动物源性食品中地西泮残留量的检测方法研究

Research on methods for determination of diazepam residue in animal original food

采用高效液相色谱法(HPLC)、气相色谱质谱联用法(GC-MS/MS)以及液相色谱质谱联用法(HPLCMS/MS)测定动物源性食品中镇静剂类药物地西泮的残留量。将样品均质粉碎后,经乙腈提取,固相萃取小柱净化后上机检测,外标法定量。实验证明,当固相萃取的洗脱液中甲醇与乙酸溶液的体积比为70:30时,洗脱效率最高。在不同仪器条件下,地西泮在各自浓度范围内的线性关系良好,相关系数(r^2)均大于0.999,回收率在84.6%～101.7%,相对标准偏差(RSD)在0.52%～9.44%(n=3),检出限为0.5μg·kg^(-1)(S/N=3,气相色谱质谱联用法以及液相色谱质谱联用法)和10.0μg·kg^(-1)(S/N=3,高效液相色谱法),定量限按照3倍检出限计算; 3种方法均可分析动物源性食品中的地西泮残留量。对比可知,质谱法灵敏度和准确率高,但有一定的基质效应;液相色谱法操作简单,几乎不受基质效应的影响,但灵敏度和准确率不如质谱法。

High performance liquid chromatography (HPLC),gas chromatography mass spectrometry (GC-MS) and liquid chromatography tandem mass spectrometry (LC-MS/MS) were applied to determine the diazepam residue in animal original food.Samples were detected quantitatively by external standard method through smashed homogeneously,extracted by acetonitrile as well as purified by solid phase extraction column.The highest efficiency of elution was reached when the ratio of methanol to acetic acid solution was 70:30 in volume.The linearity ranges of diazepam were all very well with different instruments,meanwhile,correlations were all above 0.999,the recoveries were between 84.6% and 101.7% with the RSDs in the range of 0.52% to 9.44%(n=3).The limit of detection was 0.5 μg kg^-1 for both LC-MS/MS and GC-MS,10.0 μg kg^-1 for HPLC.The diazepam residue in animal original food can be quantitatively analyzed by all these three instrumental methods.In particular,mass spectral methods were highly sensitive and accurate while the operation of HPLC were easy and matrix-effect free.