分析测试学报2017，Vol.36Issue(8)：963-968,6.DOI:10.3969/j.issn.1004-4957.2017.08.003
超高效液相色谱-串联质谱法测定动物源性食品中10种水杨酰胺类化合物
Determination of 10 Kinds of Salicylamides in Foods of Animal Origin by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
A new method was developed for the determination of 10 kinds of salicylamides,including 5-chlorosalicylanilid,4'-bromosalicylanilid,3',4'-dichloro-salicylanilid,4',5-dichloro-salicylanilid,3',4',5-trichloro-salicylanilid,5-bromo-4'-chlorosalicylanilide,3,5-dibromo-salicylanilid,4',5-dibromo-salicylanilid,3,4',5-tribromo-salicylanilid and 3,3',4',5-tetrachloro-salicylanilid in foods of animal origin using solid phase extraction(SPE) combined with ultra-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).Samples were extracted using acetonitrile,and purified with an amino(NH2) SPE column.The eluent was concentrated by nitrogen gas blowing.10 target compounds were separated on a T3 column(100 mm ×2.1 mm,1.8 μm)by gradient elution with methanol-0.1％ formic acid as mobile phase,ionized by negative electrospray ionization(ESI-),detected under multiple reaction monitoring(MRM) mode,and quantified by the external standard method.Under the optimized condition,the calibration curves of 10 kinds of salicylamides were linear in a certain concentration range with correlation coefficients (r2) no less than 0.995 7.The limits of detection(LODs,S/N =3) and limits of quantitation(LOQs,S/N =10) for the target compounds were in the ranges of 0.5-1.0 μg/kg and 1.5-3.0 μg/kg,respectively.The average recoveries at three spiked levels ranged from 81.0％ to 106％,with relative standard deviations(RSD,n =6) no more than 7.5％.The method was suitable for the identification and quantification of 10 kinds of salicylamides in foods of animal origin.关键词
动物源性食品/固相萃取(SPE)/水杨酰胺类化合物/超高效液相色谱-串联质谱法(UPLC-MS/MS)Key words
foods of animal origin/solid phase extraction (SPE)/salicylamides/ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS)分类
化学化工引用本文复制引用
周思,邓龙,林森煜,黄嘉乐,郭新东..超高效液相色谱-串联质谱法测定动物源性食品中10种水杨酰胺类化合物[J].分析测试学报,2017,36(8):963-968,6.基金项目
广东省质量技术监督局科技项目(2016PZ09) （2016PZ09）
