Agilent SampliQ Products for Sample Preparation. Improve the quality of your sample preparation so you can improve the quality of your analysis.

Transcription

1 Agilent SampliQ Products for Sample Preparation Improve the quality of your sample preparation so you can improve the quality of your analysis.

2 Table of Contents Introduction to Agilent SampliQ...3 Selection of Agilent SampliQ SPE Mode and Phase...4 Cross Reference of Comparable Phases by Manufacturer...5 Agilent SampliQ Polymer...6 SampliQ Method Development Kits...6 Agilent SampliQ Polymeric A/N/B Method...7 OPT...8 SCX...10 SAX...12 WCX and WAX...14 DVB...15 PS-DVB Well Plates...16 Agilent SampliQ Silica...17 C C18EC Endcapped...18 C8 Octyl...18 C2 Ethyl...19 Phenyl...19 Silica...20 Cyano (CN)...20 Diol...21 Amino (NH 2 )...21 Strong Cation Exchange (Si-SCX)...22 Strong Anion Exchange (Si-SAX)...23 Additional Agilent SampliQ Phases...24 Florisil PR...24 Alumina A (acidic)...24 Alumina B (basic)...25 Alumina N (neutral)...25 Carbon...26 Mixed Mode C8/Si-SCX...26 Specialty SPE...27 Evidex SPE Cartridges...27 SPE Cartridges (for Schenck variation of QuEChERS method)...28 Bulk Sorbents...29 QuEChERS...30 Extraction Kits...30 Dispersive Kits...31 Ceramic Homogenizers...32 Standards for QuEChERS Products...33 Bulk Sorbents and Salts...34 Manifolds and Accessories...35 Vacuum Manifolds for Cartridges...35 Adapters and Replacement Parts...36 Vacuum Manifolds for 96-Well Plates Well Plate Manifold Parts and Supplies...38 Sealing Mats...38 Empty Reservoirs, Frits and Caps

3 Confidently extract and concentrate samples from complex matrices and ensure accurate, reproducible results right from the start. What is SPE? Solid phase extraction (SPE) is a fast, cost effective technique for purifying extracts and improving the accuracy and reproducibility of results. Sample preparation is an essential part of successful chromatographic measurement. It reduces the number and amount of potential interferences which can jeopardize your separation, detection, and quantification. Sample preparation can also extend column lifetime. Manufactured in the U.S. to strict ISO-9001 standards the same process Agilent uses for HPLC column packing material Agilent SampliQ (pronounced sam- plēk) SPE products deliver the high quality and performance you expect from the industry's leading manufacturer of chromatography instruments, columns, and supplies. With SampliQ SPE, you get the peace of mind that comes with: A wide selection of polymer, silica, and other sorbents in formats ranging from multiple cartridge sizes to 96-well plates. Trifunctional silica bonding provides greater hydrophobicity and stability than monofunctional bonding. Industry-leading quality control processes ensure consistent particle size, so you get superior flow-through and performance. A complete range of vacuum manifolds and accessories to help you meet all your SPE challenges. For ordering information, visit Simply put, SPE reduces sample complexity. By harnessing the principles of HPLC, SPE selectively removes interferences and/or analytes from complex matrices such as foods, environmental samples, and biological specimens. SPE can also replace liquid-liquid extraction protocols, which improves sample preparation throughput and reduces solvent consumption. SPE can make the difference between a definitive measurement and inaccurate, imprecise, irreproducible results. 3

4 Move more quickly toward the method that is right for your analysis. This flowchart helps you choose the right SampliQ polymer, silica, or other sorbent cartridges for routine applications that call for consistent results with higher sample volumes and lower detection limits. Selection of Agilent SampliQ SPE Mode and Phase Sample MW < 2000 Solubility Water-soluble Organic solvent-soluble Molecular Character Ionic Non-ionic (ion-paired) Soluble in polar solvent: MeOH (methanol), ACN (acetonitrile), THF (tetrahydrofuran) Soluble in moderately polar solvent: EtOAc (Ethyl Acetate), CH 2 Cl 2 (methylene chloride), Et 2 O (diethyl ether) Soluble in non-polar solvent: C5 (n-pentane), C6 (n-hexane) and ic8 (iso-octane) Stationary Phase Cationic Anionic Polar Moderately Polar Non-polar Polar Moderately Polar Non-polar Mode CX Cation Exchange AX Anion Exchange n-bpc Normal Bonded Phase Chromatography LSC Liquid-Solid Chromatography RPC Reversed Phase Chromatography n-bpc Normal Bonded Phase Chromatography LSC Liquid-Solid Chromatography RPC Reversed Phase Chromatography Phases: Polymeric SCX/WCX Strong/ Weak Cation Exchange SAX/WAX Strong/ Weak Anion Exchange OPT, DVB, PS-DVB OPT, DVB, PS-DVB Phases: Silica-based Si-SCX, C8/Si-SCX (mixed mode) Si-SAX, Amino (WAX) Cyano, Diol, Amino Silica C18, C18EC, C8, C2, Phenyl Cyano, Diol, Amino Silica C18, C18EC, C8, C2, Phenyl Phases: Non Silica-based Florisil PR, Alumina A, Alumina B, Alumina N, Carbon Florisil PR, Alumina A, Alumina B, Alumina N, Carbon Phases: Specialty EVIDEX for drugs of abuse testing Dual Phases 4

5 Cross Reference of Comparable Phases by Manufacturer Different chemistries and manufacturing processes create sorbents that exhibit differences in selectivity, so there is no universal equalivent for every application. However, the performance of products can be similar in many applications. This table provides suggestions for using Agilent SampliQ products in comparison to products from other manufacturers. Polymers If you are using... Try this... Phenomenex strata Waters Oasis Varian Bond Elut Plexa Supelco Supelclean/Discovery Agilent SampliQ stratax HLB Plexa OPT SDB-L ENV ENVI-ChromP ENV PS-DVB strata-xc MCX Plexa PCX SCX MAX SAX strata-x-cw WCX WCX strata-x-aw WAX WAX Silica-Based and Other Sorbents If you are using... Try this... Phenomenex strata Waters Sep-Pak Varian Bond Elut Supelco Supelclean/Discovery Agilent SampliQ C18-E tc18 C18 ENVI-18, DSC-C18, LC-18 C18EC C18-U C18 C18OH C18 C8 C8 C8 DSC-8, Envi-8, LC-8 C8 tc2 C2 C2 Phenyl (PH) PH DSC-Ph, LC-Ph Phenyl Screen-C Certify-I Evidex DSC-MCAX C8/SCX Si-1 Silica SI DSC-Si, LC-SI Silica FL-PR Florisil FL LC and ENVI Florisil Florisil PR NH 2 Amino Propyl NH 2 DSC-NH 2, LC-NH 2 Amino 2OH DSC-Diol, LC-Diol Diol CN Cyano Propyl CN-U DSC-CN, LC-CN Cyano Alumina A, B, N Al A, B, N LC-Alumina A, B, N Alumina A, B, N SAX AccellPlus QMA SAX DSC-SAX, LC-SAX Si-SAX SCX AccellPlus CM SCX DSC-SCX, LC-SCX Si-SCX Carbon ENVI-Carb Carbon ENVICarb-II/NH 2 Carbon/Amino ENVICarb-II/PSA Carbon/PSA 5

6 Agilent SampliQ Polymeric SPE Sorbents Simplify your SPE method development and improve your results. The polymeric sorbents used for these products significantly reduce matrix interferences, resulting in improved analytical sensitivity and data quality. Agilent SampliQ polymer sorbents in cartridge and 96-well plate formats also offer these key advantages: High retention, outstanding recovery, and excellent reproducibility High sorbent robustness: if cartridges accidentally go dry during the SPE process, you will not risk losing analytes due to poor recovery No bleeding bonded phases or other leachables that can contaminate your valuable extracts Compatibility with most organic solvents and aqueous solutions over a ph range of 0 to 14 Spherical particles and narrow size distribution, which ensure reproducible flow characteristics Improved detection limits and reduced resin volumes Unlike silica-based sorbents, there are no residual silanol groups which can affect the recovery of basic compounds If the chemical properties of your target analytes vary between acids, neutrals, and bases, a mixed mode retention mechanism will allow you to develop one method using one sorbent. SampliQ Method Development Kits Description Ion exchange method development kit for acids Contains 10 cartridges each SAX, WAX, OPT; 1 ml, 30 mg Ion exchange method development kit for bases Contains 10 cartridges each SCX, WCX, OPT; 1 ml, 30 mg Polymeric ion exchange method development 96-well plate Contains 24 wells each (3 rows of 8 wells) of SCX, WCX, SAX, WAX Part No

7 POLYMER Agilent SampliQ Polymeric A/N/B Method Strong Acids Weak Bases pka < 1 pka 2-10 Neutral Compounds pka 3-10 Weak Acids pka > 10 Strong Bases pka 2-8 Analyte: Log P < 1.5 Log P > 1.3 Log P < 1.5 Use SampliQ WAX Use SampliQ SCX Use SampliQ OPT Use SampliQ SAX Use SampliQ WCX Prepare Sample for SPE Condition: 0.1% Formic Acid in Methanol Methanol Methanol Equilibrate: 2% Formic Acid in Water Water Water Load: Prepared sample Prepared sample Prepared sample Wash: 2% Formic Acid 5-10% Methanol in Water 5% NH 4 OH Elute 1: Weak Acids Methanol or 100% Methanol 0.1% Formic Acid 100% Methanol in Methanol Weak Bases Elute 2: 5% NH 4 OH in Methanol 2% Formic Acid in Methanol Strong Acids Weak Bases Neutrals Weak Acids Strong Bases 7

8 POLYMER Agilent SampliQ OPT: Your most versatile SPE Option SampliQ OPT Agilent SampliQ Optimized Polymer Technology (OPT) cartridges are appropriate for a broad range of samples, including weak acids, neutrals, and weak bases. SampliQ OPT utilizes a novel polyamide chemistry (patent pending) that makes OPT cartridges compatible with water and most organic solvents, as well as acidic and basic solvents with a ph level of 0 to 14. This resin technology also exhibits retention for both polar and non-polar compounds, based on its combined hydrophilic and lipophilic characteristics. The predominant retention mechanism in OPT cartridges is reversed phase, which simplifies method development and compatibility for both GC and LC separations. For hydrophilic compounds, try modifying the load and wash solvents by adjusting the ph to match the pka of the poorly retained compound. For basic compounds that are too strongly retained, try adding 0.1% formic acid to the methanol eluent. Unlike silica-bonded phases, polymeric SampliQ OPT sorbents provide excellent recovery and reproducibility even if they inadvertently dry out during the conditioning step. SampliQ OPT R N R Polyamide chemistry O R Description Unit 30 micron Part No. 60 micron Part No. 30 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 6 ml 30/pk mg, 6 ml 30/pk well plate, OPT, 10 mg, 2 ml well plate, OPT, 30 mg, 2 ml

9 POLYMER A Retention Comparison of Compounds Extracted with Wet and Dry Agilent SampliQ OPT Cartridges Dry Wet % Recovery Acetaminophen Propranolol hydrochloride Brompheniramine Mianserin Doxepin hydrochloride Fluoxetine Dihydroxy naphthalene In this study, you can see that SampliQ OPT cartridges yield the same precise recovery and reproducibility (RSDs indicated with error bars) under both wet and dry conditions. For complete details, refer to SampliQ OPT Technical Note (Agilent publication EN). Purity Comparison of Agilent SampliQ OPT Polymeric Sorbent to Competitive Polymeric Sorbents. MS Response Internal Standards 7000 Competitor SampliQ OPT Time A study of cleanliness of blank extracts by GC/MS between Agilent SampliQ OPT versus a competitive SPE polymeric sorbent with hydrophilic-lipophilic balance, shows that Agilent s manufacturing process yields cleaner materials, which contribute to cleaner sample extracts for analysis. 9

10 POLYMER Agilent SampliQ Strong Ion Exchange sorbents provide selective retention of strong acids and bases in challenging samples. SampliQ SCX Agilent's mixed mode SampliQ Strong Cation Exchange (SCX) polymeric resin is a sulfonic acid-modified divinyl benzene polymer with both ion exchange and reverse phase retention properties. As a result, the SampliQ SCX resin exhibits excellent retention for both basic and neutral compounds over a wide range of hydrophilicity (log P). The resin is also resistant to a wide variety of solvents, is stable in ph ranges from 0 to 14, and is water-wettable. The average ion exchange capacity for the SCX resin is 1000 μmole/g. SampliQ SCX R 1 R 2 Sulfonic acid-modified divinyl benzene polymer SO 3 - Description Unit 30 micron Part No. 60 micron Part No. 30 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 6 ml 30/pk well plate, SCX, 30 mg, 2 ml For Silica SCX Phase, see page

11 POLYMER Agilent 7000 Series Triple Quadrupole GC/MS and 5975C Series GC/MSD Here, neutral compounds are recovered in the methanol eluent, while basic compounds are recovered in the 3% ammonium hydroxide eluent. % Recovery Atenolol Quinidine Haloperidol Mianserin Brompheniramine Fluoxetine Propranolol Doxepin Di-OH naphth Acetaminophen In this example, the general protocol is used to remove acidic and neutral interferences and to recover basic compounds. The same protocol can be used to recover neutral compounds (blue bars) in the methanol eluent and basic compounds (green bars) in the second eluent (3% ammonium hydroxide in methanol). Keep in mind that you can achieve higher selectivity for basic compounds by changing the ph of the load and wash solutions. For complete details, refer to SampliQ SCX Technical Note (Agilent publication EN) or see general protocol on page For a complete listing of available SampliQ application and technical notes, visit 11

12 POLYMER SampliQ SAX The Agilent SampliQ Strong Anion Exchange (SAX) polymeric resin is a mixed mode, quaternary amine divinyl benzene polymer that displays both anion exchange and reversed phase behavior. As a result, the SampliQ SAX resin exhibits excellent retention for both acidic and neutral compounds over a wide range of hydrophilicity (log P). In addition, the SampliQ SAX resin is inert to a wide variety of solvents, is water-wettable, and is stable in ph ranges from 0 to 14. The average ion exchange capacity for the SAX resin is 90 μmole/g. SampliQ SAX Description Unit 30 micron Part No. 60 micron Part No. R 3 N + R 1 R 2 Quaternary amine divinyl benzene polymer 30 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 6 ml 30/pk well plate, SAX, 30 mg, 2 ml For Silica SAX Phase, see page

13 POLYMER These charts illustrate two recoveries using SampliQ SAX. In the top chart, the identified compounds are eluted in groups using different eluents. However, for analyses that require retention of all of these compounds, a general protocol that combines eluents can be used to retain them all, as the second chart illustrates. Recovery by Eluent Fraction on Agilent SampliQ SAX Cartridges. % Recovery Methanol 2% Formic Acid in Methanol 0 Salicylic acid Secobarbital Nortriptyline Ketoprofen Naproxen Ibuprofen Here, neutral compounds are recovered in the methanol eluent, while acidic compounds are recovered in the acidified methanol eluent (2% formic acid). Recovery and Reproducibility of Acid and Neutral Compounds on Agilent SampliQ SAX Cartridges / / / / / /- 1.3 % Recovery Salicylic acid Secobarbital Nortriptyline Ketoprofen Naproxen Ibuprofen In this example, a general protocol was used to remove basic and neutral interferences and to recover acidic compounds. The same protocol can be used to recover neutral compounds in one eluent and acidic compounds in the second eluent. Keep in mind that you can achieve higher selectivity for acidic compounds by changing the ph of the load and wash solutions. For complete details, refer to SampliQ SAX Technical Note (Agilent publication EN), or see general protocol on page 7. 13

14 POLYMER Agilent SampliQ Weak Ion Exchange sorbents provide selective retention of strong acids and bases in challenging samples. SampliQ WCX Agilent SampliQ WCX is designed to retain and release strong bases such as quaternary amines. The chemical functionality is a carboxylic acid in its neutral form. The average ion exchange capacity for this sorbent is 750 μmol/g. SampliQ WCX R OH Carboxylic acid functionality in hydrogen form R O Description Unit 30 micron Part No. 60 micron Part No. 30 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 6 ml 30/pk well plate, WCX, 30 mg, 2 ml SampliQ WAX Agilent SampliQ WAX is designed to retain and release strong acids such as sulfonates. The chemical functionality is a neutral amine with an average ion exchange capacity of 670 μmol/g. R CH 2 NH 2 Neutral amine functionality R SampliQ WAX Description Unit 30 micron Part No. 60 micron Part No. 30 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 6 ml 30/pk well plate, WAX, 30 mg, 2 ml

15 POLYMER Agilent SampliQ DVB sorbents provide selective retention of hydrophobic compounds in challenging samples. SampliQ DVB SampliQ DVB SPE cartridges contain a high-purity, 100% divinylbenzene resin that delivers greater sample capacity and is more retentive than either C18 silica or PS-DVB resin for neutral compounds. Its strong hydrophobic character promotes superior binding for non-polar analytes and hydrophobic compounds. The SampliQ DVB resin is compatible with most solvents used in SPE and can withstand ph values from 0 to 14, giving you more flexibility to develop loading, washing and elution conditions. SampliQ DVB 30 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 6 ml 30/pk Divinylbenzene resin Agilent SampliQ PS-DVB sorbents are ideal for extracting polar compounds from aqueous solutions. SampliQ PS-DVB SampliQ PS-DVB is a highly cross-linked polystyrene-divinylbenzene (PS-DVB) copolymer with a high surface area (600 m2/g) and high capacity. The nonselective characteristic of this sorbent is useful for screening applications where a broad range of analytes is to be extracted. The cartridge design has been optimized for phenol retention in aqueous solutions, which typically has low and irreproducible recoveries. [-CH - CH 2 - CH - CH 2 - CH - CH 2 -] n SampliQ PS-DVB [-CH - CH 2 C - CH 2 - CH - CH 2 -] n 500 mg, 6 ml 30/pk mg, 6 ml 30/pk Polystyrene-divinylbenzene 15

16 POLYMER SampliQ 96-Well Plates Agilent SampliQ SPE is available in a convenient 96-well plate format for high-throughput applications such as pharmaceutical method development. The most popular polymeric sorbents are available in various particle sizes depending on your sample viscosity and flow rate needs. Agilent's 96-well plates are manufactured with the same high standards as our SPE cartridges. The 96-well plates are vacuum packed to preserve the integrity of the plate prior to use. Each plate is packaged to avoid any damage to the plate or tips. SampliQ 96-Well Plates Description 30 micron Part No. 60 micron Part No. 96-well plate, OPT, 10 mg, 2 ml well plate, OPT, 30 mg, 2 ml well plate, SCX, 30 mg, 2 ml well plate, WCX, 30 mg, 2 ml well plate, SAX, 30 mg, 2 ml well plate, WAX, 30 mg, 2 ml

17 Agilent SampliQ Silica SPE Silica-based SPE products have been used for many years, and continue to be used reliably in many methods. All SampliQ silica-based products are based on irregular silica gel (silica) particles and have an average particle size of 45 μm and nominal pore diameter of 60Å. These particles reduce pressure drop, increase flow reproducibility and, in some cases, allow replacement of vacuum manifolds with gravity-driven flow. Agilent SampliQ Reversed Phase (Non-Polar) Silica SPE Reversed phase sorbents are non-polar, and will be used to retain (extract) non-polar analytes. For reversed phase sorbents, retention decreases as the solvent becomes more non-polar. SampliQ C18 SampliQ C18 ODS products are based on bonded, reversed phase (octadecylsilane), irregular, silica gel (silica) particles. This non-polar, non-endcapped sorbent is tri-functionally bonded, enhancing the retention of basic compounds compared with the corresponding endcapped sorbent. It is recommended as a general purpose SPE phase for both polar and non-polar analytes. SampliQ C18 has a 24% carbon loading. SampliQ C mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 3 ml 50/pk mg, 6 ml 30/pk mg, 6 ml 30/pk Bulk 25 g bottle Si O Si (CH 2 ) 17 CH 3 O Si OH Structure of octadecylsilane (C18) covalently bonded to the surface of silica particle; trifunctional bonding links remaining ODS bonds to the silica particle 17

18 SILICA Si O Si (CH 2 ) 17 CH 3 O Si O Si(CH 3 ) 3 Structure of C18 silane and trimethyl silyl endcapping group, covalently bonded to the surface of a silica particle SampliQ C18EC Endcapped SampliQ C18EC products are based on bonded, endcapped, reversed-phase octadecylsilane (ODS) silica gel particles. The non-polar sorbent is endcapped (EC), reducing polar secondary interactions associated with surface silanol groups. Non-polar analytes should be more strongly retained compared with non-endcapped SampliQ C18 products. SampliQ C18EC has a 25% carbon loading. SampliQ C18EC 100 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 3 ml 50/pk mg, 6 ml 30/pk mg, 6 ml 30/pk Bulk 25 g bottle Si O Si (CH 2 ) 7 CH 3 O Si OH Structure of octyl (C8) silane, covalently bonded to the surface of a silica particle SampliQ C8 Octyl SampliQ C8 Octyl products are based on bonded, reversed phase (octylsilane), irregular, silica gel (silica) particles. This non-polar, non-endcapped sorbent is recommended as a general purpose SPE phase for non-polar analytes. For basic analytes, octyl sorbents often can increase the extraction efficiency and enhance their purity. SampliQ C8 Octyl has a 15% carbon loading. SampliQ C8 Octyl 100 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 3 ml 50/pk mg, 6 ml 30/pk Bulk 25 g bottle

19 SILICA SampliQ C2 Ethyl SampliQ C2 Ethyl SPE products are manufactured using a trifunctional silane bonded to irregular, silica gel (silica) particles. They are not endcapped, allowing additional polar interactions with surface silanol groups. The short chain ethyl group provides less retention than the longer C8 and C18 chains, where retention is primarily based on non-polar interactions. The stronger interactions of this phase with basic and polar analytes can provide additional extraction selectivity. O Si Si O OH Si CH 2 CH 3 SampliQ C2 Ethyl Structure of ethyl (C2) silane, covalently bonded to the surface of a silica particle 100 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 3 ml 50/pk mg, 6 ml 30/pk mg, 6 ml 30/pk SampliQ Phenyl SampliQ Phenyl SPE products exhibit additional polar secondary interactions (pi-pi), which can enhance retention of aromatic compounds. They exhibit a different selectivity compared with the octadecyl and octyl phases when both aromatic and non-aromatic compounds are being extracted. O Si Si O OH Si SampliQ Phenyl 100 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 3 ml 50/pk Bulk 25 g bottle Structure of phenyl silane, covalently bonded to the surface of a silica particle 19

20 SILICA Agilent SampliQ Normal Phase (Polar) Silica SPE Normal phase sorbents are polar and used to retain (extract) polar analytes. For normal phase sorbents, retention decreases as the solvent becomes more polar. O Si Si OH OH SampliQ Silica The primary interaction available through SampliQ Silica SPE is polar (e.g. hydrogen bonding). The silanol groups are ionizable, so it can be used as a weak cation exchanger at intermediate ph values. SampliQ Silica Structure of silanol groups on the surface of a silica particle 100 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 3 ml 50/pk mg, 6 ml 30/pk mg, 6 ml 30/pk Bulk 25 g bottle SampliQ Cyano (CN) Si O Si O OH Si (CH 2 ) 3 CN SampliQ Cyano (CN) SPE products are polar, bonded sorbents that can exhibit both polar and non-polar interactions. They can be used as non-polar sorbents for extraction of both polar and non-polar molecules from aqueous samples, and for extraction of polar molecules from relatively non-polar solvents. Structure of cyanopropylsilane (CN), covalently bonded to the surface of a silica particle SampliQ Cyano (CN) 100 mg, 1 ml 100/pk mg, 6 ml 30/pk mg, 6 ml 30/pk

21 SILICA SampliQ Diol The SampliQ Diol SPE is a weakly polar, bonded sorbent that can exhibit both polar and weak non-polar interactions, depending on the cartridge preparation and sample matrix. SampliQ Diol Si O Si O OH Si (CH 2 ) 3 OCH 2 CH CH 2 OH OH 500 mg, 3 ml 50/pk Structure of diol silane, covalently bonded to the surface of a silica particle SampliQ Amino (NH 2 ) SampliQ Amino (NH 2 ) SPE products consist of a dual purpose sorbent that can act either as a polar phase or weak anion exchanger. When conditioned with a non-polar solvent, e.g., hexane, they can hydrogen bond with any molecule containing -OH, -NH, or -SH functional groups. In an aqueous environment with ph 7.8 or less, they can function as a weak anion exchanger. Si O Si (CH 2 ) 3 NH 2 O Si OH SampliQ Amino (NH 2 ) 100 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 3 ml 50/pk mg, 6 ml 30/pk mg, 6 ml 30/pk Bulk 25 g bottle Structure of aminopropyl (NH 2 ) silane, covalently bonded to the surface of a silica particle 21

22 SILICA Agilent SampliQ Ion Exchange Silica SPE Ion exchange phases are more dependent on ph, ionic strength, and counter-ion strength than on solvent strength. These phases depend on ionic interactions as the primary retention mechanism. Si O Si O Si OH (CH 2 ) 2 SO 3 - H + SampliQ Silica Strong Cation Exchange (Si-SCX) SampliQ Si-SCX SPE products are strong cation exchange sorbents used to extract positively charged basic compounds. This benzene-sulphonic acid-based sorbent has significant non-polar secondary interactions, with nominal capacity 0.3 meq/g. Structure of SCX silane, covalently bonded to the surface of a silica particle SampliQ Silica Strong Cation Exchange (Si-SCX) 100 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 3 ml 50/pk mg, 6 ml 30/pk mg, 6 ml 30/pk

23 SILICA SampliQ Silica Strong Anion Exchange (Si-SAX) SampliQ Si-SAX SPE products are strong anion sorbents that are used to extract compounds capable of carrying a negative charge from both aqueous and non-aqueous solutions. They are ideally suited to the extraction of weak acids at phs above their pka. The nominal capacity is 0.6 meq/g. SampliQ Silica Strong Anion Exchange (Si-SAX) Si O Si (CH N + (CH 3 ) 3 CI 2 ) 3 O Si OH Structure of SAX silane, covalently bonded to the surface of a silica particle 100 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 3 ml 50/pk mg, 6 ml 30/pk mg, 6 ml 30/pk Bulk 25 g bottle

24 Additional Agilent SampliQ SPE Phases The following SPE phases have varying degrees of polarity and surface acidity or basicity. They are primarily used to retain polar analytes. For these phases, solvent retention generally decreases as the solvent becomes more polar. SampliQ Florisil PR SampliQ Florisil PR is a selective synthetic magnesia-silica adsorbent, specially processed to give consistent results when used for column cleanup and separation of chlorinated pesticide residues prior to identification and measurement of the pesticide by gas, thin layer, or paper chromatography. SampliQ Florisil PR 200 mg, 3 ml 50/pk mg, 3 ml 50/pk mg, 6 ml 30/pk mg, 6 ml 30/pk Bulk 25 g bottle SampliQ Alumina A (acidic) SampliQ Alumina A sorbents, with μm particle size, can adsorb molecules by interaction with the aluminum metal center, hydrogen bonding with the surface hydroxyl groups, or ion exchange if the surface carries a charge. Acid washing results in a surface with decreased capacity for basic compounds. SampliQ Alumina A 500 mg, 3 ml 50/pk mg, 6 ml 30/pk Bulk 25 g bottle

25 ADDITIONAL PHASES SampliQ Alumina B (basic) SampliQ Alumina B sorbents, with μm particle size, can adsorb molecules by interaction with the aluminum metal center, hydrogen bonding with the surface hydroxyl groups, or ion exchange if the surface carries a charge. Washing with a basic solution results in a net negative charge, allowing retention of certain compounds as cations on the surface or by specific interaction with the center. SampliQ Alumina B 500 mg, 3 ml 50/pk mg, 6 ml 30/pk Bulk 25 g bottle SampliQ Alumina N (neutral) SampliQ Alumina N sorbents, with μm particle size, can adsorb molecules by interaction with the aluminum metal center, hydrogen bonding with the surface hydroxyl groups, or by ion exchange if the surface carries a charge. The neutralized surface allows interaction with compounds whose heteroatoms are electronegative (e.g., N, O, P, S) or with an electron-rich, highly aromatic structure. SampliQ Alumina N 500 mg, 3 ml 50/pk mg, 6 ml 30/pk Bulk 25 g bottle

26 ADDITIONAL PHASES SampliQ Carbon SampliQ Carbon (graphitized) sorbents exhibit high affinity for organic polar and non-polar compounds from both non-polar and polar matrices, when used in reversed phase conditions. Because carbon is non-porous, it allows for rapid processing, and the adsorption does not require analyte dispersion into solid phase pores. SampliQ Carbon 100 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 6 ml 30/pk Bulk 25 g bottle SampliQ C8/Si-SCX Mixed Mode SampliQ Mixed Mode Reversed Phase SPE products consist of an alkyl phase (C8) and a strong cation exchange phase (Si-SCX) in an optimized ratio that provides a dual retention mechanism. The C8 functionality interacts with the hydrophobic portions of an analyte while the Si-SCX functionality interacts with the protonated amine portion. The SampliQ mixed mode phase is non-endcapped which gives some added interaction between residual silanols and polar analytes helping to provide added retention characteristics. It is particularly useful for polar pharmaceutical compounds which are retained by a mixed-mode mechanism. SampliQ C8/Si-SCX Mixed Mode 100 mg, 1 ml 100/pk mg, 3 ml 50/pk mg, 3 ml 50/pk mg, 6 ml 30/pk mg, 6 ml 30/pk

27 Agilent SampliQ Specialty SPE Evidex SPE Cartridges Effective sample preparation is an important step in building compelling evidence in drugs-of-abuse cases. The Evidex SPE cartridge suitable for all necessary methods supports the kind of reliable, accurate separation that you need: Cartridge designed for SAMHSA (Substance Abuse and Mental Health Services Administration) drug classes: Amphetamine/Methamphetamine, PCP (angel dust), Benzoylecgonine (cocaine), Codeine/Morphine, THC-COOH (marijuana) Accurate, reproducible results (<5% RSD) Tested to ensure lot-to-lot reproducibility, high recovery, and clean extracts with low background Proprietary mixed phase bonding chemistry Evidex SPE Cartridges 200 mg, 3 ml 50/pk mg, 6 ml 30/pk For information on the Agilent J&W Evidex GC columns for Drugs of Abuse confirmation, please visit 27

28 SPECIALTY SPE SPE Cartridges (for Schenck variation of QuEChERS method) This dual phase SPE cartridge removes high levels of pigments and sterols from extraction solvent. Based on the Schenck method, it allows for the recovery of planar or polar organic pesticides when using a 3:1 acetone:toluene mix. SPE Cartridges (for Schenck variation of QuEChERS method) SampliQ Carbon/PSA 250 mg Carbon/500 mg PSA, 6 ml 30/pk mg Carbon/500 mg PSA, 6 ml 30/pk SampliQ Carbon/Amino 500 mg Carbon/500 mg Amino, 6 ml 30/pk

29 SPECIALTY SPE SampliQ Bulk Sorbents SampliQ sorbents are available in bulk, along with a selection of reservoirs and frits, for those who wish to pack their own SPE cartridges or to perform "flash" chromatography. To investigate a new sample preparation technique, see QuEChERS on page 30. SampliQ Bulk Sorbents C18 25 g bottle C18EC 25 g bottle g bottle C8 Octyl 25 g bottle Graphitized Carbon Black (GCB) 25 g bottle Phenyl 25 g bottle Silica 25 g bottle Amino (NH 2 ) 25 g bottle Si-SAX 25 g bottle Alumina A (acidic) 25 g bottle Alumina B (basic) 25 g bottle Alumina N (neutral) 25 g bottle Florisil PR 25 g bottle PSA (Primary Secondary Amine) 25 g bottle g bottle

30 QuEChERS These sorbents are available for use with the QuEChERS method, specifically for analyzing pesticide residues in fruits and vegetables. The method was developed by chemists from the US Department of Agriculture and the CVUA Laboratory in Stuttgart, Germany. QuEChERS is an acronym for "Quick, Easy, Cheap, Effective, Rugged and Safe." Information about the method can be found at QuEChERS Extraction Kits Step 1: Extraction Adding solvent and salts to a small (10 g or 15 g) comminuted fruit or vegetable sample enables you to extract the pesticides of interest into the organic layer. However, adding a food sample with a high percentage of water directly to the salts may create an exothermic reaction that can affect your analyte recoveries. Choose the extraction salt packet below based on your method of analysis, AOAC or EN. The buffered extraction salts are amenable for more liable pesticides. QuEChERS Extraction Kits Extraction Salt Packet Content Extraction Kits (Extraction Salt Packets with 50 ml Centrifuge Tubes) Extraction Salt Packets (No Centrifuge Tubes) Description Unit Part No. Unit Part No. Buffered QuEChERS extraction tubes 6 g MgSO 4, 50/pk /pk AOAC Method , for use with 15 g samples 1.5 g NaAcetate 200/pk With Ceramic Homogenizers 100/pk CH Buffered QuEChERS extraction tubes EN Method 15662, for use with 10 g samples 4 g MgSO 4, 1 g NaCl, 1 g NaCitrate, 0.5 g disodium citrate sesquihydrate With Ceramic Homogenizer 100/pk CH Original QuEChERS method (non-buffered) extraction tubes for use with 10 g samples 4 g MgSO 4, 1 g NaCl With Ceramic Homogenizer 100/pk CH Original QuEChERS method (non-buffered) extraction tubes for use with 15 g samples 6 g MgSO 4, 1.5 g NaCl QuEChERS extraction tubes for acrylamides* 1 4 g MgSO 4, 0.5 g NaCl 50/pk /pk /pk /pk /pk /pk /pk /pk /pk *Katerina Mastovaka and Steven J. Lehotay have done work to extend the scope of QuEChERS beyond fruits and vegetables (1), using it to extract acrylamides in potato chips and other fried foods. 1"Rapid Sample Preparation Method for LC-MS/MS or GC-MS Analysis of Acrylamides in Various Food Matrices", J. Agric. Food Chem, 2006, 54,

31 QUECHERS QuEChERS Dispersive Kits Step 2: Dispersive SPE Clean-Up Select the Dispersive SPE kit suited to the type of food being analyzed and the method you are following. QuEChERS Dispersive Kits Kit Size Unit General fruits and vegetables: Removes polar organic acids, some sugars and lipids Fruits and vegetables with fats and waxes: Removes polar organic acids, some sugars, more lipids and sterols Pigmented fruits and vegetables: Removes polar organic acids, some sugars and lipids, and carotinoides and chlorophyll; not for use with planar pesticides Highly pigmented fruits and vegetables: Removes polar organic acids, some sugars and lipids, plus high levels of carotinoides and chlorophyll; not for use with planar pesticides AOAC Method Kit Contents Part No. 2 ml 100/pk 50 mg PSA 150 mg MgSO CH 15 ml 50pk 400 mg PSA 1200 mg MgSO CH 2 ml 100/pk 50 mg PSA 50 mg C18EC 150 mg MgSO CH 15 ml 50/pk 400 mg PSA 400 mg C18EC 1200 mg MgSO CH 2 ml 100/pk 50 mg PSA 50 mg GCB 150 mg MgSO CH 15 ml 50/pk 400 mg PSA 400 mg GCB 1200 mg MgSO CH European Method EN Kit Contents Part No. 25 mg PSA 150 mg MgSO CH 150 mg PSA 900 mg MgSO CH 25 mg PSA 25 mg C18EC 150 mg MgSO CH 150 mg PSA 150 mg C18EC 900 mg MgSO CH 25 mg PSA 2.5 mg GCB 150 mg MgSO CH 150 mg PSA 15 mg GCB 900 mg MgSO CH 2 ml 100/pk 25 mg PSA 7.5 mg GCB 150 mg MgSO CH 15 ml 50/pk 150 mg PSA 45 mg GCB 900 mg MgSO CH Part numbers ending in 'CH' indicate tubes containing ceramic homogenizers. 31

32 QUECHERS QuEChERS Dispersive Kits AOAC Method Kit Contents Kit Size Unit Part No. Fruits and vegetables 2 ml 100/pk 50 mg PSA with pigments and fats: 50 mg GCB Removes polar organic acids, some sugars 150 mg MgSO 4 and lipids, plus carotinoides and chlorophyll; 50 mg C18EC not for use with planar pesticides CH 15 ml 50/pk 400 mg PSA 400 mg GCB 1200 mg MgSO mg C18EC CH European Method EN Kit Contents Part No. Kit Size Unit Kit Contents Other Food Methods 2 ml 100/pk 25 mg C18 Removes biological matrix interferences, 150 mg MgSO 4 including hydrophobic substances (fats, lipids) and proteins CH 15 ml 50/pk 150 mg C mg MgSO CH QuEChERS Ceramic Homogenizers The same great ceramic homogenizers available in our QuEChERS Kits are also available for bulk purchase, providing excellent grinding capabilities of the samples. QuEChERS Ceramic Homogenizers Ceramic homogenizer for 50 ml tubes 100/pk Ceramic homogenizer for 15 ml tubes 100/pk Ceramic homogenizer for 2 ml tubes 200/pk

33 QUECHERS Standards for QuEChERS Products In addition to our industry-leading SampliQ QuEChERS Kits, Agilent makes your analysis easier by providing standards for the most commonly used regulatory methods, including AOAC and EN. Save time and hassle of making up standards Available for both GC and LC instruments Ready to use for QuEChERS extractions no dilutions required Standards for QuEChERS Products Description Concentration Kit Contents Part No. HPLC & GC Internal Standard, AOAC Method 1000 μg/ml Parathion-d10 (diethyl-d10), Alpha-BHC-d6 (alpha-hch-d6) QC Solution, AOAC Method 500 μg/ml Triphenyl Phosphate HPLC Internal Standard, EN Method 100 μg/ml Tris (1,3-dichloroisopropyl) phosphate, Nicarbazin GC Internal Standard, EN Method 5000 μg/ml (2,2'5,5'-tetrachlorobiphenyl), Triphenylmethane, Tris (1,3-dichloroisopropyl) phosphate QC Surrogate for GC Standard, EN Method 500 μg/ml 1000 μg/ml (2,2',3,4,4',5'-hexachlorobiphenyl) Anthracene-d10 GC Standard Mix, EN Method 100 μg/ml Malathion, Methyl parathion, Parathion (ethyl), Chlorpyriphos, Fenitrothion, Dichlorvos, Deltamethrin, Chlorpyriphos-methyl, Heptachlor, Bromopropylate, Gamma-HCH, Aldrin, Dieldrin, Disulfoton, Fenvalerate, Procymidone, Hexachlorobenzene, Lamda-cyhalothrin, 4,4'-DDT, Endosulfan I, Endosulfan II, Endosulfan sulfate, 4.4'-DDE, 4,4,-DDD, Alpha-BHC, Beta-BHC For more information on QuEChERS, download the brochure at 33

34 QUECHERS QuEChERS Bulk Sorbents and Salts If you prefer to pack your own tubes for QuEChERS, these bulk sorbents and salts provide high-quality materials for that purpose. QuEChERS Bulk Sorbents and Salts Magnesium Sulfate 100 g bottle Sodium Acetate 100 g bottle Sodium Chloride 100 g bottle PSA (Primary Secondary Amine) 25 g bottle g bottle C18EC 25 g bottle g bottle Graphitized Carbon Black (GCB) 25 g bottle Si-SAX 25 g bottle Comparison of Agilent SampliQ QuEChERS AOAC General Fruits and Vegetables Dispersive SPE Kits by LC/MS/MS ml 8 ml % Recovery Methamidophos Acephate Pymetrozine Carbendazim Imidacloprid Thiabendazole Dichlorvos Propoxur Thiophanate methyl Carbaryl Ethoprophos Penconazole Cyprodinil Dichlorfluanid Kresoxim methyl Tolyfluanid In the above example, the two different sample aliquot sizes specified by the AOAC method are compared using the Agilent SampliQ QuEChERS General Fruits and Vegetables Dispersive SPE Kit. The results show that comparable recoveries were obtained across all analytes. 34

35 MANIFOLDS AND ACCESSORIES Manifolds and Accessories Agilent manifolds and accessories complement the quality of SampliQ sorbents. Flexible configurations and availability as complete assemblies or individual components mean that the user has the necessary capability at any stage from method development to high-throughput operation. Vacuum Manifold Processing Stations Both 12- and 20-position processing stations available Tank constructed of chemically resistant, vacuum safe glass Ultra high molecular weight polyethylene lid ensures excellent solvent resistance Vacuum gauge with coarse and fine control valves for monitoring and adjustment of vacuum levels, plus a safety release valve Choice of height adjustable racks to accommodate a variety of collection vessels (rack options to fit 10-, 12- and 16-mm tube diameters) Compatible with standard Luer-tipped SPE and filtration columns Individually controlled PTFE stopcocks permit flow control at each port position Clearly marked ports and racks to ensure correct positioning of collection vessels 12-port vacuum manifold processing station, Vacuum Manifold Processing Stations for SPE Cartridges Description 12-port vacuum manifold processing station Includes rack for 16 x 100 mm tubes 20-port vacuum manifold processing station Includes rack for 16 x 100 mm tubes Part No Port Vacuum Manifold Assembly, Luer plugs, Needle tips, Long stopcock valve, Ejector tool,

36 MANIFOLDS AND ACCESSORIES Replacement Parts for Vacuum Manifolds Description Part No. Common Supplies Manifold ball ring/vacuum quick release Manifold exit valve replacement kit Manifold vacuum gauge assembly with valve Port Vacuum Manifolds White cover for 12-port manifold Sealing gasket for 12-port manifold Glass chamber for 12-port manifold port rack for 13 x 75 mm tubes port rack for 13 x 100 mm tubes port rack for 16 x 75 mm tubes port rack for 16 x 100 mm tubes Port Vacuum Manifolds White cover for 20-port manifold Sealing gasket for 20-port manifold Glass chamber for 20-port manifold port rack for 13 x 75 mm tubes port rack for 13 x 100 mm tubes port rack for 16 x 75 mm tubes port rack for 16 x 100 mm tubes A full selection of adapters allows stacking cartridges for multi-step separation of or use of flexible cartridges on 12- or 20-port manifolds. Parts and Disposables for Cartridge Manifolds Manifold disposable needle tip 20/pk Manifold stainless steel needle with polypropylene coating 20/pk Manifold short valve stopcock 20/pk Manifold long valve stopcock 20/pk Manifold male luer plugs 25/pk Manifold needle tip ejector tool Cartridge stacking adapters 12/pk

37 MANIFOLDS AND ACCESSORIES Vacuum Manifolds for 96-Well Plates Can handle 96-well fixed position plates or second version to handle 96-well flexible format plate Constructed with polypropylene base and polyethylene lid Small footprint Supplied with on-off switch, vacuum gauge, and fine vacuum control valve Supplied with disposable reservoir tray to collect excess sample and wash solvents Spacer inserts can be placed into the base so that collection plates of differing heights can be processed (both deep well and standard microtiter plates), ensuring maximum penetration of the SPE plate into the collection plate and reducing well-to-well contamination Solvent resistance gasket in the manifold lid Vacuum Manifolds for 96-Well Plates Description 96-well vacuum manifold base assembly Includes base, vacuum gauge and needle valve Part No Vacuum manifolds for 96-well plates are designed to allow both convenient method development and high-throughput operation. The base accommodates fixed format 96-well plates with each well loaded with the same sorbent. Complete assembly, Replaceable parts: 1. Base assembly, Vacuum gauge, On/off valve, Needle valve, Vacuum outlet, The setup shown includes: 6. Lid for fixed well manifold, Fixed 96-well plate which is available in various sizes to meet your needs 37

38 MANIFOLDS AND ACCESSORIES Parts and Disposables for 96-Well Plate Manifolds Base O-ring, Collection plate spacer in sizes to match the collection plate used Base O-ring for 96-well plate manifold Collection plate spacer for Agilent 1 ml deep well, 12 mm Collection plate spacer for microtiter plate and Agilent 0.5 ml shallow well plate, 29 mm Collection plate spacer for most industry-standard deep well plates, 2 mm Disposable reservoir tray for 96-well manifold 25/pk well vacuum manifold base assembly Includes base, vacuum gauge and needle valve Lid for 96-fixed well vacuum manifold Lid gasket for 96-well plate manifold Luer adapters for 96-well flexible cartridge 25/pk Needle valve for 96-well manifold On/off valve for 96-well manifold Vacuum gauge for 96-well manifold Vacuum outlet (Ni plated) for 96-well manifold Sealing Mats Sealing mats help prevent sample contamination or evaporation that can occur when plates are left exposed to environmental conditions. Sealing Mats 96-well plate sealing mats, round 50/pk well plate sealing mats, square 10/pk

39 MANIFOLDS AND ACCESSORIES SampliQ Empty Reservoirs, Frits and Caps Empty reservoirs and separate frits are available if you would like to prepare your own solid phase extraction cartridges. By purchasing bulk SPE sorbents, you can pack larger or different weights of sorbent, mixed phases or any combination that you desire. The larger volume reservoirs can be used for low pressure or flash chromatography. Caps on each end will allow for safe transport of your cartridge. SampliQ Empty Reservoirs, Frits and Caps Empty SPE Cartridge, 1 ml 50/pk Empty SPE Cartridge, 3 ml 50/pk Empty SPE Cartridge, 6 ml 50/pk Empty SPE Cartridge, 70 ml 50/pk SPE Frits, 1 ml 100/pk SPE Frits, 3 ml 100/pk SPE Frits, 6 ml 100/pk SPE Frits, 70 ml 100/pk SPE caps, 1 ml 100/pk SPE caps, 3 ml 100/pk SPE caps, 6 ml 100/pk Luer caps (fit all cartridge sizes) 100/pk You need 2 frits to pack one cartridge. 39

40 A portfolio of solutions designed to give you ultimate confidence in your results. New Agilent SampliQ SPE products improve the quality of your samples, so you improve the quality of your analysis. Next-generation GC, LC and MS systems deliver all the elements for perfect chemistry. Agilent J&W Ultra Inert Capillary GC columns are individually tested with the industry's most demanding test probe and include a performance summary in each box. Agilent J&W High Efficiency Capillary GC columns let you analyze more samples, faster. Poroshell 120 HPLC columns give you the speed and performance of sub-2 μm with up to 50% less backpressure. Certified vials, liners, syringes and lamps provide extra confidence for your sensitive analyses. Over four decades of application and method expertise can lower your limits of detection (LODs) and limits of quantitation (LOQs) for a wide range of matrices. Software solutions allow you to screen for hundreds of compounds, manage large quantities of data, and preserve the integrity of your results. World-class service boosts your productivity and optimizes your resources. For more information Learn more: Buy online: Find an Agilent customer center in your country: U.S. and Canada agilent_inquiries@agilent.com Europe info_agilent@agilent.com Asia Pacific adinquiry_aplsca@agilent.com Information, descriptions, and specifications in this publication are subject to change without notice. Agilent Technologies, Inc Printed in the USA May 1, EN