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，R2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 R2 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.

国家重点研发计划项目（2022YFF1100804）