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谆质谱（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（30m×0．25mm×0．25μm）进行分离，电子轰击电离源（E1），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O．0488,-0．7808mgm，0．1039-1．2468mg／L，0．0971-1．4566mg／L，0．1006-1．5090mg／L，0,0975～1．1700mg／L，0．0605～1．5360mgm，0．0454～1．0896mg/L），相关系数大于0．997，检出限为0,020-0．082mg／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。
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 Cis 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 0.0264）.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.
出处
《现代食品科技》
EI
CAS
北大核心
2014年第2期274-278,共5页
Modern Food Science and Technology
基金
广东省质监局科技计划项目(2011CS02)
中山市科技局科技计划项目(20114A239)
关键词
气相色谱-质谱
镇静剂类药物
残留
腊肠
肉制品
gas chromatography-mass spectrometry
sedatives
residues
sausage
meat product
