Journal
JOURNAL OF FORENSIC SCIENCES
Volume 68, Issue 4, Pages 1352-1358Publisher
WILEY
DOI: 10.1111/1556-4029.15279
Keywords
chiral analysis; mass spectrometry; MS; SFC; supercritical fluid chromatography; zopiclone
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A supercritical fluid chromatography (SFC) method was developed for the enantiomeric analysis of ZOP, a hypnotic drug. The SFC-MS/MS method achieved the baseline separation of S-ZOP and R-ZOP within 2 minutes, and showed good precision and recovery. The quick analysis ability of this method makes it a valid option for forensic drug analysis.
Zopiclone (ZOP) is a hypnotic drug prescribed to treat insomnia. Due to the chiral nature of ZOP, the psychologically active S-form and inactive R-form need to be determined enantiomerically in a forensic drug analysis. In the present study, a supercritical fluid chromatography (SFC) method was designed with a faster analysis ability than that of previously reported techniques. The SFC-tandem mass spectrometry (SFC-MS/MS) method was optimized using a column with a chiral polysaccharide stationary phase (Trefoil CEL2). ZOP was extracted from pooled human serum using solid-phase extraction (Oasis HLB) and analyzed. The developed SFC-MS/MS method achieved the baseline separation of S-ZOP and R-ZOP within 2 min. The fit-for-purpose method validation indicated that the optimized solid-phase extraction achieved near complete recovery and approximately 70% of the matrix effect. Both the retention time and peak area showed sufficient precision. The lower and upper limits of quantification (LOQ) were 5.7 x 10(-2) ng/mL and 25 ng/mL for R-ZOP, and 5.2 x 10(-2) ng/mL and 25 ng/mL for S-ZOP. The calibration line was linear in the range from lower LOQ to upper LOQ. The stability test indicated that ZOP in serum stored in a refrigerator (4 degrees C) degraded and about 55% remained in 31 days. The quick analysis of the SFC-MS/MS method makes it a valid option for the enantiomeric analysis of ZOP.
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