通过式固相萃取/超高效液相色谱-串联质谱法快速测定动物源性食品中安乃近代谢物残留量  

Rapid Determination of Dipyrone Metabolite Residues in Foods of Animal Origin by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with a Through-type Solid-phase Extraction

作　　者：张婧雯 张海超 范斌 艾连峰 王敬 李玮 康维钧[3] ZHANG Jing-wen;ZHANG Hai-chao;FAN Bin;AI Lian-feng;WANG Jing;LI Wei;KANG Wei-jun(Shijiazhuang Customs Technology Center,Shijiazhuang 050051,China;Hebei Food Inspection and Research Institute,Shijiazhuang 050000,China;School of Public Health,Hebei Medical University,Shijiazhuang 050017,China)

机构地区：[1]石家庄海关技术中心,河北石家庄050051 [2]河北省食品检验研究院,河北石家庄050000 [3]河北医科大学公共卫生学院,河北石家庄050017

出　　处：《分析测试学报》2019年第9期1114-1119,共6页Journal of Instrumental Analysis

基　　金：国家自然科学基金项目(81872628)

摘　　要：建立了通过式固相萃取/超高效液相色谱-串联质谱(UPLC-MS/MS)快速测定动物源性食品中4-甲氨基安替比林(MAA)、4-氨基安替比林(AA)、4-甲酰氨基安替比林(FAA)和4-乙酰氨基安替比林(AAA)4种安乃近代谢物的方法。样品采用乙腈提取,PRiME HLB固相萃取柱净化,在ACQUITY BEH C18色谱柱上以乙腈和0.1%甲酸水溶液为流动相梯度洗脱,超液相色谱-串联质谱MRM方式进行定量分析。结果表明,4种化合物在0.5~50μg/L范围内线性关系良好,相关系数(r)大于0.996,方法的检出限(LOD)为2μg/kg,定量下限(LOQ)为5μg/kg。4种化合物在3个加标水平(5、10和50μg/kg)下的回收率为75.1%~115%,相对标准偏差(RSD)为1.6%~7.4%。该方法简单、快速、准确,可实现动物源性食品中安乃近代谢物的快速测定。A method was developed for the rapid detection of 4-methylaminoantipyrine(MAA),4-aminoantipyrine(AA),4-formylaminoantipyrine(FAA)and 4-acetylaminoantipyrine(AAA)in foods of animal origin by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)with a through-type solid-phase extraction.Samples were extracted with acetonitrile,then cleaned up with a PRiME HLB column,finally quantified by UPLC-MS/MS in MRM mode after gradient elution on an ACQUITY BEH C 18 column with acetonitrile and 0.1%formic acid as mobile phases.Results showed that the calibration curves for four analytes were linear in the range of 0.5-50μg/L with correlation coefficients(r)larger than 0.996.The limits of detection(LODs)and the limits of quantitation(LOQs)were 2μg/kg and 5μg/kg,respectively.The average recoveries at three spiked levels of 5,10 and 50μg/kg ranged from 75.1%to 115%,with relative standard deviations(RSD)of 1.6%-7.4%.The proposed method is simple,rapid and accurate,and could be applied in the simultaneous determination of dipyrone metabolite residues in foods of animal origin.

关 键 词：安乃近代谢物 通过式固相萃取 PRIME HLB 超高效液相色谱-串联质谱 动物源性食品 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]