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| Simultaneous Determination of 16 Sedative Residues in Livestock Products by Solid Phase Extraction/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| DOI： |
| KeyWord:solid phase extraction ultra performance liquid chromatography-tandem mass spectrometry sedative livestock products |
| Author | Institution |
| LIU Jia-yang，HUANG Xu，JIA Hong-xin |
辽宁省食品检验检测院 |
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| Abstract: |
| 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 0.22μm syringe filter. Chromatographic separation was performed on a Waters ACQUITY UPLC BEH C18（2.1mm×100mm,1.7μm） 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 0.9968.The limits of detection（LOD） and quantitation（LOQ） for 16 sedative residues were in the range of 0.01-0.05μg/kg and 0.1-0.5μg/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. |
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