Skip to Content
Merck
CN
  • 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
Salicylic acid, ReagentPlus®, ≥99%
Sigma-Aldrich
Sodium hydroxide, BioUltra, for luminescence, ≥98.0% (T), pellets
Sigma-Aldrich
Sodium hydroxide solution, BioUltra, for molecular biology, 10 M in H2O
Sigma-Aldrich
Salicylic acid, puriss. p.a., ≥99.0% (T)
Sigma-Aldrich
Salicylic acid, ACS reagent, ≥99.0%
Sigma-Aldrich
3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
Salicylic acid, ≥99%, FG
Sigma-Aldrich
Salicylic acid, meets analytical specification of Ph. Eur., BP, USP, 99.5-100.5% (calc. to the dried substance)
Sigma-Aldrich
Methanol, purification grade, 99.8%
Sigma-Aldrich
Salicylic acid, BioXtra, ≥99.0%
Sigma-Aldrich
Sodium hydroxide solution, 1.0 N, BioReagent, suitable for cell culture
Sigma-Aldrich
Salicylic acid, suitable for plant cell culture
Sigma-Aldrich
Cyclobenzaprine hydrochloride
Sigma-Aldrich
Phenylbutazone
Sigma-Aldrich
2-Propylpentanoic acid
Sigma-Aldrich
Methanol, NMR reference standard
Supelco
Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC
Sigma-Aldrich
Methanol, ACS spectrophotometric grade, ≥99.9%
Trimethoprim, European Pharmacopoeia (EP) Reference Standard
USP
Salicylic acid, United States Pharmacopeia (USP) Reference Standard
USP
Trimethoprim, United States Pharmacopeia (USP) Reference Standard
Metronidazole, European Pharmacopoeia (EP) Reference Standard
Supelco
Residual Solvent - Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Phenylbutazone, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Valproic acid for system suitability, European Pharmacopoeia (EP) Reference Standard
Valproic acid, European Pharmacopoeia (EP) Reference Standard
Phenylbutazone, European Pharmacopoeia (EP) Reference Standard
USP
Valproic acid, United States Pharmacopeia (USP) Reference Standard