Rapid screening for acidic non-steroidal anti-inflammatory drugs in urine by gas chromatography-mass spectrometry in the selected-ion monitoring mode.
A rapid screening procedure is described for the simultaneous determination of various acidic non-steroidal anti-inflammatory drugs (NSAIDs) at sub-nanogram levels. The procedure involves solid-phase extraction (SPE) of NSAIDs using Chromosorb P as the adsorbent in partition mode, with subsequent single-step conversion to tert-butyldimethylsilyl (TBDMS) derivatives, followed by direct analysis by gas chromatography-mass spectrometry (GC-MS). The characteristic [M-57]+ high-mass ions constituting the base peaks in the electron-impact mass spectra of most TBDMS derivatives permitted sensitive detection of NSAIDs by GC-MS in selected-ion monitoring (SIM) mode, even in the presence of higher levels of coextracted urinary organic acids. The detection limit for SIM of each drug was in the range 0.03-0.9 pg. When applied to urine samples (250 microliters) spiked with NSAIDs, the present GC-SIM-MS method allowed simultaneous screening for various NSAIDs with good overall precision and accuracy in the range of 10-40 ng.
Kim
K R
KR
College of Pharmacy, Sunigkyunkwan University, Suwon, South Korea.
Yoon
H R
HR
D000284:Administration, Oral; D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000008:administration & dosage / Q000737:chemistry / Q000652:urine*; D002940:Circadian Rhythm; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D016014:Linear Models; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
D000894:Anti-Inflammatory Agents, Non-Steroidal