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建立了畜肉中16种镇静剂类兽药残留的固相萃取净化/超高效液相色谱-串联质谱(LC-MS/MS)的同时测定方法。样品均质后经氢氧化钠溶液水解,加入盐酸溶液提取。提取液经固相萃取柱MCX净化,洗脱液氮气吹干后用流动相溶解,经0.22μm滤膜过滤,采用Waters ACQUITY UPLC BEH C18(2.1mm×100mm,1.7μm)色谱柱分离,在电喷雾电离源(ESI)和多反应监测(MRM)正离子模式下测定,外标法定量。结果表明:采用基质匹配外标法测定,16种镇静剂类化合物在一定浓度范围内呈良好的线性关系(r2≥0.9968),在样品中的检出限和定量下限分别为0.01~0.05μg/kg和0.1~0.5μg/kg,在3个浓度加标水平下的平均回收率为71.6%~112%,相对标准偏差(RSD)为2.9%~15.8%。市售多种鲜肉制品的测定结果表明,该方法选择性好、操作简单快速、结果准确,适用于畜肉中16种镇静剂类兽药残留的同时快速测定。
The simultaneous determination of 16 kinds of sedatives veterinary drug residues in livestock meat by solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) was established. Samples were homogenized by sodium hydroxide solution hydrolysis, hydrochloric acid solution was added to extract. The extract was purified by solid-phase extraction cartridge MCX. The eluate was dried with nitrogen and dissolved in the mobile phase. The residue was filtered through a 0.22 μm filter and separated on a Waters ACQUITY UPLC BEH C18 (2.1 mm × 100 mm, 1.7 μm) column. Spray ionization source (ESI) and multiple reaction monitoring (MRM) positive ion mode determination, external standard quantitative. The results showed that 16 kinds of sedative compounds showed a good linear relationship (r2 ≥ 0.9968) with matrix matching and external standard method. The detection limits and the lower limits of quantitation were 0.01 ~ 0.05 μg / kg And 0.1 ~ 0.5μg / kg. The average recoveries were 71.6% ~ 112% with RSDs of 2.9% ~ 15.8% at three spiked levels. The test results of a variety of fresh meat products on the market show that the method has the advantages of good selectivity, simple and quick operation and accurate results, and is applicable to the rapid determination of 16 kinds of sedative veterinary drugs residues in livestock meat at the same time.