凝胶渗透色谱净化-超高效液相色谱-串联质谱法测定海带中扑草净残留量  

Determination of prometryn residues in kelp by gel permeation chromatography purification-ultra performance liquid chromatography-tandem mass spectrometry

作　　者：刘慧 卢加文 赵艳 张艳红 张凤枰 刘耀敏[1,2] 王锡昌 LIU Hui;LU Jia-Wen;ZHAO Yan;ZHANG Yan-Hong;ZHANG Feng-Ping;LIU Yao-Min;WANG Xi-Chang(Sichuan Willtest Technology Co.,Ltd.,Chengdu 610041,China;Tongwei Co.Ltd.,Chengdu 610041,China;College of Food Science and Technology,Shanghai Ocean University,Shanghai 201306,China)

机构地区：[1]四川威尔检测技术股份有限公司,成都610041 [2]通威股份有限公司,成都610041 [3]上海海洋大学食品学院,上海201306

出　　处：《食品安全质量检测学报》2018年第20期5340-5345,共6页Journal of Food Safety and Quality

基　　金："十二五"国家科技支撑计划项目(2015BAD17B00);四川省科技支撑计划项目(2016NZ0068)~~

摘　　要：目的建立凝胶渗透色谱(gel permeation chromatography,GPC)净化-超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)法测定海带中扑草净残留量的分析方法。方法样品用乙腈超声提取,经凝胶渗透色谱净化,收集15～35 min的流出液并进行浓缩,通过超高效液相色谱柱分离后进行质谱检测。结果称样量为2 g时,最佳提取条件为10 mL乙腈超声提取时间10 min;在添加量为0.05～2.66μg/kg范围时,扑草净平均回收率为100.1%～102.1%,相对标准偏差(relative standard deviation,RSD)为1.6%～2.6%(n=6);方法检出限为0.15μg/kg;并将GPC与HLB、固相萃取进行净化效果比较,结果表明GPC净化更适用于海带中扑草净的净化。结论该方法简便、快速、灵敏度高、重复性好,可用于测定海藻类样品的扑草净残留。Objective To establish a novel method for the determination of prometryn residues in kelp by gel permeation chromatography（GPC） purification-ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. Methods The sample was ultrasonically extracted with acetonitrile, purified by gel permeation chromatography, and the effluent was collected at 15-35 minutes and concentrated, and separated by ultra performance liquid chromatography column for mass spectrometry. Results When the sample weight was 2 g, the optimal extraction condition was ultrasonic extraction with 10 mL acetonitrile for 10 min. When the addition amount was in the range of 0.05-2.66 μg/kg, the average recovery rates of chlorpyrifos were 100.1%-102.1%, and the relative standard deviations（RSDs） were 1.6%-2.6%（n=6）. The limit of detection was 0.15 μg/kg. Compared with HLB and Carb-NH2 solid phase extraction, the results showed that GPC purification was more suitable for the purification of chlorpyrifos in kelp. Conclusion This method is simple, rapid, sensitive and repeatable, which can be used for the determination of prometryn residues in marine algae sample.

关 键 词：凝胶渗透色谱净化 超高效液相色谱-串联质谱法 外标法 扑草净 海带 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]