气相色谱/质谱法测定猪肉中4种苯二氮类镇静剂残留

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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。 A method for the simultaneous determination of four benzodiazepines (diazepam, estazolam, alprazolam, triazolam) residues in pork by gas chromatography-mass spectrometry was established. Drug extraction with acetonitrile, C18 solid phase extraction column purification, GC / MS analysis. Separation was performed on a HP5 capillary column (30 m × 0.25 mm × 0.25 μm). Electron impact ionization mass spectrometry (EI) mass spectrometry with ion-mode selective ionization (SIM) detection (diazepam m / z 241,256,257,284; estazolam m / z205,239,259,294; alprazolam m / z204,273,279,308; triazolam m / z238,313,315,342), external standard method (quantitative ion m / z 256 , 259, 270 and 313). The linear regression coefficients of four standard benzodiazepines were above 0.99, the linear range of diazepam was over 5 ~ 100 μg / L, the recovery was 60% ~ 70%, the relative standard deviation was 7.6% ~ 12.9%, the lowest The detection limit was 2μg / kg. The linear ranges of eszolam, alprazolam and triazolam were over 50 ~ 1000μg / L, the recoveries were 60% ~ 115%, the relative standard deviations were 3.8% ~ 19.7% .The detection limits were 10μg / kg.
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