固相萃取/超高效液相色谱-串联质谱法测定畜肉中16种镇静剂类兽药残留

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 C_(18)(2.1 mm×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(r~2≥0.996 8),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。

Simultaneous Determination of 16 Sedative Residues in Livestock Products by Solid Phase Extraction/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

A multi-residue method was established for the simultaneous determination of 16 sedative residues (e.g.xylaznie,methaqualone,diazepan,promethazine,oxazepam,carazolol,chlordiazepoxide,zolpidem,chlorpromazine,acetopromaizine,azaperone,azaperol,propionylpromazin,haloperidol,droperidol,perphenazine) in pork using solid phase extraction/ultra performance liquid chromaography-tandem mass spectrometry (LC-MS/MS).The homogenized samples were hydrolyzed with NaOH,then the analytes were extracted with HCl and cleaned up with an Oasis MCX SPE column.After evaporated to dryness under nitrogen and reconsituted,the reconstituted solution was filtrated through a 0.22 μm syringe filter.Chromatographic separation was performed on a Waters ACQUITY UPLC BEH C18(2.1 mm × 100 mm,1.7 μm) column.The qualitative and quantitative detections of 16 analytes were operated by electrospray ionization-tandem mass spectrometry under the positive mode using multiple reaction monitoring(MRM) mode,with the external standard method.The matrix matching external standard method was used for quantitation analysis.All sedative residues have good linear relationship in the certain concentration range with correlation coefficients (r2) not less than 0.996 8.The limits of detection(LOD) and quantitation(LOQ) for 16 sedative residues were in the range of 0.01-0.05 μg/kg and 0.1-0.5 μg/kg,reapectively.The average recoveries at three spiked concentration levels varied from 71.6％ to 112％,and the relative standard deviations(RSD) were 2.9％-15.8％.The method was of high sensitivity,simplicity,reliability and low cost,and was suitable for the simultaneous determination of 16 sedative residues in livestock products.