Journal
JOURNAL OF AOAC INTERNATIONAL
Volume 97, Issue 6, Pages 1526-1537Publisher
AOAC INT
DOI: 10.5740/jaoacint.13-333
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Funding
- National Science Centre (Cracow, Poland) [N N204 355840]
- Ministry of Science and Higher Education (Warsaw, Poland) [IP2011 032271]
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A rapid and sensitive ultra-HPLC/MS/MS (UHPLC/MS/MS) assay method for the simultaneous determination in human urine of 22 drugs belonging to different pharmaceutical groups was developed. The drugs were extracted from urine samples and then separated on a Zorbax Rapid Resolution High Definition SB-C18 column. The mobile phase consisted of methanol and water containing formic acid with gradient elution. The chromatographic separation time was 7 min. The MS/MS detector, equipped with an electrospray ionization source, was set up in both positive and negative modes. The lower LOQs for the drugs in this method were between 0.05 and 0.60 ng/mL. Calibration curves in human urine were generated in the range of 0.05-600 ng/mL. Method validation parameters such as intraday and interday precision, accuracy, extraction recovery, stability, selectivity, dilution integrity, and carryover effect for all the compounds were within the acceptable ranges. This simple and fast method was applied successfully to study the pharmacokinetics of four selected drugs in human urine collected from patients. This UHPLC/MS/MS method offers an attractive way forward for the development of a routine rapid analysis for selected substances, particularly given the growing amount of new information about drug properties.
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