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.
作者
张婧雯
张海超
范斌
艾连峰
王敬
李玮
康维钧
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)
出处
《分析测试学报》
CAS
CSCD
北大核心
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)
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
dipyrone metabolite
through-type solid-phase extraction
PRiME HLB
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
foods of animal origin
