QuEChERS-液相色谱-串联质谱法测定乳及乳制品中活化酯及其代谢物阿拉酸式苯含量  

Determination of Acibenzolar-S-methyl and Their Metabolite Acibenzolar Acid in Milk and Dairy Products by QuEChERS-Liquid Performance Chromatography-Tandem Mass Spectrometry

作　　者：汪春明 霍江莲[2] 陈冬东[3] 彭涛[3] 余丽波 贾景建 WANG Chunming;HUO Jianglian;CHEN Dongdong;PENG Tao;YU Libo;JIA Jingjian(CAIQ(Beijing)Testing and Certification Co.Ltd.,Beijing 100176,China;China National Accreditation Service for Conformity Assessment,Beijing 100062,China;Chinese Academy of Inspection and Quarantine,Beijing 100176,China;CAIQ(Beijing)Science and Technology Co.Ltd.,Beijing 100176,China)

机构地区：[1]中检科(北京)测试认证有限公司,北京100176 [2]中国合格评定国家认可中心,北京100062 [3]中国检验检疫科学研究院,北京100176 [4]检科院(北京)科学技术有限公司,北京100176

出　　处：《现代食品科技》2024年第10期362-369,共8页Modern Food Science and Technology

基　　金：国家重点研发计划项目(2022YFF1100804)。

摘　　要：该文研究了高效液相色谱-三重四级杆质谱法(HPLC-MS/MS)测定乳及乳制品中活化酯和阿拉酸式苯的测试方法。样品经甲酸乙腈(含1%甲酸(V/V))涡旋提取,分析液经QuEChERSdSPE EMR-Lipid除脂专用管净化,离心后过膜上机检测。测试方法以甲醇-0.1%甲酸水(V/V)为流动相,流速设置为0.2 mL/min,应用梯度洗脱程序,采用ACQUITY UPLC HSS T3色谱柱进行分离,电喷雾正、负离子模式(活化酯为ESI+、阿拉酸式苯为ESI-),多反应离子监测模式(MRM)检测,基质匹配外标法进行定量。对于乳及乳制品基质,活化酯和阿拉酸式苯在1~30 ng/mL的质量浓度与其相对应的峰面积之间线性关系良好,R^(2)均大于0.996,在0.01、0.02和0.1 mg/kg 3种不同浓度添加水平下,活化酯和阿拉酸式苯的平均回收率在91.8%~109.6%之间,相对标准偏差在1.3%~11.5%之间。该方法可满足残留检测的准确度、精密度和灵敏度的要求。This study explored a test method for the determination of acibenzolar-S-methyl and acibenzolar acid in milk and dairy products by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples were subjected to vortex extraction with formic acid-acetonitrile(containing 1%(V/V)formic acid),and purified by QuEChERSdSPE EMR-Lipid tubes,centrifuged then filtered before detection.The test method used gradient elution using methanol-0.1%(V/V)formic acid as the mobile phase,a flow rate of 0.2 mL/min and ACQUITY UPLC HSS T3 column for separation.Electrospray positive and negative ion modes(ESI+for acibenzolar-S-methyl and ESI-for acibenzolar)and multiple reaction monitoring(MRM)were used for detection,and the matrix-matched external standard method was used for quantification.For milk and dairy products,good linearity between the mass concentrations of acibenzolar-S-methyl and acibenzolar acid,and their corresponding peak areas,in the concentration range of 1~30 ng/mL,with the correlation coefficients R^(2) higher than 0.996.The mean recoveries of acibenzolar-S-methyl and acibenzolar acid were 91.8%~109.6%and the corresponding relative deviation(RSD)values were 1.3%~11.5%at three spiking levels(0.01,0.02 and 0.1 mg/kg).This method can meet the requirements of accuracy,precision,and sensitivity for residue detection.

关 键 词：活化酯 阿拉酸式苯 乳及乳制品 液相色谱-串联质谱法 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]