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Simultaneous determination of carisoprodol and meprobamate in human hair using solid‐phase extraction and gas chromatography/mass spectrometry of the trimethylsilyl derivatives
Author(s) -
Kim Jin Young,
In Moon Kyo,
Paeng KiJung,
Chung Bong Chul
Publication year - 2005
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.2173
Subject(s) - chemistry , bstfa , chromatography , solid phase extraction , gas chromatography–mass spectrometry , mass spectrometry , extraction (chemistry) , metabolite , gas chromatography , trimethylsilyl , sample preparation , organic chemistry , biochemistry
Carisoprodol (CSP) is a musculoskeletal relaxant whose active metabolite is meprobamate (MPB). This drug has recently been noticed to be abused as an inexpensive alternative to illicit drugs in Korea. A method using solid‐phase extraction (SPE) and gas chromatography/mass spectrometry (GC/MS) was developed for the determination of CSP and MPB in human hair. Hair samples (30 mg) were washed with distilled water and acetone, cut into small fragments (<1 mm), incubated in 1.0 M HCl overnight at 50°C, and then adjusted to pH 6.5. The drugs were extracted from the resulting hydrolyzed solutions using a SPE column. The eluents were evaporated to dryness, then derivatized using N,O ‐bis(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% trimethylchlorosilane (TMCS) at 120°C for 30 min. The derivatized extract (1 µL) was injected into the GC/MS system. Recoveries were in the range of 91.5–93.1% for CSP and 85.5–93.0% for MPB. The linear ranges were 0.5–10.0 ng/mg for both CSP and MPB with good correlation coefficients (r 2 = 0.995). The intra‐day precision and accuracy ranged from 1.5 to 9.3% and −17.5 to 3.6%, respectively, and the inter‐day precision and accuracy ranged from 3.9 to 6.2% and −15.0 to −3.9%, respectively. The limits of detection for CSP and MPB were 0.13 and 0.12 ng/mg, respectively. The applicability of the method was proven by analyzing a hair sample from an authentic abuser. Copyright © 2005 John Wiley & Sons, Ltd.