气相色谱-质谱法同时测定腊肠中7种镇静剂类药物残留

Determination of Seven Sedative Residues in Sausage by Gas Chromatography-mass Spectrometry 2 (1.) (2.) Abstract: Key words:

摘要:

本研究建立了同时测定腊肠中地西泮、奥沙西泮、艾司唑仑、阿普唑仑、三唑仑、苯巴比妥、异丙嗪7种镇静剂残留的固相萃取气相色谱-质谱（GC-MS）方法。试样中的镇静剂类药物经氨化乙腈和酸化乙腈提取，用C18固相萃取柱净化，甲醇:丙酮（5: 5，V/V）洗脱，上GC-MS分析。采用毛细管色谱柱DB-5MS（30 m×0.25 mm×0.25 μm）进行分离，电子轰击电离源（EI），在选择离子扫描（SIM）模式下测定，外标法定量（定量离子分别为256、205、259、279、313、204、72）。实验结果表明，7种镇静剂类药物在一定的含量范围内线性关系良好（分别为0.0488~0.7808 mg/L，0.1039~1.2468 mg/L，0.0971~1.4566 mg/L，0.1006~1.5090 mg/L，0.0975~1.1700 mg/L，0.0605~1.5360 mg/L，0.0454~1.0896 mg/L），相关系数大于0.997，检出限为0.020~0.082 mg/L，回收率为63.20~88.23%，相对标准偏差（n=5）为7.02~16.89%。结果表明，该方法简便快速、灵敏可靠，适用于肉制品中多种镇静剂类药物残留的检测。

Abstract:

A method for the determination of seven sedative residues (diazepam, oxazepam, estazolam, alprazolam, triazolam, phenobarbital, promethazine) in sausage using solid-phase extraction (SPE) and gas chromatography–mass spectrometry (GC-MS) was established. Five different sausage samples were extracted respectively with basic and acidic acetonitrile solutions, followed by purified on C18 column and eluted by methanol: acetone (5:5, V/V), the analytes were then screened with GC-MS. After separated on chromatographic column DB-5MS (30 m × 0. 25 mm×0. 25 μm), external standard calibration was used for quantitative analysis of targeted compounds. The characteristic ions were 256, 205, 259, 279, 313, 204 and 72. The results indicated that seven sedatives had a satisfactory linearity in certain range of concentration (from 0.0488 to 0.7808 mg/L, 0.1039 to 1.2468 mg/L, 0.0971 to 1.4566 mg/L, 0.1006 to 1.5090 mg/L, 0.0975 to 1.1700 mg/L, 0.0605 to 1.5360 mg/L, 0.0454 to 1.0896 mg/L, respectively), with the correlation coefficient more than 0.997. The limit of detection (LOD) of seven sedatives was in the range of 0.020~0.082 mg/L and the average recoveries ranged from 63.20% to 88.23%, and the RSD was from 7.02% to 16.89%. The developed method was simple and accurate, which was available for the detection of sedative residues in meat product.