QuEChERS-高效液相色谱-串联质谱法同时测定动物源性食品中21种琥珀酸脱氢酶抑制剂类杀菌剂的残留量  

QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of 21 Succinate Dehydrogenase Inhibitor Fungicides in Animal Foods

作　　者：李敏青 陈姿竹 李菊 庄嘉 吴舒悦 徐娟 LI Minqing;CHEN Zizhu;LI Ju;ZHUANG Jia;WU Shuyue;XU Juan(Technology Center of Guangzhou Customs,Guangzhou 510623)

机构地区：[1]广州海关技术中心,广东广州510623

出　　处：《分析科学学报》2024年第5期501-510,共10页Journal of Analytical Science

摘　　要：通过优化QuEChERS盐析提取条件和分散固相萃取(dSPE)净化剂组合条件,基于高效液相色谱-三重四极杆串联质谱仪,建立了适用于动物源性食品(畜禽肉、水产品、内脏、脂肪、奶和禽蛋)中21种琥珀酸脱氢酶抑制剂类杀菌剂残留量的检测方法。针对不同类别的动物源食品基质特点,以回收率和净化效率为判定指标分别对提取溶剂、除水剂和净化剂进行了优化,实现了靶标物质高效提取和基体杂质有效去除,同时选取更佳的色谱柱和流动相提高了目标分析物的灵敏度和分离效率。样品经水分散均匀后,以正己烷饱和的乙腈提取,借助乙二胺-N-丙基硅烷(PSA)和十八烷基键合硅胶(C_(18))吸附剂净化,采用Thermo Accucore aQ(150×2.1mm,2.6μm)色谱柱分离,以含5mmol/L甲酸铵+0.1%甲酸水溶液和甲醇为流动相进行梯度洗脱,多反应监测(MRM)正离子模式测定,基质匹配外标法定量。结果表明,21种农药在1~50μg/L范围内线性关系良好,相关系数(r)均不少于0.999,检出限为0.005~0.28μg/kg,定量限为0.02~0.93μg/kg。向猪肉、猪脂肪、牛奶、鸡蛋4种不同类别的动物源空白样品基质添加标准溶液,21种农药在低、中、高3个浓度水平(5、10、50μg/kg)下的平均回收率为83.0%~107%,相对标准偏差为0.20%~7.40%。该方法操作简便快速、准确高效,目前已广泛应用于进出口动物源食品中多种琥珀酸脱氢酶抑制剂类杀菌剂的筛查检测与确证分析任务中,具有一定的应用价值。By optimizing the conditions of QuEChERS salt-out extraction and dispersive solid-phase extraction,a method for the determination of 21 kinds of succinate dehydrogenase inhibitor(SDHD fungicideresidues in animal-derived foods(livestock and poultry products,aquaticproducts,viscera,fat,milk and egg)was established based on high performance liquid chromatography-triplequadrupole tandem mass spectrometer(HPLC-MS/MS).Based on the characteristics of different types of animal-derived food substrates,the extraction solvent,dehydrator and purification agent were optimized with the recovery and purification efficiency as the criteria to achieve efficient extraction of target substances and effective removal of matrix impurities.At the same time,better chromatographic columns and mobile phases were selected to improve the sensitivity and separation efficiency of target analytes.The samples were evenly dispersed with water,extracted with acetonitrile saturated with n-hexane+and cleaned up with PSA and Ca adsorbents.The extracts were separated on Thermo Accucore aQ column(150 X 2.1 mm,2.6μm)using 5 mmol/L ammonium formate,0.1%formic acid aqueous solution and methanol solution as mobile phase by gradient elution.The detection of SDHIs was detected byHPLC-MS/MS with positive electrospray ion source under multiple reaction monitoring(MRMmode.The matrix-matched external standard method was used for the quantitation.The method showed good linearities in the range of 1-50 pg/L.The correlation coefficients(r)were greater than 0.999.The limits of detection(LODs)were in the range of 0.005-0.28μg/kg.The limits of quantitation(LOQs)were in the range of 0.02-0.93μg/kg.The standard solution was added to the blank sample matrix of pork,fat,milk and egg of different categories of animal origin.The average recoveries obtained ranged from 83.0%to 107%and the relative standard deviations(RSDs)from 0.20%to 7.40%for spiking levels of 5,10 and 50 pg/kg.The proposed method was applied successfully for the residue determination of the selected p

关 键 词：动物源性食品 琥珀酸脱氢酶 分散固相萃取 高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]