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  • Fast targeted analysis of 132 acidic and neutral drugs and poisons in whole blood using LC-MS/MS.

Fast targeted analysis of 132 acidic and neutral drugs and poisons in whole blood using LC-MS/MS.

Forensic science international (2014-05-06)
Matthew Di Rago, Eva Saar, Luke N Rodda, Sophie Turfus, Alex Kotsos, Dimitri Gerostamoulos, Olaf H Drummer
ABSTRACT

The aim of this study was to develop an LC-MS/MS based screening technique that covers a broad range of acidic and neutral drugs and poisons by combining a small sample volume and efficient extraction technique with simple automated data processing. After protein precipitation of 100μL of whole blood, 132 common acidic and neutral drugs and poisons including non-steroidal anti-inflammatory drugs, barbiturates, anticonvulsants, antidiabetics, muscle relaxants, diuretics and superwarfarin rodenticides (47 quantitated, 85 reported as detected) were separated using a Shimadzu Prominence HPLC system with a C18 separation column (Kinetex XB-C18, 4.6mm×150mm, 5μm), using gradient elution with a mobile phase of 25mM ammonium acetate buffer (pH 7.5)/acetonitrile. The drugs were detected using an ABSciex(®) API 2000 LC-MS/MS system (ESI+ and -, MRM mode, two transitions per analyte). The method was fully validated in accordance with international guidelines. Quantification data obtained using one-point calibration compared favorably to that using multiple calibrants. The presented LC-MS/MS assay has proven to be applicable for determination of the analytes in blood. The fast and reliable extraction method combined with automated processing gives the opportunity for high throughput and fast turnaround times for forensic and clinical toxicology.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Metronidazole, BioXtra
Sigma-Aldrich
Papaverine hydrochloride, powder
Supelco
Metronidazole, analytical standard
Sigma-Aldrich
Trimethoprim, ≥98.5%
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Prednisolone, ≥99%
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Acetazolamide, ≥99%, powder
Sigma-Aldrich
Ipratropium bromide monohydrate, ≥98% (TLC), powder
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Sodium hydroxide solution, 1.0 N, BioReagent, suitable for cell culture
Sigma-Aldrich
Chlorothiazide, thiazide diuretic
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Metronidazole, VETRANAL®, analytical standard
Supelco
Methanol, analytical standard
Sigma-Aldrich
Salicylic acid, BioXtra, ≥99.0%
Sigma-Aldrich
Salicylic acid, suitable for plant cell culture
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Sodium hydroxide solution, BioUltra, for molecular biology, 10 M in H2O
Sigma-Aldrich
Salicylic acid, meets analytical specification of Ph. Eur., BP, USP, 99.5-100.5% (calc. to the dried substance)
Supelco
Sodium hydroxide solution, 49-51% in water, eluent for IC
Supelco
Prednisolone, VETRANAL®, analytical standard
Supelco
Trimethoprim, VETRANAL®, analytical standard
Sigma-Aldrich
Salicylic acid, ReagentPlus®, ≥99%
Sigma-Aldrich
Salicylic acid, puriss. p.a., ≥99.0% (T)
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Trimethoprim, ≥99.0% (HPLC)
Sigma-Aldrich
Methanol, anhydrous, 99.8%
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3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
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Salicylic acid, ACS reagent, ≥99.0%
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Sodium hydroxide, BioUltra, for luminescence, ≥98.0% (T), pellets
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Cyclobenzaprine hydrochloride
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Phenylbutazone
Sigma-Aldrich
Ammonia-14N, 99.99 atom % 14N
Chlorothiazide, European Pharmacopoeia (EP) Reference Standard
USP
Salicylic acid, United States Pharmacopeia (USP) Reference Standard