Estrogenic Effects of Bisphenol A and its Alternative. Replacements Bisphenol S, Bisphenol F and Bisphenol AF in Zebrafish.
1 Supporting Information 2 3 Toxicity, Teratogenic and Estrogenic Effects of Bisphenol A and its Alternative Replacements Bisphenol S, Bisphenol F and Bisphenol AF in Zebrafish. 4 5 John Moreman, Okhyun
More informationDetermination of Beta-Blockers in Urine Using Supercritical Fluid Chromatography and Mass Spectrometry
Determination of Beta-Blockers in Urine Using Supercritical Fluid Chromatography and Mass Spectrometry Application Note Doping Control Authors Prof. Maria Kristina Parr Freie Universität Berlin Institute
More informationExtraction of Methylmalonic Acid from Serum Using ISOLUTE. SAX Prior to LC-MS/MS Analysis
Application Note AN89.V.1 Extraction of Methylmalonic Acid from Serum Using ISOLUTE SAX Page 1 Extraction of Methylmalonic Acid from Serum Using ISOLUTE SAX Prior to LC-MS/MS Analysis Sample Preparation
More informationHPLC Winter Webinars Part 2: Sample Preparation for HPLC
HPLC Winter Webinars Part 2: Sample Preparation for HPLC Jon Bardsley, Application Chemist Thermo Fisher Scientific, Runcorn/UK The world leader in serving science What am I Going to Talk About? What do
More informationQuantification of growth promoters olaquindox and carbadox in animal feedstuff with the Agilent 1260 Infinity Binary LC system with UV detection
Quantification of growth promoters olaquindox and carbadox in animal feedstuff with the Agilent 126 Infinity Binary LC system with UV detection Application Note Food Author Srividya Kailasam Agilent Technologies,
More informationExtraction of Aflatoxins and Ochratoxin from Dried Chili Using ISOLUTE. Myco Prior to LC-MS/MS Analysis
Application Note AN785 Extraction of Aflatoxins and chratoxin From Dried Chili Using ISLUTE Myco prior to LC-MS/MS Analysis Page Extraction of Aflatoxins and chratoxin from Dried Chili Using ISLUTE Myco
More informationAgilent s New Weak Anion Exchange (WAX) Solid Phase Extraction Cartridges: SampliQ WAX
Agilent s New Weak Anion Exchange (WAX) Solid Phase Extraction Cartridges: SampliQ WAX Technical Note Agilent s SampliQ WAX provides Applications for strongly acidic, acidic and neutral compounds Excellent
More informationRapid method development to study plasma stability of diverse pharmaceutical compounds using Rapid Resolution LC and triple quadrupole MS
Rapid method development to study plasma stability of diverse pharmaceutical compounds using Rapid Resolution LC and triple quadrupole MS Application Note Drug Discovery Authors Srividya Kailasam Agilent
More informationSolid Phase Extraction Method Development Tips and Tricks
Solid Phase Extraction Method Development Tips and Tricks Carol Haney Ball, Ph.D. Application Scientist Agilent Technologies, Inc. February 3, 2009 Sources of Error Generated and Time Spent During a Typical
More informationIdentification and Quantitation of Pesticides in Chamomile and Ginger Extracts Using an Agilent 6460 Triple Quadrupole LC/MS system with Triggered MRM
Identification and Quantitation of Pesticides in Chamomile and Ginger Extracts Using an Agilent 646 Triple Quadrupole LC/MS system with Triggered MRM Application Note Authors Thomas Glauner Agilent Technologies,
More informationGB Translated English of Chinese Standard: GB NATIONAL STANDARD OF THE
Translated English of Chinese Standard: GB5009.28-2016 www.chinesestandard.net Buy True-PDF Auto-delivery. Sales@ChineseStandard.net NATIONAL STANDARD OF THE GB PEOPLE S REPUBLIC OF CHINA GB 5009.28-2016
More informationLC/MS/MS Analysis of Pesticide Residues in Apples Using Agilent Chem Elut Cartridges
LC/MS/MS Analysis of Pesticide Residues in Apples Using Agilent Chem Elut Cartridges Application ote Food Testing & Agriculture Author Andy Zhai Agilent Technologies Shanghai Co. Ltd. Abstract This application
More informationQuantitative Analysis of EtG and EtS in Urine Using FASt ETG and LC-MS/MS
Quantitative Analysis of EtG and EtS in Urine Using FASt ETG and LC-MS/MS UCT Part Numbers: CSFASETG203 - CLEAN SCREEN FASt ETG, 200mg / 3mL tube SLETG100ID21-3UM - Selectra ETG HPLC column, 100 x 2.1
More informationSupporting Information
Supporting Information Discovery of Hydrocarbon-Stapled Short α-helical Peptides as Promising Middle East Respiratory Syndrome Coronavirus (MERS-CoV) Fusion Inhibitors Chao Wang,, Shuai Xia,, Peiyu Zhang,
More informationAgilent 6460 Triple Quadrupole LC/MS System with an Agilent 1290 Infinity LC For Multi-Plant Growth Regulator Analysis in Grapes
Agilent 6460 Triple Quadrupole LC/MS System with an Agilent 1290 Infinity LC For Multi-Plant Growth Regulator Analysis in Grapes Application Note Food Safety Author Sunil Kulkarni Agilent Technologies
More informationGB Translated English of Chinese Standard: GB NATIONAL STANDARD OF THE
Translated English of Chinese Standard: GB31604.35-2016 www.chinesestandard.net Buy True-PDF Auto-delivery. Sales@ChineseStandard.net GB NATIONAL STANDARD OF THE PEOPLE S REPUBLIC OF CHINA GB 31604.35-2016
More informationDepartment of Analytical Chemistry, International Institute of Biotechnology and Toxicology (IIBAT), Padappai, Kancheepuram , India
International Scholarly Research Network ISRN Analytical Chemistry Volume 2012, Article ID 908795, 5 pages doi:10.5402/2012/908795 Research Article Development and Validation of a HPLC-UV Method for Simultaneous
More informationValidation Report 18
EURL for Cereals and Feeding stuff National Food Institute Technical University of Denmark Validation Report 18 Determination of pesticide residues in maize for livestock feed by GC-MS/MS and LC-MS/MS
More informationDetermination of Aminoglycosides in animal tissue by means of LC/MS-MS
Austrian Agency for Health and Food Safety (AGES) Determination of Aminoglycosides in animal tissue by means of LC/MS-MS Created / revised Technical check QM check Release Name Thomas Aichinger Martin
More informationApplication Note. Author. Abstract. Food Safety. Syed Salman Lateef Agilent Technologies, Inc. Bangalore, India
Analysis of fumonisin, FB1 and FB2 mycotoxins in corn food and feed samples using the Agilent 1120 Compact LC System coupled to the Agilent 6140 Single Quadrupole LC/MS System Application Note Food Safety
More informationEPA Method 535: Detection of Degradates of Chloroacetanilides and other Acetamide Herbicides in Water by LC/MS/MS
Application Note EPA Method 535 EPA Method 535: Detection of Degradates of Chloroacetanilides and other Acetamide Herbicides in Water by LC/MS/MS API 3200 LC/MS/MS System Overview Described here is the
More informationThe Analysis of Fluoroquinolones in Beef Kidney Using HPLC Electrospray Mass Spectrometry Application
The Analysis of Fluoroquinolones in Beef Kidney Using HPLC Electrospray Mass Spectrometry Application Food Authors Ralph Hindle Access Analytical Labs #3, 2616-16 Street N.E. Calgary, Alberta T2E 7J8 Canada
More informationMethod Development in Solid Phase Extraction using Non-Polar ISOLUTE SPE Columns for the Extraction of Aqueous Samples
Technical Note 101 Method Development in Solid Phase Extraction using Non-Polar ISOLUTE SPE Columns for the Extraction of Aqueous Samples This technical note includes by specific information on the extraction
More informationThe Quantitation and Identification of Coccidiostats in Food by LC-MS/MS using the AB SCIEX 4000 Q TRAP System
The Quantitation and Identification of Coccidiostats in Food by LC-MS/MS using the AB SCIEX 4000 Q TRAP System Bertram ieland 1 and Stephen Lock 2 1 AB SCIEX ieuwerkerk aan den Ijssel, The etherlands;
More informationDetermination of Pharmaceuticals in Water by SPE and LC/MS/MS in Both Positive and Negative Ion Modes Application
Determination of Pharmaceuticals in Water by SPE and LC/MS/MS in Both Positive and Negative Ion Modes Application Environmental Authors Chin-Kai Meng Agilent Technologies, Inc. 85 Centerville Road Wilmington,
More informationAmphetamines, Phentermine, and Designer Stimulant Quantitation Using an Agilent 6430 LC/MS/MS
Amphetamines, Phentermine, and Designer Stimulant Quantitation Using an Agilent 643 LC/MS/MS Application Note Forensic Toxicology Authors Jason Hudson, Ph.D., James Hutchings, Ph.D., and Rebecca Wagner,
More informationMaximizing Triple Quadrupole Mass Spectrometry Productivity with the Agilent StreamSelect LC/MS System
Maximizing Triple Quadrupole Mass Spectrometry Productivity with the Agilent StreamSelect LC/MS System Application Note Authors Kevin McCann, Sameer Nene, Doug McIntyre, Edmond Neo, Dennis Nagtalon, and
More informationSimultaneous Determination of Paraquat and Diquat in Environmental Water Samples by HPLC-MS/MS
Simultaneous Determination of Paraquat and Diquat in Environmental Water Samples by HPLC-MS/MS Richard Jack, Xiaodong Liu, Leo Wang, and Chris Pohl OT70806_E 08/13S 1 The world leader in serving science
More informationDETERMINATION OF CHLORAMPHENICOL RESIDUES IN HONEY BY MONOLITHIC COLUMN LIQUID CHROMATOGRAPHY MASS SPECTROMETRY AFTER USE OF QUECHERS CLEAN-UP
ACTA CHROMATOGRAPHICA, NO. 17, 2006 DETERMINATION OF CHLORAMPHENICOL RESIDUES IN HONEY BY MONOLITHIC COLUMN LIQUID CHROMATOGRAPHY MASS SPECTROMETRY AFTER USE OF QUECHERS CLEAN-UP C. Pan 1,*, H. Zhang 2,
More informationStrategies for the Analysis of Therapeutic Peptides in Biofluids by LC-MS/MS. Lee Goodwin
Strategies for the Analysis of Therapeutic Peptides in Biofluids by LC-MS/MS Lee Goodwin Sample Preparation Chromatography Detection General Strategies Examples New Approaches Summary Outline ABUNDANCE
More informationYun W. Alelyunas, Mark D. Wrona, Russell J. Mortishire-Smith, Nick Tomczyk, and Paul D. Rainville Waters Corporation, Milford, MA, USA INTRODUCTION
Quantitation by High Resolution Mass Spectrometry: Using Target Enhancement and Tof-MRM to Achieve Femtogram-level On-column Sensitivity for Quantitation of Drugs in Human Plasma Yun W. Alelyunas, Mark
More informationThis method describes the identification of the following prohibited colorants in cosmetic products:
A. IDENTIFICATION BY TLC 1. SCOPE AND FIELD OF APPLICATION This method describes the identification of the following prohibited colorants in cosmetic products: Names C I number Pigment Orange 5 12075 Metanil
More information5 Efrotomycin. [Summary of efrotomycin] ET A 2 ET A 1 ET B 2 ET B 1 C 59 H 88 N 2 O 20 MW: 1145
5 Efrotomycin H H N H N H ET A 1 ET A 2 H H N N H NH H H ET B 1 ET B 2 H C 59 H 88 N 2 20 MW: 1145 [Summary of efrotomycin] Efrotomycin (ET) is an antibiotic obtained by the incubation of Nocardia lacamduranns,
More informationQuantitative Analysis of EtG and EtS in Urine Using FASt ETG and LC-MS/MS
Quantitative Analysis of EtG and EtS in Urine Using FASt ETG and LC-MS/MS UCT Part Numbers: CSFASETG203 - CLEAN SCREEN FASt ETG, 200mg / 3mL tube SLETG100ID21-3UM - Selectra ETG HPLC column, 100 x 2.1
More information12 Nicarbazin Nicarbazin (4,4 -dinitro carbanilid (DNC) and 2-hydroxy-4,6-dimethyl pyrimidine (HDP))
12 Nicarbazin Nicarbazin (4,4 -dinitro carbanilid (DNC) and 2-hydroxy-4,6-dimethyl pyrimidine (HDP)) O - O - O N + O N + O N NH N H N H O 1,3-bis(4-nitrophenyl)urea, 4,6-dimethyl-1H-pyrimidin-2-one C 13
More informationA RP-HPLC METHOD DEVELOPMENT AND VALIDATION OF PARA- PHENYLENEDIAMINE IN PURE FORM AND IN MARKETED PRODUCTS
A RP-HPLC METHOD DEVELOPMENT AND VALIDATION OF PARA- PHENYLENEDIAMINE IN PURE FORM AND IN MARKETED PRODUCTS CH.MOUNIKA*, M.KINNERA Research Article SIR.C.R.REDDY COLLEGE OF PHARMACEUTICAL SCIENCES, ELURU.
More informationEPA Method 535: Detection of Degradates of Chloroacetanilides and other Acetamide Herbicides in Water by LC/MS/MS
EPA Method 535: Detection of Degradates of Chloroacetanilides and other Acetamide Herbicides in Water by LC/MS/MS Christopher Borton AB SCIEX Golden, Colorado verview Described here is the analysis of
More information[ Care and Use Manual ]
Oasis HLB DISKS I. Introduction Oasis HLB is a Hydrophilic-Lipophilic-Balanced, water-wettable, reversed-phase sorbent for all your SPE needs. It is made from a specific ratio of two monomers, the hydrophilic
More information25-OH VITAMIN D 3 AND 25-OH VITAMIN D 2 IN PLASMA BY UV / VIS FAST CODE Z19710
25-OH VITAMIN D 3 AND 25-OH VITAMIN D 2 IN PLASMA BY UV / VIS FAST CODE Z19710 BIOCHEMISTRY Quantification of 25-hydroxyvitamin D 3 (25-hydroxycholecalciferol) in serum is the best established indicator
More informationSulfonamide Residues (Three) ELISA Quantitation Kit. Manual
Sulfonamide Residues (Three) ELISA Quantitation Kit Manual Catalog number: 40-784-140023 Immunoperoxidase Assay for Determination of Sulfamerzine (SM1), Sulfanethazine (SM2), Sulfadimethoxine (SDM) in
More informationMETHOD 8032A ACRYLAMIDE BY GAS CHROMATOGRAPHY
METHOD 8032A ACRYLAMIDE BY GAS CHROMATOGRAPHY 1.0 SCOPE AND APPLICATION 1.1 Method 8032 is used to determine trace amounts of acrylamide monomer (CAS No. 79-06-1) in aqueous matrices. This method may be
More informationImproved Extraction of THC and its Metabolites from Oral Fluid Using Oasis PRiME HLB Solid Phase Extraction (SPE) and a UPLC CORTECS C 18
Using Oasis PRiME HLB Solid Phase Extraction (SPE) and a UPLC CORTECS C 18 Column Xin Zhang, Jonathan P. Danaceau, and Erin E. Chambers Waters Corporation, Milford, MA, USA APPLICATION BENEFITS Semi-validated
More informationQuantitative analysis of small molecules in biological samples. Jeevan Prasain, Ph.D. Department of Pharmacology & Toxicology, UAB.
Quantitative analysis of small molecules in biological samples 100 Jeevan Prasain, Ph.D. Department of Pharmacology & Toxicology, UAB % 0 300 500 700 900 1100 1300 1500 1700 m/z Class Overview Introduction
More informationIntroduction to Pharmaceutical Chemical Analysis
Introduction to Pharmaceutical Chemical Analysis Hansen, Steen ISBN-13: 9780470661222 Table of Contents Preface xv 1 Introduction to Pharmaceutical Analysis 1 1.1 Applications and Definitions 1 1.2 The
More informationCHAPTER 1 Role of Bioanalytical Methods in Drug Discovery and Development
UMMERY The need to develop new analytical methods for assurance of quality, safety and efficacy of drugs and pharmaceuticals is quite important because of their use not only as health care products but
More informationElectronic Supplementary Information. The selective response of templated polymer for the cationic drug
Electronic Supplementary Material (ESI) for RSC Advances. This journal is The Royal Society of Chemistry 2017 Electronic Supplementary Information The selective response of templated polymer for the cationic
More informationVALIDATION OF A UPLC METHOD FOR A BENZOCAINE, BUTAMBEN, AND TETRACAINE HYDROCHLORIDE TOPICAL SOLUTION
VALIDATION OF A UPLC METHOD FOR A BENZOCAINE, BUTAMBEN, AND TETRACAINE HYDROCHLORIDE TOPICAL SOLUTION Andrew J. Aubin and Tanya L. Jenkins Waters Corporation, Milford, MA, USA INTRODUCTION Benzocaine (4-Aminobenzoic
More information[application note] INTRODUCTION EXPERIMENTAL. Specimens. Extraction
Testing for GHB in hair by GC tandem quadrupole MS Marie Bresson, Vincent Cirimele, Pascal Kintz, Marion Villain; Laboratoire Chemtox, Illkirch, France Timothy Jenkins, Waters Corporation, Manchester,
More informationHighly sensitive and rapid analysis of synthetic dyes in sea food by LC/MS/MS
PO-CON1745E Highly sensitive and rapid analysis of synthetic dyes in sea food by LC/MS/MS ASMS 2017 MP 189 Shailendra Rane 1, Ashutosh Shelar 1, Shailesh Damale 1, Rashi Kochhar 1, Purshottam Sutar 1,
More informationDetermination of Off-Odor Compounds in Drinking Water Using an SPME Device with Gas Chromatography and Mass Spectrometry
Application Note Environmental Determination of Off-Odor Compounds in Drinking Water Using an SPME Device with Gas Chromatography and Mass Spectrometry Authors Ye Kong and Zhe Cao Agilent Technologies,
More informationAnalysis of Pharmaceuticals and Personal Care Products in River Water Samples by UHPLC-TOF
application Note Liquid Chromatography/ Mass Spectrometry Author Sharanya Reddy PerkinElmer, Inc. Shelton, CT USA Analysis of Pharmaceuticals and Personal Care Products in River Water Samples by UHPLC-TOF
More informationRapid quantification of Chinese medicine Zuo Jin Pill using rapid resolution liquid chromatography
Rapid quantification of Chinese medicine Zuo Jin Pill using rapid resolution liquid chromatography Application Note Traditional Chinese Medicine Authors Xu Liang, Xi Zhang School of Pharmacy Second Military
More informationCHAPTER INTRODUCTION OF DOSAGE FORM AND LITERATURE REVIEW
75 CHAPTER 3 DEVELOPMENT AND APPLICATION OF STABILITY-INDICATING HPLC METHOD FOR THE DETERMINATION OF NEVIRAPINE AND ITS IMPURITIES IN COMBINATION DRUG PRODUCT 3.1 INTRODUCTION OF DOSAGE FORM AND LITERATURE
More informationDETERMINATION OF ANTIBIOTICS AND OTHER COMPONENTS IN MEDICINAL-LOTION AND EVALUATION
IJRRAS 4 () March www.arpapress.com/volumes/vol4issue/ijrras_4 5.pdf DETERMINATION OF ANTIBIOTICS AND OTHER COMPONENTS IN MEDICINAL-LOTION AND EVALUATION Changming Zhang*, Zhanggen Huang, Shijie Guo &
More informationSupporting Information. Detection and Occurrence of Chlorinated By-products of Bisphenol A, Nonylphenol and
1 2 3 Supporting Information Detection and Occurrence of Chlorinated By-products of Bisphenol A, Nonylphenol and Estrogens in Drinking Water of China: Comparison to the Parent Compounds 4 5 6 7 8 1 Laboratory
More informationSupporting Information For:
Supporting Information For: Peptidic α-ketocarboxylic Acids and Sulfonamides as Inhibitors of Protein Tyrosine Phosphatases Yen Ting Chen, Jian Xie, and Christopher T. Seto* Department of Chemistry, Brown
More informationDetermination of 17 Organotin Compounds in Beverages Using Triple Quadrupole GC-MS/MS System
Determination of 17 Organotin Compounds in Beverages Using Triple Quadrupole GC-MS/MS System Application Note Authors Wenwen Wang, Zhe Cao Agilent Technologies, Inc. No.3, Wang Jing Bei Lu, Chao Yang District,
More informationInternational Journal of Research in Pure and Applied Chemistry
Available online at http://www.urpjournals.com International Journal of Research in Pure and Applied Chemistry Universal Research Publications. All rights reserved Original Article Simultaneous determination
More informationAPPLICATION BENEFITS INTRODUCTION WATERS SOLUTIONS KEY WORDS. Simultaneous high-throughput screening of melamine (MEL) and cyanuric acid (CYA).
A Rapid and Sensitive Method for the Simultaneous Determination of and Cyanuric Acid in Infant Formulas, Adult utritional Products, and Protein Powders APPLICATIO BEEFITS Simultaneous high-throughput screening
More informationA New Polymer-based SPE Sorbent to Reduce Matrix Effects in Bioanalytical LC-MS/MS
A ew Polymer-based SPE Sorbent to Reduce Matrix Effects in Bioanalytical LC-MS/MS M. Cleeve, L. Williams, A. owells, G. Davies, S. Merriman, S. Plant,. Gooding, J. Labadie, R. Johnston, M. Burke 1, R.
More informationApplication Note GCMS-03 Reliable high-throughput quantification of melamine and related analogs below regulatory limits in food using the EVOQ GC-TQ
Application Note GCMS03 Reliable highthroughput quantification of melamine and related analogs below regulatory limits in food using the EVOQ GCTQ Introduction is a molecule that presents a high content
More informationGlyphosate in all its forms
Glyphosate in all its forms S. Goscinny and V. Hanot Scientific Institute for Public Health Pesticides Unit A breakthrough molecule Since its first appearance on the market in 1974, glyphosate has become
More informationMethod Development and Validation for the Estimation of Darunavir in Rat Plasma by RP-HPLC
World Journal of Pharmaceutical Sciences ISSN (Print): 2321-3310; ISSN (Online): 2321-3086 Published by Atom and Cell Publishers All Rights Reserved Available online at: http://www.wjpsonline.org/ Original
More informationDetection of 9-tetrahydrocannabinol ( 9-THC) in human urine by Solid Phase Extraction and HPLC.
Detection of 9-tetrahydrocannabinol ( 9-THC) in human urine by Solid Phase Extraction and HPLC. Abstract Chetna Mittal, PhD, Asha Oroskar, PhD,, Anil Oroskar, PhD Orochem Technologies Inc. Lombard, IL,
More informationNew Dynamic MRM Mode Improves Data Quality and Triple Quad Quantification in Complex Analyses
New Dynamic MRM Mode Improves Data Quality and Triple Quad Quantification in Complex Analyses Technical Overview Authors Abstract Peter Stone, Thomas Glauner, Frank Kuhlmann, Tim Schlabach and Ken Miller
More informationONDERSTEPOORT VETERINARY INSTITUTE METHOD: RTETH 042 DETERMINATION OF TETRACYCLINES IN HONEY 1. INTRODUCTION 2. EQUIPMENT
ONDERSTEPOORT VETERINARY INSTITUTE Analytical Methods Page 1 of 9 Revision: 3 Review date: November 2013 Approved by: L/T Manager METHOD: RTETH 042 DETERMINATION OF TETRACYCLINES IN HONEY 1. INTRODUCTION
More informationFractionation of Acidic, Basic, and Neutral Drugs from Plasma with an SPE Mixed Mode Strong Cation Exchange Polymeric Resin (Agilent SampliQ SCX)
Fractionation of Acidic, Basic, and Neutral Drugs from Plasma with an SPE Mixed Mode Strong Cation Exchange Polymeric Resin (Agilent SampliQ SCX) Application Note Forensic Toxicology Authors Bellah. Pule,
More informationAssay Robustness Improvement for Drug Urinalysis Using FAIMS and H-SRM on a Triple- Quadrupole Mass Spectrometer
38 Current Trends in Mass Spectrometry November 6 Assay Robustness Improvement for Drug Urinalysis Using FAIMS and H-SRM on a Triple- Quadrupole Mass Spectrometer This article demonstrates the improved
More informationApplication Note. Author. Abstract. Food Testing & Agriculture. Edgar Naegele Agilent Technologies, Inc. Waldbronn, Germany
Analysis of Pesticides by Supercritical Fluid Chromatography/ Mass Spectrometry Optimizing the Agilent 126 Infi nity Analytical SFC System in Combination with the Agilent 646 Triple Quadrupole LC/MS Application
More informationHigh Sensitivity HPLC Analysis of Perchlorate in Tap Water Using an Agilent 6460 Triple Quadrupole LC/MS System
High Sensitivity HPLC Analysis of Perchlorate in Tap Water Using an Agilent 66 Triple Quadrupole LC/MS System Application Note Environmental Authors Don Noot, Matthew Noestheden, and Ralph Hindle Vogon
More information- A7/13 - PART 2. Matrix Analyte(s) Method LOQ Reference. HPLC with fluorescence detection after acid hydrolysis
- A7/1 - Appendix 7 Format for the Compilation of Tier II Summaries - Active substance PART Section Analytical methods The example of a summary and assessment of data which follows is intended to illustrate
More informationCHROMABOND HLB. Introduction. Advantages of CHROMABOND HLB. Technical data
Introduction The enrichment of hydrophilic analytes from polar matrices is a challenge because they often cannot be retained by C 18 / C 8 -modified silica or hydrophobic polymer adsorbents. To overcome
More informationRapid and Sensitive Analysis of Antibiotics in Children s Urine Using the X500R QTOF System
Rapid and Sensitive Analysis of Antibiotics in Children s Urine Using the X500R QTOF System Binjie Liu, Haiyan Chen, Lei Yi, Wan Wang, Lijun Li, Wenhai Jin SCIEX, Asia & Pacific area Application Support
More informationUsing UHPLC-Triple Quadrupole MS/MS to Detect the Presence of Bark Extract and Yohimbine Adulteration in Dietary Supplements and Botanicals
Using UHPLC-Triple Quadrupole MS/MS to Detect the Presence of Bark Extract and Adulteration in Dietary Supplements and Botanicals Application Note Food Testing & Agriculture Authors James Neal-Kababick
More informationApplication Note. Edgar Naegele. Abstract
Fast identification of main drug metabolites by quadrupole time-of-flight LC/MS Measuring accurate MS and MS/MS data with the Agilent 651 Q-TOF LC/MS and identification of main meta-bolites by comparison
More informationClinical Toxicology. Biomass Component Extraction: The uneaten cooked plant specimen was prepared for
Clinical Toxicology Page of 0 Materials and Methods Biomass Component Extraction: The uneaten cooked plant specimen was prepared for chemical analysis as follows. The sample was frozen, diced, pulverized
More informationChapter 5. Irbesartan. Page no. 64 to 80
Page no. 64 to 80 , a nonpeptide tetrazole derivative, is an angiotensin receptor blocker (ARB) used mainly for the treatment of hypertension and diabetic nephropathy [65]. It is a specific competitive
More informationVolume 6, Issue 2, January February 2011; Article-015
Research Article DEVELOPMENT AND VALIDATION OF A RP-HPLC METHOD FOR THE DETERMINATION OF DAPOXETINE HYDROCHLORIDE IN PHARMACEUTICAL FORMULATION USING AN EXPERIMENTAL DESIGN Pratik Mehta*, Ujjwal Sahoo,
More informationDetermination of pesticides in baby food by UHPLC/MS/MS using the Agilent 1290 Infinity LC system and the Agilent 6460 triple quadrupole LC/MS
Determination of pesticides in baby food by UHPLC/MS/MS using the Agilent 1290 Infinity LC system and the Agilent 6460 triple quadrupole LC/MS Application Note Food Authors Gerd Vanhoenacker, Frank David,
More information7. Stability indicating analytical method development and validation of Ramipril and Amlodipine in capsule dosage form by HPLC.
7. Stability indicating analytical method development and validation of and in capsule dosage form by HPLC. 7.1 INSTRUMENTS AND MATERIALS USED 7.1.1 INSTRUMENTS 1. Shimadzu LC-2010 CHT with liquid chromatograph
More informationEVOLUTE WCX Columns for Solid Phase Extraction of Quaternary Amines and Strongly Basic Compounds from Aqueous Samples
TN143 EVOLUTE WCX Columns for Solid Phase Extraction of Quaternary Amines and Strongly Basic Compounds from Aqueous Samples This Chemistry Data Sheet provides guidelines for the extraction of quaternary
More information