Sampling, sample preparation and analyte isolation
|
|
- Muriel Parsons
- 5 years ago
- Views:
Transcription
1 H 3C COOH O CH3 OH OH HOOC O CH3 HOOC O CH 3 OH NH 2 COOH O Sampling, sample preparation and analyte isolation Hans van Egmond, with assistence of Tom Whitaker, Ton van Osenbruggen & John Gilbert Beijing, 12 December SELAMAT China Maize load: Fumonisin = x Fumonisin tolerance? Research Quality control Regulatory Export/Import 2 1
2 What do we do with this shipload? Official (AOAC, CEN): HPLC/GC, LC/MS, ELISA, FL, TLC sample laboratory analysis 3 Techniques used in mycotoxin regulatory analysis LC GC/MS GC ELISA fluorometry TLC minicolumn frequency of techniques 4 2
3 What do we do with this shipload? sample laboratory analysis Official (AOAC, CEN): HPLC/GC, LC/MS, ELISA, FL, TLC rapid: ELISA, dipstick, sensor, lateral flow Management decision - valid results 5 Is this shipload okay? The fumonisin concentration in the lot cannot be determined with 100% certainty by taking samples from the lot Uncertainty is due to variablity among sample test results 6 3
4 Outline of presentation Introduction Variability associated with sampling, sample preparation and analysis Analyte isolation and clean-up Focus on immunoaffinity cleanup Summary 7 Outline of presentation Introduction Variability associated with sampling, sample preparation and analysis Analyte isolation and clean-up Focus on immunoaffinity cleanup Summary 8 4
5 Lot Avg.= 3.6 mg/kg GOOD BAD ACCEPT REJECT x (Seller s Risk) ACCEPT x (Buyer s Risk) REJECT 0 Tolerance mg/kg 10 5
6 The perfect Operating Characteristic curve Lots Accepted (%) 10 0 Good Lots Bad Lots 0 Tolerance Lot Concentration High False Pos. (Seller's Risk) Lots Accepted (%) Good Lots Bad Lots (Buyer's Risk) False Neg. 0 Tolerance Lot Concentration 12 6
7 Mycotoxin test procedure Variability Distribution Performance evaluation 13 Lot test procedure sample Mill sample preparation analysis test result 14 7
8 sampling error total error sample preparation error analytical error lot sample preparation analysis 15 s 2 = s 2 + s 2 + s 2 t s sp a s 2 s 2 s 2 spa sp a = + s 2 a = s a
9 Coefficient of Variation (%) Coefficient of Variation Total Sampling (1.1 kg) Sample Prep. (25 g, Romer) Analysis (1 aliquot, HPLC) Fumonisin Concentration - C (mg/kg) 17 Variance at 2 mg/kg Test Variance Ratio 1.1 kg Romer, 25 g HPLC Total
10 Variance at 2 mg/kg Test Variance Test Variance 1.1 kg kg Romer, 25 g Romer, 25 g HPLC HPLC Total Total Variance at 2 mg/kg Test Variance Test Variance 1.1 kg kg Romer, 25 g Romer, 50 g HPLC HPLC Total Total
11 Variance at 2 mg/kg Test Variance Test Variance 1.1 kg kg Romer, 25 g Romer, 25 g HPLC HPLC Total Total Variance at 2 mg/kg Test Variance Test Variance 1.1 kg kg Romer, 25 g Romer, 50 g HPLC HPLC Total Total
12 Acceptance Probability (%) OC Curve for 1.1 kg Sample Sample kg Sample Prep. - Romer Mill, 25g Analysis - HPLC Accept/Reject Limit - 2 mg/kg Fumonisin Concentration (mg/kg) 23 Reduce Both Buyer s and Seller s Risk s Reduce Variability of Test Procedure - Increase Sample Size 24 12
13 OC curves for 1.1, 2.2, and 4.4 kg samples Acceptance Probability (%) Sample Prep. - Romer Mill, 25g Analysis - HPLC Accept/Reject Limit - 2 mg/kg 1.1 kg 2.2 kg 4.4 kg Fumonisin Concentration (mg/kg) 25 Reduce seller s risk Accept/reject limit > tolerance Reduce buyer s risk Accept/reject limit < tolerance 26 13
14 OC curves for 1, 2, and 4 mg/kg accept/reject limits Acceptance Probability (%) Sample kg Sample Prep. - Romer Mill, 25g Analysis - HPLC 1 mg/kg 2 mg/kg 3 mg/kg Fumonisin Concentration (mg/kg) 27 Sampling plans developed by Tom Whitaker Mycotoxin maize peanuts cottonseed Commodity almonds wheat barley coffee aflatoxin fumonisin DON ochratoxin 28 14
15 Evaluation of mycotoxin sampling plans FAO Food & Nutrition Paper 55 Sampling Plans for Aflatoxin Analysis in Peanuts and Corn 29 Outline of presentation Introduction Variability associated with sampling, sample preparation and analysis Analyte isolation and clean-up Focus on immunoaffinity cleanup Summary 30 15
16 Sampling Extraction Clean-up Concentration Ultimate separation Detection and quantitation Confirmation of identity 31 Extraction from food and feed Choice of suitable solvent (mixtures) - methanol/water - acetonitrile/water - addition of chloroform/hexane for defatting Deconjugation if mycotoxin is bound to matrix (e.g. issue samples) Blending at high speed or shaking (avoid emulsion formation) Filter or centriguge to obtain clear supernatant 32 16
17 Extraction Need to demonstrate adequate extraction from naturally contaminated materials Spiking of matrices does NOT demonstrate adequate extraction Repeated extraction of same matrix gives some indication of recovery 33 Extraction of mycotoxins from foods and feeds Spiking gives good indication of losses through analytical stages post-extraction Performance of extraction solvents evaluated relative one another, but difficult to measure recovery in absolute terms as true mycotoxin content never known Repeated extraction of same matrix gives some indication of recovery Foods containing radio-labelled mycotoxins can facilitate extraction studies 34 17
18 Sampling Extraction Clean-up Concentration Ultimate separation Detection and quantitation Confirmation of identity 35 Clean-up for mycotoxin determination Removal of co-extractives Preliminary separation and concentration Various possibilities exist (crude chromatography, adsorption, antibodies) 36 18
19 Clean-up after extraction Silicagel chromatography SPE columns Ion exchange columns Romer Mycosep columns Immuno affinity columns 37 Solid Phase Extraction On- or off line Based on polar separation Concentration possible 38 19
20 Ion exchange columns Fumonisins, moniliformin The primary retention mechanism of the compound is based on the electrostatic attraction of the charged functional group Charging can be modified by changing ph 39 Mycosep (1) A & B-trichothecenes, zearalenone Loaded with adsorbents like charcoal, Celite, ion exchange resins Fast and easy to use 40 20
21 Mycosep (2) 41 Outline of presentation Introduction Variability associated with sampling, sample preparation and analysis Analyte isolation and clean-up Focus on immunoaffinity cleanup Summary 42 21
22 Immuno affinity columns Advantage IACs: -selective - sample concentration Disadvantage IACs: - no high concentration of organic phase - ph sensitive - relatively expensive, multiple use sometimes possible, but declining recivery Final separation with HPLC or GC 43 Immuno affinity columns 44 22
23 Comparison of SPE clean-up with affinity column for aflatoxin M 1 in cheese Fluorescence detector response Aflatoxin M 1 Aflatoxin M 1 Time (minutes) 45 Immuno affinity columns ph can be important ph important: Spike sometimes in acetic acid solution Acid capacity PBS-buffer low 46 23
24 47 Immuno affinity columns Elute with organic solvent Add sample Clean with water or buffer 48 24
25 Gilson ASPEC System for Automated Analysis 49 Automated system - ASPEC Sample loaded on to affinity column Column washed Mycotoxin eluted Sample concentrated Injection on to HPLC Full system control processing and analysis 50 25
26 Gilson ASPEC System 51 Immuno affinity columns available for several Fusarium toxins Zearalenone Fumonisins Deoxynivalenol T-2 & HT-2 toxins 52 26
27 Immuno affinity columns in combination with HPLC Provide excellent clean-up of complex matrices and coloured food and feed matrices Concentrate the toxin of interest allowing more sensitive detection Successfully validated, accepted and standardized by international organisations 53 CEN working group biotoxins 54 27
28 Analysis of fumonisins B 1 and B 2 by HPLC Extraction from maize with acetonitrile:water (1:1) Shake 60 min or blend for 1-2 min Filter Purify on SPE, SAX or affinity column Derivatize with o-phthaldialdehyde and 2- mercaptoethanol RP-HPLC with fluorescence detection 55 Cleanup - analysis Conventional cleanup is relatively time consuming LC-MS is rapidly coming up - 1 extraction step - Inject on LC-MS - Expensive but low hands-on costs - Multi method 56 28
29 Outline of presentation Introduction Variability associated with sampling, sample preparation and analysis Analyte isolation and clean-up Focus on immunoaffinity cleanup Summary 57 Summary Variability in sampling > variability in sampling preparation and analysis Detailed studies on sampling done and sampling plans developed e.g. by Tom Whitaker For clean-up of sample extracts, various possibilities exist: IA-LC technique efficient, validated and frequently used LC-MS is now developing as an alternative technique, but not yet fully validated 58 29
30 H 3C COOH O CH3 OH OH HOOC O CH3 HOOC O CH 3 OH NH 2 COOH O Sampling, sample preparation and analyte isolation Hans van Egmond, with assistence of Tom Whitaker, Ton van Osenbruggen & John Gilbert Beijing, 12 December 2006 Thank you for listening! 59 SELAMAT China 30
Deoxynivalenol, sometimes called DON or vomitoxin,
WHITAKER ET AL.: JOURNAL OF AOAC INTERNATIONAL VOL. 83, NO. 5, 000 185 SPECIAL GUEST EDITOR SECTION Sampling, Sample Preparation, and Analytical Variability Associated with Testing Wheat for Deoxynivalenol
More informationChoosing Fit-For-Purpose Food Safety Methods
Choosing Fit-For-Purpose Food Safety Methods Outline Method selection Screening & quantification methods Extraction, cleanup and chromatography Detection methods Method criteria validation Conclusions
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 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 informationSensitive Femtogram Determination of Aflatoxins B 1 , B 2 , G 1. and G 2. in Food Matrices using Triple Quadrupole LC/MS. Authors.
Sensitive Femtogram Determination of Aflatoxins B 1, B 2, G 1 and G 2 in Food Matrices using Triple Quadrupole LC/MS Application Note Food Safety Authors Yang Chen and Jack Cappozzo National Center for
More informationMulti-Mycotoxin testing A routine approach
EDITORIAL Globalization of the trade of agricultural products contributed significantly to the discussion about potential hazards involved, thereby increasing especially the awareness for mycotoxins. Approximately
More informationSimultaneous Determination of 26 Mycotoxins in Sesame Butter Using Modified QuEChERS Coupled with UHPLC-ESI/Triple Quadrupole Mass Spectrometry
Simultaneous Determination of 2 Mycotoxins in Sesame Butter Using Modified QuEChERS Coupled with UHPLC-ESI/Triple Quadrupole Mass Spectrometry Application Note Food Authors Ying Liu, Shen Han, Pei-Yue
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 informationQ U A L I T Y I N N O V A T I O N S E R V I C E
Q U A L I T Y I N N O V A T I O N S E R V I C E Sample preparation challenges for determination of ochratoxin A in wheat Canadian Grain Commission, 2005 Tom Nowicki & Mike Roscoe Grain Research Laboratory
More informationPHL-IL and Mycotoxins. Andreia Bianchini, PhD University of Nebraska - Lincoln
PHL-IL and Mycotoxins Andreia Bianchini, PhD University of Nebraska - Lincoln Concerns About Mycotoxins Where populations have a single dietary staple May be exposed to great amounts Acute and chronic
More informationMULTI-ANALYTE MYCOTOXIN ANALYSIS. Mark Benvenuti, Jim Krol, Joe Romano, Waters Corporation, Milford, MA
ApplicationNTE Agricultural raw commodity foodstuffs, such as grains, vegetables and fruits, are subject to microbiological contamination during harvesting, storage and transport. Various molds and fungi
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 informationSpeaker/Author: W.P. Nxumalo*, ** Co-authors: Y. Naudé**, and M. Fernandes-Whaley*
Combining Ultrasonic Extraction (USE) and Solid Phase Extraction (SPE) for the Analysis of 11 Mycotoxins in Maize by Isotope Dilution Liquid Chromatography Tandem Mass Spectrometry (SIDA-UHPLC-MS/MS) Speaker/Author:
More informationDetection of Mycotoxins in Corn Meal Extract Using Automated Online Sample Preparation with Liquid Chromatography-Tandem Mass Spectrometry
Detection of Mycotoxins in Corn Meal Extract Using Automated Online Sample Preparation with Liquid Chromatography-Tandem Mass Spectrometry Yang Shi, Catherine Lafontaine, Timothy B. Haney, and François
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 informationDetection limit: grain, feed 500 ppb; milk 50 ppb; cream, cheese 5 ppb
Product information Background Deoxynivalenol (DON) Deoxynivalenol, called vomitoxin, is a toxic metabolite mainly produced by Fusarium graminearum. It is mainly found in wheat, barley, corn and feed.
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 informationSample Prep Options for GC users
Sample Prep Options for GC users Tina Chambers Technical Specialist Sample Preparation tina.chambers@agilent.com 949-842-0493 Why Bother? Removal of interferences which would otherwise affect detection
More informationAnalysis and Quantification of Mycotoxins in Cereals Using MRM HR on the SCIEX X500R QTOF System with SCIEX OS
Analysis and Quantification of Mycotoxins in Cereals Using MRM HR on the SCIEX X500R QTOF System with SCIEX OS Yang Zong 1, Cheng Haiyan 1, Zhong Hongjian 2, Li Lijun 1, Jin Wenhai 1 Phil Taylor 3 1. SCIEX,
More informationMETHOD 3600B CLEANUP
METHOD 3600B CLEANUP 1.0 SCOPE AND APPLICATION 1.1 Method 3600 provides general guidance on selection of cleanup methods that are appropriate for the target analytes of interest. Cleanup methods are applied
More informationChromatography Outline
Chem 2001 Summer 2004 Outline What is? The Chromatogram Optimization of Column Performance Why Do Bands Spread? Gas High-Performance Liquid Ion-Exchange 2 What is? In chromatography, separation is achieved
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 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 informationChemical Analysis Problem
Chemical Analysis Problem Hair analysis is frequently used for the long-term monitoring of drug and alcohol users. You are working at a forensics laboratory and have been given the task of developing a
More informationCHAPTER CHROMATOGRAPHIC METHODS OF SEPARATIONS
Islamic University in Madinah Department of Chemistry CHAPTER - ----- CHROMATOGRAPHIC METHODS OF SEPARATIONS Prepared By Dr. Khalid Ahmad Shadid Chemistry Department Islamic University in Madinah TRADITIONAL
More informationApplication of Raman Spectroscopy for Detection of Aflatoxins and Fumonisins in Ground Maize Samples
Application of Raman Spectroscopy for Detection of Aflatoxins and Fumonisins in Ground Maize Samples Kyung-Min Lee and Timothy J. Herrman Office of the Texas State Chemist, Texas A&M AgriLife Research
More informationEvaluation of Several Columns and Solvents for Post-Extraction Gel Permeation Chromatography (GPC) Clean-up of Fish Tissue Prior to PCB Analysis
Evaluation of Several Columns and Solvents for Post-Extraction Gel Permeation Chromatography (GPC) Clean-up of Fish Tissue Prior to PCB Analysis Keywords: Automated GX-271 GPC Clean-up System, Contaminants,
More informationWe are IntechOpen, the world s leading publisher of Open Access books Built by scientists, for scientists. International authors and editors
We are IntechOpen, the world s leading publisher of Open Access books Built by scientists, for scientists 3,500 108,000 1.7 M Open access books available International authors and editors Downloads Our
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 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 informationMETHOD 3600C CLEANUP
METHOD 3600C CLEANUP 1.0 SCOPE AND APPLICATION 1.1 Method 3600 provides general guidance on selection of cleanup methods that are appropriate for the target analytes of interest. Cleanup methods are applied
More informationThermo Scientific HyperSep Dispersive SPE Products. Efficient sample preparation and clean-up using the QuEChERS Method
Thermo Scientific HyperSep Dispersive SPE Products Efficient sample preparation and clean-up using the QuEChERS Method The QuEChERS method overcomes the problems associated with time consuming, expensive
More informationPrinciples of Gas- Chromatography (GC)
Principles of Gas- Chromatography (GC) Mohammed N. Sabir January 2017 10-Jan-17 1 GC is a chromatographic technique utilizes gas as the mobile phase which is usually an inert gas (Hydrogen, Helium, Nitrogen
More informationBasics in Solid Phase Extraction (SPE)
Basics in Solid Phase Extraction (SPE) Claudia Thiele, Sigma Aldrich Taufkirchen Euroanalysis 2011 Belgrade Lunch Symposium 13.09.2011 Agenda The Importance of Sample Prep Overview of SPE Technology SPE
More informationExperiment 1: Thin Layer Chromatography
Experiment 1: Thin Layer Chromatography Part A: understanding R f values Part B: R f values & solvent polarity Part C: R f values & compound functionality Part D: identification of commercial food dye
More informationPressurized Fluid Extraction for Quantitative Recovery of Aflatoxins B1 and B2 from Pistachio
Pressurized Fluid Extraction for Quantitative Recovery of Aflatoxins B1 and B2 from Pistachio Hassan S. Ghaziaskar*, Ali Sheibani Department of Chemistry, Isfahan University of Technology Isfahan, I.R.
More informationThis document is meant purely as a documentation tool and the institutions do not assume any liability for its contents
2006R0401 EN 13.03.2010 001.001 1 This document is meant purely as a documentation tool and the institutions do not assume any liability for its contents B COMMISSION REGULATION (EC) No 401/2006 of 23
More informationHPLC Background Chem 250 F 2008 Page 1 of 24
HPLC Background Chem 250 F 2008 Page 1 of 24 Outline: General and descriptive aspects of chromatographic retention and separation: phenomenological k, efficiency, selectivity. Quantitative description
More informationChromatographic Analysis
Chromatographic Analysis Distribution of Analytes between Phases An analyte is in equilibrium between the two phases [S 1 ] [S 2 ] (in phase 1) (in phase 2) AS [S2 ] K 2 A S [S1 ] 1 AS, A 1 S Activity
More informationIntroduction to Chromatography
Introduction to Chromatography Dr. Sana Mustafa Assistant Professor Department of Chemistry, Federal Urdu University of Arts, Science & Technology, Karachi. What is Chromatography? Derived from the Greek
More informationMacrolides 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 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 informationVeronica Maria Teresa Lattanzio, Stefania Della Gatta, Michal Godula, Angelo Visconti
Quantitative analysis of mycotoxins in cereal foods by Collision Cell Fragmentation - High Resolution Mass Spectrometry: performances and comparison with triple stage quadrupole detection. Veronica Maria
More informationYuhui Yang, An Trinh, Michael Ye, and Tom Henderson 595 North Harrison Road, Bellefonte, PA T HKB
Use of An Improved Version of C8+SCX Mixed-Mode Solid Phase Extraction Material for Clean Extraction and Recovery of Basic, Zwitterionic, Neutral and Acidic Compounds from Biological Fluids Yuhui Yang,
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 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 informationELISA Kit for Detection of Aflatoxin B1
ELISA Kit for Detection of Aflatoxin B1 (Product Number: 5501E101) (Aflatoxin is a class Ⅰ carcinogenic substance) INSTRUCTION MANUAL (v. 1.00) microtiter Color developed Measurement 1. Introduction Aflatoxin
More informationAnalytical Chemistry
Analytical Chemistry Chromatographic Separations KAM021 2016 Dr. A. Jesorka, 6112, aldo@chalmers.se Introduction to Chromatographic Separations Theory of Separations -Chromatography Terms Summary: Chromatography
More informationin animal feed Received: 29 June 2007 / Accepted: 20 May Wageningen Academic Publishers
World Mycotoxin Journal, August 2008; 1(3): 247-253 Wageningen g Academic P u b l i s h e r s Single laboratory validation data and uncertainty estimation of a liquid chromatographic method for determination
More informationFlash chromatography purification of high pka organic compounds with Teledyne Isco s specialty RediSep columns
Flash chromatography purification of high pka organic compounds with Teledyne Isco s specialty RediSep columns Mikael Mahler*, Veronica Thomason, and John Urh Teledyne Isco Inc., P.O. Box 82531, Lincoln
More informationSupporting Information
Electronic Supplementary Material (ESI) for RSC Advances. This journal is The Royal Society of Chemistry 214 Supporting Information Rapid and sensitive detection of acrylic acid using a novel fluorescence
More informationChromatographic Separation
What is? is the ability to separate molecules using partitioning characteristics of molecule to remain in a stationary phase versus a mobile phase. Once a molecule is separated from the mixture, it can
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 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 informationWhat type of samples are common? Time spent on different operations during LC analyses. Number of samples? Aims. Sources of error. Sample preparation
What type of samples are common? Sample preparation 1 2 Number of samples? Time spent on different operations during LC analyses 3 4 Sources of error Aims Sample has to be representative Sample has to
More informationHPLC. High Performance Liquid Chromatography (HPLC) Harris Chapter 25
High Performance Liquid Chromatography (HPLC) Harris Chapter 25 12/1/2005 Chem 253 - Chapter 25 1 HPLC Separation of nonvolatile or thermally unstable compounds. If the analyte/sample can be found to be
More informationThe Effect of Contact Angle and Wetting on Performance in Solid Phase Extraction
The Effect of Contact Angle and Wetting on Performance in Solid Phase Extraction Edouard S. P. Bouvier, Randy E. Meirowitz and Uwe D. Neue Waters Corporation, 34 Maple Street, Milford, MA 01757 USA Presented
More informationChromatography: Thin-Layer Chromatography (TLC) & Column Chromatography
Chromatography: Thin-Layer Chromatography (TLC) & Column Chromatography Part 1, p. 184: Separation of spinach pigments by TLC. (4 th Ed. P. 180) Part 2, p. 192: Separation of Fluorene and Fluorenone by
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 informationBIOO FOOD AND FEED SAFETY. Histamine Enzymatic Assay Kit Manual. Catalog #: Reference #:
BIOO FOOD AND FEED SAFETY Histamine Enzymatic Assay Kit Manual Catalog #: 1032-05 Reference #: 1032-05 BIOO Scientific Corp. 2010 TABLE OF CONTENTS GENERAL INFORMATION... 1 Product Description... 1 Procedure
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 informationAnalysis of Trace (mg/kg) Thiophene in Benzene Using Two-Dimensional Gas Chromatography and Flame Ionization Detection Application
Analysis of Trace (mg/kg) Thiophene in Using Two-Dimensional Gas Chromatography and Flame Ionization Detection Application Petrochemical Authors James D. McCurry and Bruce D. Quimby Agilent Technologies
More informationCHROMATOGRAPHY. The term "chromatography" is derived from the original use of this method for separating yellow and green plant pigments.
CHROMATOGRAPHY The term "chromatography" is derived from the original use of this method for separating yellow and green plant pigments. THEORY OF CHROMATOGRAPHY: Separation of two sample components in
More informationShodex TM ODP2 HP series columns
HPLC Columns Shodex TM ODP2 HP series columns Better retention of highly polar substances Technical notebook No. 6 Contents 1. Introduction 1-1. Specifications 1-2. Eluent Compatibility of ODP2 HP Series
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 informationDisadvantage: Destructive Technique once analyzed by GC, the sample is lost
Gas Chromatography Like other methods of chromatography, a partitioning of molecules must occur between the stationary phase and the mobile phases in order to achieve separation. This is the same equilibrium
More informationSPE. Simply Efficient! Watchers bond Solid Phase Extraction by ISU. Ver
SPE Simply Efficient! Watchers bond Solid Phase Extraction by ISU Ver. 05-11 Solid Phase Extraction Basic principles of Solid Phase Extraction Solid phase extraction (SPE) is a powerful method for sample
More informationApplication Note No Introduction. DMI Instrumentation. DMI Method. DMI for Lettuce and Pea Extracts. Lettuce results
Application Note No. 082 Multi-Residue Analysis of Pesticides in Samples of Lettuce and Peas Using Large Volume-Difficult Matrix Introduction-Gas Chromatography-Mass Spectrometry (LV-DMI-GC-MS) Richard
More informationACD/AutoChrom Assisted Method Development for Challenging Separations. Vera Leshchinskaya February 7, 2018
ACD/AutoChrom Assisted Method Development for Challenging Separations Vera Leshchinskaya February 7, 2018 Introduction Resolution of isomeric species is one of the most challenging areas of separation
More informationProline Fungicide on Corn Silage to Reduce Mycotoxins
Proline Fungicide on Corn Silage to Reduce Mycotoxins Purpose: To assess use of a fungicide such as Proline on corn silage to reduce mycotoxins in the stored feed and to access impact on corn silage yield.
More informationPLEASE SCROLL DOWN FOR ARTICLE
This article was downloaded by:[b-on Consortium - 27] On: 15 October 27 Access Details: [subscription number 77838475] Publisher: Taylor & Francis Informa Ltd Registered in England and Wales Registered
More informationHPLC Column Material - Bulk Ware
HPLC Column Material - Bulk Ware Constantly growing demands on separation efficiency and availability of solid phase material for packing HPLC columns and column packing stations have motivated us to provide
More informationGUIDELINES ON THE USE OF MASS SPECTROMETRY (MS) FOR IDENTIFICATION, CONFIRMATION AND QUANTITATIVE DETERMINATION OF RESIDUES CAC/GL
CAC/GL 56-2005 Page 1 of 6 GUIDELINES ON THE USE OF MASS SPECTROMETRY (MS) FOR IDENTIFICATION, CONFIRMATION AND QUANTITATIVE DETERMINATION OF RESIDUES CONFIRMATORY TESTS CAC/GL 56-2005 When analyses are
More informationProPac WCX-10 Columns
ProPac WCX-10 Columns Guidance for column use Tips to maximize column lifetime ProPac WCX-10 Column Tips and Tricks This guide provides essential information and invaluable guidelines for mobile phases,
More informationDATES: LAB: Liquid Chromatography Separation of Grape Kool-Aid
NAME: AP CHEMISTRY DATES: LAB: Liquid Chromatography Separation of Grape Kool-Aid PURPOSE There are a number of analytical techniques used to separate components of a mixture, or solution. They include
More informationSample Preparation. Approaches to Automation for SPE
Sample Preparation Approaches to Automation for SPE i Wherever you see this symbol, it is important to access the on-line course as there is interactive material that cannot be fully shown in this reference
More informationCfE Higher Chemistry. Unit 3: Chemistry in Society. Chemical Analysis as part of quality control
CfE Higher Chemistry Unit 3: Chemistry in Society Chemical Analysis as part of quality control 06/12/2017 Composition and purity 06/12/2017 Learning Outcomes : I can explain the basic principle of how
More informationValidation Report Determination of isoprothiolane residues in rice by GC-MS/MS (QuEChERS method)
NRL for Cereals DTU National Food Institute Validation Report Determination of isoprothiolane residues in rice by GC-MS/MS (QuEChERS method) Mette Erecius Poulsen & Hanne Bjerre Christensen 16 July 21
More informationIon Chromatography (IC)
Ion Chromatography (IC) Purpose: This module provides an introduction to Ion Chromatography (IC). In this module the basic theory and applications of IC will be presented at a level that assumes a basic
More informationLiquid Chromatography
Liquid Chromatography 1. Introduction and Column Packing Material 2. Retention Mechanisms in Liquid Chromatography 3. Method Development 4. Column Preparation 5. General Instrumental aspects 6. Detectors
More informationMeasuring ochratoxine A in wine after going through an immunoaffinity column and HLPC with fluorescence detection
Method OIV-MA-AS315-10 Type II method Measuring ochratoxine A in wine after going through an immunoaffinity column and HLPC with fluorescence detection (Oeno 16/2001 revised by Oeno 349-2011) 1. FIELD
More informationZearalenone ELISA Kit
Zearalenone ELISA Kit Catalog Number KA1428 96 assays Version: 10 Intended for research use only www.abnova.com Table of Contents Introduction... 3 Background... 3 Principle of the Assay... 3 General Information...
More informationQuantitative Analysis of Caffeine in Energy Drinks by High Performance Liquid Chromatography
Quantitative Analysis of Caffeine in Energy Drinks by High Performance Liquid Chromatography CHEM 329 Professor Vogt TA: Fahad Hasan Allison Poget Date Performed: April 5, 2016 Date Submitted: April 12,
More informationLiquid storage: Holds the solvent which is going to act as the mobile phase. Pump: Pushes the solvent through to the column at high pressure.
High performance liquid chromatography (HPLC) is a much more sensitive and useful technique than paper and thin layer chromatography. The instrument used for HPLC is called a high performance liquid chromatograph.
More informationLC-MS Based Method of Analysis for the Simultaneous Determination of four Mycotoxins in Cereals and Feed
LC-MS Based Method of Analysis for the Simultaneous Determination of four Mycotoxins in Cereals and Feed Results of a Collaborative Study Andreas Breidbach Katrien Bouten Katy Kroeger-Negiota Jörg Stroka
More informationLuminescence transitions. Fluorescence spectroscopy
Luminescence transitions Fluorescence spectroscopy Advantages: High sensitivity (single molecule detection!) Measuring increment in signal against a dark (zero) background Emission is proportional to excitation
More informationDetermination of mycotoxins in different food commodities by ultra-high-pressure liquid chromatography coupled to triple quadrupole mass spectrometry
RAPID COMMUNICATIONS IN MASS SPECTROMETRY Rapid Commun. Mass Spectrom. 2009; 23: 1801 1809 Published online in Wiley InterScience (www.interscience.wiley.com).4077 Determination of mycotoxins in different
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 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 informationChapter 27: Gas Chromatography. Principles Instrumentation Detectors Columns and Stationary Phases Applications
Chapter 27: Gas Chromatography Principles Instrumentation Detectors Columns and Stationary Phases Applications GC-MS Schematic Interface less critical for capillary columns Several types of Mass Specs
More informationChapter content. Reference
Chapter 7 HPLC Instrumental Analysis Rezaul Karim Environmental Science and Technology Jessore University of Science and Technology Chapter content Liquid Chromatography (LC); Scope; Principles Instrumentation;
More informationLiquid Chromatography
Liquid Chromatography 1. Introduction and Column Packing Material 2. Retention Mechanisms in Liquid Chromatography 3. Method Development 4. Column Preparation 5. General Instrumental aspects 6. Detectors
More informationAbstract: An minimalist overview of chromatography for the person who would conduct chromatographic experiments, but not design experiments.
Chromatography Primer Abstract: An minimalist overview of chromatography for the person who would conduct chromatographic experiments, but not design experiments. At its heart, chromatography is a technique
More informationDilution(*) Chromatography
WA20264 Poster # 184, HPLC 2002, Montreal, 4-5 June 2002 At-Column Column-Dilution for Preparative Dilution(*) Chromatography Cecilia Mazza, Jie Cavanaugh, Ziling Lu,Tom Sirard,Tom Wheat and Uwe Neue Waters
More informationTribo TM Ochratoxin-A ELISA Kit (Catalog No. TBS21133)
Tribo TM Ochratoxin-A ELISA Kit (Catalog No. TBS21133) General Description The Tribo TM Ochratoxin-A ELISA Kit is a solid phase direct competitive enzyme immunoassay. An Ochratoxin specific antibody optimized
More informationDetermination of Pesticide Residues in Oats by Automated. QuEChERS and LC/QQQ. Application Note. Abstract. Introduction
Determination of Pesticide Residues in Oats by Automated QuEChERS and LC/QQQ Application Note Abstract The QuEChERS (Quick-Easy-Cheap-Effective-Rugged-Safe) sample extraction method was developed for the
More informationUse of Ultra-High Performance LC-MS for Challenging Assays. David Browne, Laboratory Manager (LC-MS-MS), Covance Laboratories, Harrogate
Use of Ultra-High Performance LC-MS for Challenging Assays David Browne, Laboratory Manager (LC-MS-MS), Covance Laboratories, Harrogate Department of Bioanalytical Services Determination of drug substance
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 informationMulti-residue analysis of pesticides by GC-HRMS
An Executive Summary Multi-residue analysis of pesticides by GC-HRMS Dr. Hans Mol is senior scientist at RIKILT- Wageningen UR Introduction Regulatory authorities throughout the world set and enforce strict
More informationJo Marie Cook Bureau of Chemical Residue Laboratories
Jo Marie Cook Bureau of Chemical Residue Laboratories Incident Command Do as your told! Wait and see not on our shores! Yet! Follow FDA lead Hesitation to spend $$$ FERN and ccap activation Bring up NOAA
More information