气相色谱/质谱法测定猪肉中4种苯二氮类镇静剂残留

Determination of Four Benzodiazepines Residues in Pork Using Gas Chromatography-Mass Spectrometry

建立了同时测定猪肉中4种苯二氮类药物(地西泮、艾司唑仑、阿普唑仑、三唑仑)残留量的固相萃取气相色谱质谱方法。用乙腈提取药物,C18固相萃取柱净化,GC/MS分析。运用HP5毛细管柱(30m×0.25mm×0.25μm)进行分离,电子轰击电离源(EI)质谱选择离子模式(SIM)检测(地西泮m/z241、256、257、284;艾司唑仑m/z205、239、259、294;阿普唑仑m/z204、273、279、308;三唑仑m/z238、313、315、342),外标法定量(定量离子m/z分别为256、259、270和313)。4种苯二氮类药物的标准曲线线性回归系数均在0.99以上,地西泮线性范围超过5～100μg/L;回收率为60%～70%;相对标准偏差7.6%～12.9%,最低检出限为2μg/kg。艾司唑仑、阿普唑仑、三唑仑3种药物的线性范围超过50～1000μg/L;回收率为60%～115%;相对标准偏差3.8%～19.7%,检出限为10μg/kg。

Solid phase extraction (SPE) and gas chromatography-mass spectrometric method have been developed for the determination of diazepam, estazolam, alprazolam and triazolam residues in pork. The conditions for extraction and cleanup on C_ 18 column of benzodiazepines were investigated and optimized. The analytes were separated by HP-5 chromatographic column, detected by mass detector in electron impact and time program-selected ion monitoring mode (EI/SIM) and quantified with the external standard calibration curve method. Linear calibration curves were obtained in the concentration ranges from 5 to 100 μg/L for diazepam and from 50 to 1000 μg/L for estazolam, alprazolam and triazolam (the correlation coefficients were above 0.99). The average recoveries for the four benzodiazepines spiked in pork ranged from 60% to 115% and their relative standard deviations were between 3.8% and 19.7%. The limits of detection were 2 μg/kg for diazepam and 10 μg/kg for estazolam, alprazolam and triazolam in pork.