超高效液相色谱-串联质谱法快速测定猪尿液中30种不同种类“瘦肉精”药物残留
发布时间：2018-08-22 07:28
【摘要】：建立了超高效液相色谱-串联质谱快速简单地同时测定猪尿液中30种不同种类"瘦肉精"药物(赛庚啶、可乐定及28种β-受体激动剂类)残留的方法。对液相色谱分离条件、MS/MS检测参数及样品前处理方式进行了优化。试样经5000 r/min离心5 min后直接经MCX柱净化,分别用3 m L水和3 m L甲醇淋洗,5%氨化甲醇进行洗脱,N2吹干后以流动相进行复溶,UPLC-MS/MS进行测定。结果表明,30种药物可在5.0 min内有效分离;各药物在0.1~10μg/L范围内呈良好的线性关系,相关系数均大于0.992;方法的检出限为0.1μg/L,定量限为0.3μg/L。在3个浓度水平下的平均回收率为67.6%~103.2%,日内、日间相对标准偏差分别为2.8%~16.8%和2.6%~15.8%。
[Abstract]:A rapid and simple method for the simultaneous determination of 30 different kinds of "lean meatine" (cyproheptadine, clonidine and 28 尾 -agonists) in pig urine by ultra-high performance liquid chromatography-tandem mass spectrometry was established. The detection parameters and sample pretreatment methods of MS / MS were optimized. The samples were purified by MCX column after centrifugation for 5 min with 5000 r/min. The samples were eluted with 3 mL water and 3 mL methanol respectively. The samples were eluted by N _ 2 and dried by N _ 2. The mobile phase was determined by UPLC-MS / MS. The results showed that 30 drugs could be effectively separated within 5.0 min, the linear range of each drug was 0.1 渭 g / L and the correlation coefficient was greater than 0.992.The detection limit of the method was 0.1 渭 g / L and the quantitative limit was 0.3 渭 g / L. The average recoveries were 67.6 and 103.2, and the relative standard deviations during the day were 2.816.8% and 2.615.8%, respectively.
【作者单位】： 中国动物卫生与流行病学中心动物产品安全监测室;农业部畜禽产品质量安全风险评估实验室(青岛);青岛易邦生物工程有限公司;安徽农业大学动物科技学院;
【基金】：农业部"农产品质量风险评估项目"(No.GJFP201600706) 中国动物卫生与流行病学中心创新基金项目(No.2014IF-0003FF)资助
【分类号】：S859.8;O657.63
，
本文编号：2196403
[Abstract]:A rapid and simple method for the simultaneous determination of 30 different kinds of "lean meatine" (cyproheptadine, clonidine and 28 尾 -agonists) in pig urine by ultra-high performance liquid chromatography-tandem mass spectrometry was established. The detection parameters and sample pretreatment methods of MS / MS were optimized. The samples were purified by MCX column after centrifugation for 5 min with 5000 r/min. The samples were eluted with 3 mL water and 3 mL methanol respectively. The samples were eluted by N _ 2 and dried by N _ 2. The mobile phase was determined by UPLC-MS / MS. The results showed that 30 drugs could be effectively separated within 5.0 min, the linear range of each drug was 0.1 渭 g / L and the correlation coefficient was greater than 0.992.The detection limit of the method was 0.1 渭 g / L and the quantitative limit was 0.3 渭 g / L. The average recoveries were 67.6 and 103.2, and the relative standard deviations during the day were 2.816.8% and 2.615.8%, respectively.
【作者单位】： 中国动物卫生与流行病学中心动物产品安全监测室;农业部畜禽产品质量安全风险评估实验室(青岛);青岛易邦生物工程有限公司;安徽农业大学动物科技学院;
【基金】：农业部"农产品质量风险评估项目"(No.GJFP201600706) 中国动物卫生与流行病学中心创新基金项目(No.2014IF-0003FF)资助
【分类号】：S859.8;O657.63
，
本文编号：2196403
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