PAIN PANEL. Research and Solutions

Transcription

1 PAIN PANEL Research and Solutions

2 Pain management drug use and abuse has increased significantly in recent years. The 21 National Survey on Drug Use & Health (NSDUH) reports that 17.3% of first-time drug users used pain relievers to initiate drug use, second only to marijuana. NSDUH also reported the number with pain reliever dependence or abuse increased (from 1. million to 1.9 million) while abuse or dependence on marijuana and cocaine stayed the same or went down during the period of This increase in pain management drug use and abuse has led to an increased demand for more accurate and sensitive testing methods. Advanced analytical techniques such as LC/MS/ MS have been an essential part in improving laboratory testing. Phenomenex is committed to providing solutions for clinical laboratories that are: 1. High-throughput 2. Accurate 3. Reproducible For Research Use Only. Not for use in diagnostic procedures Phenomenex, Inc. All rights reserved.

3 TABLE OF CONTENTS Sample Preparation SPE using Strata -X-Drug B... 4 Core shell solutions for HPLC and UHPLC users Kinetex Phenyl-Hexyl... Kinetex C Fully porous solutions for HPLC and UHPLC users Luna PFP(2)... 7 Gemini NX-C Ordering Information

4 SPE Procedures for Pain Panel Summary: Part No.: Strata -X-Drug B 33 µm Polymeric Strong Cation, 6 mg / 6 ml, Tube, 3/box 8B-S128-UCH Also available in 96-well format The solvent volumes shown below are for a 6 mg bed mass. The solvent volumes will need to be adjusted for a smaller or larger bed mass. Morphine For Urine Samples Condition: No conditioning required. Load: To 2 ml urine sample, add µl of conc. Hydrochloric acid. i. Heat at 9 C for 2 hours. ii. Add 2 ml of 2 mm Sodium acetate buffer (ph 4.). iii. Add 1 ml of 6 N KOH. Vortex. iv. Centrifuge for mins at rpm. v. Verify ph of sample is between vi. Load pre-treated sample directly onto Strata-X-Drug B sorbent. Wash: 2 ml of 1 mm Sodium acetate buffer (ph.). i. 2 ml of Methanol. ii. 2 ml of Ethyl acetate/isopropanol/ammonium hydroxide (7:2:1). Evaporate: to dryness under a stream of nitrogen at C. Reconstitute: 1 ml of 1 % Methanol. Inject: μl on HPLC / Mass Spectrometer (MS). Codeine Oxycodone H N For serum/plasma samples 1. Dilute Plasma sample 3:1 with 1 % Acetic acid. 2. Vortex 3. Centrifuge minutes at 3 g. 4. Load Directly onto Strata-X-Drug B sorbent. No conditioning required. -8. Follow the Wash, Evaporate, Reconstitute, and Inject steps above. Methamphetamine Lorazepam For saliva samples 1. Dilute Saliva sample 3:1 with 1 % Acetic acid. 2. Vortex 3. Centrifuge minutes at 3 g. 4. Load Directly onto Strata-X-Drug B sorbent. No conditioning required. -8. Follow the Wash, Evaporate, Reconstitute and Inject steps above. O N OH O O Benzoylecgonine Want help optimizing your procedure? Contact us at clinicalresearch@phenomenex.com Instant Method Development Create your Own SPE Method in under 1 minute! 4

5 Pain Control and Illicit Drug Panel Kinetex 2.6 µm Phenyl-Hexyl, x 4.6 mm 4.6e6 4.2e6 3.8e6 3.4e6 3.e6 2.6e6 2.2e6 Column: Kinetex 2.6 µm Phenyl-Hexyl Dimensions: x 4.6 mm Part No.: B-449-E Mobile Phase: A: 1 mm Ammonium formate B: Methanol with.1 % Formic Acid Gradient: Time (min) Flow Rate:.6 ml/min Injection Volume: 1 µl Temperature: 22 C Detection: MS (ambient) Detector: API % B e6 1.4e6 1.e6 6.e 2.e min App ID 2847 Retention Time (min) 6-MAM 1 (quantifier) MAM 2 (confirmation) Alprazolam Alprazolam Amphetamine Amphetamine Benzoylecgonine Benzoylecgonine Buprenorphine Buprenorphine Carisoprodol Carisoprodol Clonazepam Clonazepam Codeine Codeine Diazepam Diazepam EDDP EDDP Fentanyl Fentanyl Flunitrazepam Flunitrazepam Flurazepam Flurazepam Hydrocodone Hydrocodone Hydromorphone Hydromorphone Hydroxyalprazolam Hydroxyalprazolam Lorazepam Retention Time (min) Lorazepam MDA MDA MDEA MDEA MDMA MDMA Meperidine Meperidine Meprobamate Meprobamate Methadone Methadone Methamphetamine Methamphetamine Midazolam Midazolam Morphine Morphine Naloxone Naloxone Naltrexone Naltrexone Norbuprenorphine Norbuprenorphine Nordiazepam Nordiazepam Norfentanyl Norfentanyl Normeperidine Normeperidine Norpropoxyphene Norpropoxyphene Retention Time (min) Oxazepam Oxazepam Oxycodone Oxycodone Oxymorphone Oxymorphone PCP PCP Propoxyphene Propoxyphene Sufentanil Sufentanil Temazepam Temazepam Tramadol Tramadol MAM-d Amphetamine-d Benzoylecgonine-d Codeine-d Fentanyl-d Hydrocodone-d Hydromorphone-d Meperidine-d Methadone-d Methamphetamine-d Morphine-d Nordiazepam-d Normeperidine-d Norpropoxyphene-d PCP-d

6 Pain Control and Illicit Drug Panel Kinetex 2.6 µm C18, x 3. mm 2.e6 1.9e6 1.8e6 1.7e6 1.6e6 1.e6 1.4e6 1.3e6 1.2e6 1.1e6 1.e6 9.e 8.e 7.e 6.e.e 4.e 3.e 2.e 1.e Column: Kinetex 2.6 µm C18 Dimensions: x 3. mm Part No.: B-4462-Y Mobile Phase: A: 1 mm Ammonium formate B: Methanol with.1 % Formic Acid Gradient: Time (min) min % B 1 1 Flow Rate:. ml/min Injection Volume: 1 µl Temperature: Ambient Detection: MS/MS (ambient) Detector: API 4 App ID Oxymorphone Morphine Hydromorphone Amphetamine Methamphetamine Oxycodone MDA MDMA Codeine Naltrexone MDEA MAM Hydrocodone Benzoylecgonine Norfentanyl Tramadol Naloxone Normeperidine Meperidine Meprobamate PCP Norbuprenorphine EDDP Norpropoxyphene Clonazepam Flunitrazepam a-hydroxyalprazolam Carisoprodol Oxazepam Methadone Lorazepam Fentanyl Flurazepam Alprazolam Temazepam Propoxyphene Nordiazepam Diazepam Midazolam Sufentanil Buprenorphine Resolution of Critical Isobars Codeine/Hydrocodone 2.4e 2.e 1.e. 3.e 2.e 1.e. 1.e6 9.e 8.e 7.e 6.e.e 4.e 3.e 2.e 1.e min Morphine/Hydromorphone/Norhydrocodone min Oxymorphone/Dihydrocodeine/Noroxycodone min

7 Pain Panel Mix in Human Urine Fully Porous Solution on Luna 3 µm PFP(2).9e6.e6.e6 4.e6 4.e6 3.e6 3.e6 2.e6 Column: Luna 3 µm PFP(2) Dimensions: x 3. mm Part No.: B-4447-Y Mobile Phase: A: 1 mm Ammonium formate B: Methanol Gradient Time (min) % B Flow Rate: μl/min Temperature: 4 C Detection: MS (ambient) Detector: API 4 2.e6 1.e6 1.e6.e App ID min Morphine 286.2/ /16 Oxymorphine 32.1/ /198.1 Hydromorphone 286.2/ /128 Oxycodone 316.2/ /26 Codeine 3.1/ /11.1 Amphetamine 136.1/ /119 Naltrexone 342.2/ /12.1 Methamphetamine 1.1/ /119.2 MDA 18.1/ /128.1 Hydrocodone 3.1/ / MAM 328.1/ /1.2 MDMA 194.1/ /23.1 Naloxone 328.1/ /23.1 MDEA 28.2/ /1.2 Benzoylecgonine 29.2/ /1 Norfentanyl 233.2/ /1 Tramadol 264.2/ /42.1 Meperidine 248.2/ /174.1 Normeperidine 234.1/ /188.1 Meprobamate 219.2/ /97.1 PCP 244.3/ /19.3 Norbuprenorphine 414.3/ /16.1 EDDP 278.3/ /186.2 Fentanyl 337.2/ /188.1 Flurazepam 388.2/ /134.1 Norpropoxyphene 38.2/ /143.2 Clonazepam 316/ /214.2 Flunitrazepam 314.1/ /239.2 a-hydroxyalprazolam 32.1/ /216.1 Propoxyphene 34.2/ /91.1 Methoadone 31.2/ /1 Sufentanil 387.2/ /111 Carisoprodol 261.2/ /97.2 Oxazepam 287.1/ /269.1 Lorazepam 321/ /229.1 Midazolam 39.1/ /2.1 Temazepam 31.1/ /177.1 Nordiazepam 271.1/ /16.1 Midazolam 326.1/ /249.1 Buprenorphine 468.3/ /414.2 Diazepam 28.1/ /14 7

8 Pain Panel Opiates Fully Porous Solution on Gemini 3 µm NX-C18 1.e6 9.e 8.e 7.e 6.e.e 4.e 3.e 2.e 1.e. 1. Column: Gemini 3 µm NX-C18 Dimensions: x 2. mm Part No.: B-443-B Mobile Phase: A: 1 mm Ammonium formate B: Acetonitrile Gradient: Time (min) % B Flow Rate: μl/min Temperature: Ambient Detection: MS (ambient) min App ID e4 3.e4 2.e4 1.e Oxymorphone / Noroxycodone m 1.19e 1.e 8.e4 Codeine / Hydrocodone 6.e4 4.e4 2.e m 8.e4 6.e4 4.e4 2.e4 Morphine / Hydromorphone / Norhydrocodone m Noroxycodone Buprenorphine Buprenorphine Codeine Codeine Fentanyl Fentanyl Hydrocodone Hydrocodone Hydromorphone Hydromorphone Meperidine Meperidine Methadone Methadone Morphine Morphine Naloxone Naltrexone Norbuprenorphine Norbuprenorphine Norfentanyl Norfentanyl Oxycodone Oxycodone Oxymorphone Oxymorphone Tramadol MAM MAM Norhydrocodone

9 Kinetex Ordering Information 2.6 µm Analytical Columns (mm) SecurityGuard ULTRA Cartridges* Phases 3 x 4.6 x x x x 4.6 3/pk XB-C18 B-4496-E C-4496-E D-4496-E F-4496-E AJ-8768 C18 A-4462-E B-4462-E C-4462-E D-4462-E F-4462-E AJ-8768 C8 B-4497-E C-4497-E D-4497-E F-4497-E AJ-877 PFP A-4477-E B-4477-E C-4477-E D-4477-E F-4477-E AJ-8773 HILIC A-4461-E B-4461-E C-4461-E D-4461-E F-4461-E AJ-8772 Phenyl-Hexyl B-449-E D-449-E F-449-E AJ-8774 for 4.6 mm ID 2.6 µm MidBore Columns (mm) SecurityGuard ULTRA Cartridges* Phases 3 x 3. x 3. 7 x 3. 1 x 3. 1 x 3. 3/pk Award Recipient XB-C18 A-4496-Y B-4496-Y C-4496-Y D-4496-Y F-4496-Y AJ-877 C18 A-4462-Y B-4462-Y C-4462-Y D-4462-Y F-4462-Y AJ-877 C8 A-4497-Y B-4497-Y C-4497-Y D-4497-Y F-4497-Y AJ-8777 PFP A-4477-Y B-4477-Y C-4477-Y D-4477-Y F-4477-Y AJ-878 HILIC A-4461-Y F-4461-Y AJ-8779 Phenyl-Hexyl AJ-8781 for 3. mm ID 2.6 µm Minibore Columns (mm) SecurityGuard ULTRA Cartridges* Phases 3 x 2.1 x x x 2.1 3/pk XB-C18 A-4496-AN B-4496-AN D-4496-AN F-4496-AN AJ-8782 C18 A-4462-AN B-4462-AN D-4462-AN F-4462-AN AJ-8782 C8 A-4497-AN B-4497-AN D-4497-AN F-4497-AN AJ-8784 PFP A-4477-AN B-4477-AN D-4477-AN F-4477-AN AJ-8787 HILIC A-4461-AN B-4461-AN D-4461-AN F-4461-AN AJ-8786 Phenyl-Hexyl B-449-AN D-449-AN AJ-8788 for 2.1 mm ID 1.7 µm MidBore Columns (mm) SecurityGuard ULTRA Cartridges* Phases 3 x 3. x 3. 1 x 3. 3/pk XB-C18 A-4498-Y B-4498-Y D-4498-Y AJ-877 C18 B-447-Y D-447-Y AJ-877 C8 A-4499-Y B-4499-Y D-4499-Y AJ-8777 PFP D-4476-Y AJ-878 HILIC B-4474-Y AJ-8779 for 3. mm ID 1.7 µm Minibore Columns (mm) SecurityGuard ULTRA Cartridges* Phases 3 x 2.1 x x x 2.1 3/pk XB-C18 A-4498-AN B-4498-AN D-4498-AN F-4498-AN AJ-8782 C18 A-447-AN B-447-AN D-447-AN F-447-AN AJ-8782 C8 A-4499-AN B-4499-AN D-4499-AN F-4499-AN AJ-8784 PFP A-4476-AN B-4476-AN D-4476-AN F-4476-AN AJ-8787 HILIC A-4474-AN B-4474-AN D-4474-AN AJ-8786 Phenyl-Hexyl B-4-AN D-4-AN F-4-AN AJ-8788 for 2.1 mm ID If you are not completely satisfied with Kinetex core-shell columns, send in your comparative data to a similar product within 4 days for a FULL REFUND. NEW! SecurityGuard SecurityGuard µm Columns (mm) ULTRA Cartridges* ULTRA Cartridges* x 2.1 3/pk x x x x 4.6 3/pk XB-C18 B-46-AN AJ-8782 B-46-E D-46-E F-46-E G-46-E AJ-8768 C18 B-461-AN AJ-8782 B-46v1-E D-461-E F-461-E G-461-E AJ-8768 PFP B-462-AN AJ-8787 B-462-E D-462-E F-462-E G-462-E AJ-8773 Phenyl-Hexyl B-463-AN AJ-8788 B-463-E D-463-E F-463-E G-463-E AJ-8774 for 2.1 mm ID for 4.6 mm ID NEW! 1.3 µm Columns (mm) x 2.1 *SecurityGuard ULTRA cartridges require holder, Part No. AJ-9. C18 B-41-AN SecurityGuard ULTRA Cartridge Holder Part No. Unit Price AJ-9 ea Core-Shell Performance Enhancement Kit Part No. Unit Price AQ-8892 ea 9

10 Luna Ordering Information *SecurityGuard Analytical Cartridges require holder, Part No. KJ SecurityGuard 3 μm Microbore and Minibore Columns (mm) Cartridges (mm) Phases 3 x 2. x 2. 1 x 2. 1 x 2. 4 x 2.* PFP(2) A-4447-B B-4447-B D-4447-B F-4447-B AJ-8326 for ID: mm SecurityGuard 3 μm Narrow Bore and Analytical Columns (mm) Cartridges (mm) Phases x 3. 1 x 3. x x x x 2.* 4 x 3.* PFP(2) B-4447-Y F-4447-Y B-4447-E D-4447-E F-4447-E AJ-8326 AJ-8327 for ID: mm mm SecurityGuard μm Microbore and Minibore Columns (mm) Cartridges (mm) Phases 3 x 2. x 2. 1 x 2. 4 x 2.* If Luna analytical columns do not provide at least an equivalent separation as compared to a competing column of the same particle size, similar phase, and dimensions, return the column with comparative data within 4 days for a FULL REFUND. PFP(2) A-4448-B B-4448-B F-4448-B AJ-8326 for ID: mm μm Narrow Bore and Analytical Columns (mm) SecurityGuard Cartridges (mm) Phases x 3. 1 x 3. x x 2.* 4 x 3.* PFP(2) B-4448-Y F-4448-Y B-4448-E AJ-8326 AJ-8327 for ID: mm mm μm Analytical and Semi-Prep Columns (mm) SecurityGuard Cartridges (mm) Phases 1 x x x x 1 4 x 3.* 1 x 1 PFP(2) D-4448-E F-4448-E G-4448-E G-4448-N AJ-8327 AJ-8376 for ID: mm 9-16 mm Gemini U.S. Patent No. 7, 63, 367 If Gemini analytical columns do not provide at least an equivalent separation as compared to a competing column of similar particle size, similar phase and dimensions, return the column with comparative data within 4 days for a FULL REFUND. Ordering Information 3 µm Microbore, Minibore and Narrow Bore Columns (mm) SecurityGuard Cartridges (mm) Phases 2 x 2. 3 x 2. x 2. 1 x 2. 1 x 2. x 3. 1 x 3. 1 x 3. 4 x 2.* NX-C18 M-443-B A-443-B B-443-B D-443-B F-443-B B-443-Y D-443-Y F-443-Y AJ-8367 for ID: mm 3 µm Analytical Columns (mm) SecurityGuard Cartridges (mm) Phases x x x x x 3.* NX-C18 B-443-E D-443-E F-443-E G-443-E AJ-8368 for ID: mm µm Minibore and Narrow Bore Columns (mm) SecurityGuard Cartridges (mm) Phases 3 x 2. x 2. 1 x 2. x 3. 1 x 3. 1 x 3. 2 x 3. 4 x 2.* NX-C18 A-444-B B-444-B F-444-B B-444-Y D-444-Y F-444-Y G-444-Y AJ-8367 for ID: mm µm Analytical Columns (mm) SecurityGuard Cartridges (mm) Phases x x x x x 3.* NX-C18 B-444-E D-444-E F-444-E G-444-E AJ-8368 for ID: mm *SecurityGuard Analytical Cartridges require holder, Part No.: KJ

11 Strata-X-Drug B U.S. Patent No. 7,119,14 Strata-X-Drug B is a polymeric strong cation-exchange SPE sorbent that is designed and quality controlled with Substance Abuse and Mental Health Services Administration (SAMHSA) regulations in mind. 3 Easy to Follow Methods Methods are written for 6 mg/6 ml Strata-X-Drug B; however they can be scaled to accommodate smaller or larger sample sizes and sorbent masses. Opiates, 6-MAM, PCP, and Amphetamines* Condition: Load: No conditioning required Pre-treated urine sample Wash 1: 2 ml of 1 mm Sodium acetate buffer (ph.) Wash 2: Dry: Elute: 2 ml Methanol Marijuana Metabolites Condition: Load: 1 minutes under full vacuum 2 ml of Ethyl acetate/isopropanol/ammonium hydroxide (7:2:1) No conditioning required Pre-treated urine sample Wash 1: 2 ml of 1 mm Sodium acetate buffer (ph.) Wash 2: Dry: 2 ml of Acetonitrile/1 mm Sodium acetate buffer (ph.) (3:7) 1 minutes under full vacuum Elute: 2 ml of Ethyl acetate/isopropanol (8:1) Cocaine Metabolites Condition: Load: Wash 1: Wash 2: Dry: Elute: No conditioning required Pre-treated urine sample 2 ml of.1 N Hydrochloric acid 2 ml Methanol 1 minutes under full vacuum 2 ml of Ethyl acetate/isopropanol/ammonium hydroxide (7:2:1) * Opiates, 6-MAM, PCP, and Amphetamines can be extracted simultaneously or separately using the same SPE methodology. Strata-X-Drug B Ordering Information Format Sorbent Mass Part Number Unit Price Tube 1 mg 8B-S128-AAK 1 ml (1/box) 1 mg 8L-S128-AAK 1 ml (1/box) 3 mg 8B-S128-TAK 1 ml (1/box) 3 mg 8L-S128-TAK 1 ml (1/box) 3 mg 8B-S128-TBJ 3 ml (/box) 6 mg 8B-S128-UBJ 3 ml (/box) 6 mg 8B-S128-UCH 6 ml (3/box) 6 mg 8B-S128-UCL 6 ml (2/box) 96-Well Plate 1 mg 8E-S128-AGB 2 Plates/box 3 mg 8E-S128-TGB 2 Plates/box 6 mg 8E-S128-UGB 2 Plates/box Tab-less tube Accessories for SPE Tubes Manifolds Part No. Description Unit Price AH-623 SPE 12-Position Vacuum Manifold Set, ea complete assembly AH-624 SPE 24-Position Vacuum Manifold Set, complete assembly ea Accessories for 96-Well Plates Manifold Part No. Description Unit Price AH-89 Strata 96-Well Plate Manifold, Universal w/vacuum gauge ea Collection Plates (deep well, polypropylene) Part No. Description Unit Price AH-7192 Strata 96-Well Collection Plate, 3 µl/conical /pk AH-7193 Strata 96-Well Collection Plate, 1 ml/conical /pk AH-7279 Strata 96-Well Collectin Plate, 1 ml Round, 7 mm /pk AH-863 Strata 96-Well Collection Plate, 2 ml Square/Round-Conical /pk AH-8636 Strata 96-Well Collection Plate, 2 ml Round/Round, 8 mm /pk Sealing Mats Part No. Description Unit AH-897 Sealing Mats, Pierceable, 96-Square Well, Silicone /pk AH-8631 Sealing Mats, Pierceable, 96-Round Well 7 mm, Silicone /pk AH-8633 Sealing Mats, Pierceable, 96-Round Well 8 mm, Silicone /pk AH-7362 Sealing Tape Pad 1/pk If Strata-X SPE products do not perform as well or better than your current SPE product of similar phase, mass and size, send in your comparative data within 4 days for a FULL REFUND. Instant Method Development Create your Own SPE Method in under 1 minute! 11

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