HPLC-MS／MS同时检测全血中佐匹克隆、唑吡坦和扎来普隆

目的建立全血中佐匹克隆、唑吡坦和扎来普隆的液相色谱一四级杆飞行时间串联质谱联用同时检测方法。方法采用液液萃取进行提取,提取物以ZorbaxEclipsePlusC18（2．1×50mm,1．8fire）色谱柱分离,以10mmol／L甲酸铵（含0．1％甲酸）一乙腈为流动相梯度洗脱,流速为0．2mL／min,四级杆一飞行时间串联质谱检测。结果全血中佐匹克隆和扎来普隆的线性范围为10ng／mL-500ng／mL,检出限为3ng／mL唑吡坦的线性范围为3ng／mL-300ng／mL,检出限为lng／mL。结论本方法准确、快速、灵敏,可用于全血中佐匹克隆、唑吡坦和扎来普隆的同时定性、定量检测。     

液相色谱/质谱法检测血液中的艾司佐匹克隆

目的建立手性分离-液相色谱/质谱法,用于分离检测血液中艾司佐匹克隆。方法血液经HLB小柱固相萃取后,采用手性分离柱,用电喷雾正离子模式离子化、多反应监测模式检测艾司佐匹克隆,外标法定量。结果采用本文方法可有效分离佐匹克隆的左旋、右旋异构体,血中艾司佐匹克隆在1～100ng/mL范围内线性关系良好,相关系数为0.996 4,最低检出限为0.8ng/mL,回收率为76%～88%,日内与日间精密度均小于8%。结论本文所建方法简便、快速、分离度好,适用于血液中艾司佐匹克隆的检测。     

Rapid enantiomeric analysis of zopiclone in serum by supercritical fluid chromatography–tandem mass spectrometry

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 × 10⁻² ng/mL and 25 ng/mL for R-ZOP, and 5.2 × 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°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.     

固相萃取-气相色谱法检测全血中佐匹克隆

目的采用固相萃取-气相色谱法检测全血中佐匹克隆。方法采用Oasis HLB固相萃取柱对样品进行前处理,去离子水、0.5%氨水-甲醇/水((V/V 40∶60)溶液先后淋洗,二氯甲烷/异丙醇(V/V 75∶25)洗脱后进行GC/NPD检测。结果血液中佐匹克隆在50～5 000ng/mL范围内线性良好(R2=0.998 8),平均萃取回收率为96.9%,检出限为30ng/mL,日内RSD为2.1%～5.7%,日间RSD为3.3%～6.2%,结论固相萃取-气相色谱检测法灵敏度高,重现性好,可在血液中佐匹克隆的检测中选用。