快速高分辨率液相色谱-串联质谱法测定牛肉中24种镇静剂类兽药残留量  

Determination of 24 sedative residues in beef by rapid resolution liquid chromatography-tandem mass spectrometry

作　　者：魏晋梅[1] 周围 解迎双 张丽[3] 方素栎[4] 罗玉柱[1] 张咏梅[1] 

机构地区：[1]甘肃农业大学研究测试中心,甘肃省草食动物生物技术重点实验室,甘肃兰州730070 [2]甘肃出入境检验检疫局,甘肃兰州730020 [3]甘肃农业大学食品科学与工程学院,甘肃兰州730070 [4]甘肃农业大学动物科学技术学院,甘肃兰州730070

出　　处：《食品与发酵工业》2016年第2期191-196,共6页Food and Fermentation Industries

基　　金：甘肃省自然科学基金项目(1208RJZA156);甘肃省自然科学基金重点项目(1010RJZA202);甘肃省财政厅项目(基于指纹图谱技术的牦牛产地鉴别与新鲜度评价研究)

摘　　要：建立了牛肉中24种镇静剂类药物残留量的检测方法。样品经氨水-乙腈溶液（体积比10∶90）和30μLβ-葡糖苷酸酶/芳基硫酸酯酶提取后,用HLB固相萃取小柱净化,采用快速高分辨率液相色谱-串联质谱（RRLC-MS/MS）检测,以信噪比（S/N）分别为3和10时测定药物的检出限（LODs）和定量限（LOQs）。各药物在添加浓度水平范围均有良好的线性关系,相关系数（r^2）在0.963 9～0.999 8之间,LODs为0.2～2.5μg/kg,LOQs为0.5～5μg/kg,平均添加回收率为74.1%～123.9%,日内相对标准偏差（RSD）为2.6～9.9%,日间相对标准偏差（RSD）为2.9～9.9%。该方法灵敏度高、回收率高,为镇静剂类药物残留量检测提供了基础方法,可满足同类实验室的检测需求。A rapid resolution liquid chromatography-tandem mass spectrometry（ RRLC-MS / MS） method was established for the determination of 24 sedatives residues in beef. After enzymolysis,sedatives residues in beef were extracted by ammonium hydroxide-acetonitrile（ 10∶ 90,v / v） and determined by RRLC-MS / MS and quantified by standard curve. The calibration curves showed good linearity within the concentrations of spiked levels with the correlation coefficients（ r^2） ranged from 0. 9639 to 0. 999 8. The limits of detection（ LODs） and quantification（ LOQs） were 0.2 ～ 2. 5 and 0. 5 ～ 5 μg kg-1,respectively. The average recoveries of spikes samples were in the ranges of 74. 1 ～123. 9% with relative standard deviations of intra-and inter-day ranged from 2. 6% to 9. 9% and from 2. 9% to 9.9%,respectively. This method is simple,sensitive and accurate in the determination of sedative residues.

关 键 词：镇静剂 高分辨率液相色谱-串联质谱 牛肉 

分 类 号：O657.63[理学—分析化学] TS251.52[理学—化学]