全自动固相萃取-超高效液相色谱/串联质谱法测定水产品中9种微囊藻毒素

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英文篇名：Determination of 9 microcystins in aquatic products by automated solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry 作者：朱文涛 ; 邵国健 ; 张鹏 ; 付云 英文作者：ZHU Wen-tao;SHAO Guo-jian;ZHANG Peng;FU Yun;Huzhou Center for Disease Control and Prevention; 关键词：水产品 ; 微囊藻毒素 ; 固相萃取 ; 液相色谱-串联质谱法 英文关键词：Aquatic products;;Microcystins;;Solid phase extraction;;Ultra performance liquid chromatography-tandem mass spectrometry 中文刊名：ZWJZ 英文刊名：Chinese Journal of Health Laboratory Technology 机构：湖州市疾病预防控制中心; 出版日期：2019-01-25 出版单位：中国卫生检验杂志 年：2019 期：v.29 基金：浙江省公益技术应用研究计划项目(2016C37022);浙江省公益技术应用研究计划项目(2016C33218);; 浙江省医药卫生科技计划项目(2018RC072) 语种：中文; 页：ZWJZ201902007 页数：5 CN：02 ISSN：41-1192/R 分类号：32-36

摘要

目的建立固相萃取-超高效液相色谱串联质谱法测定水产品中9种微囊藻毒素的分析方法。方法均质样品经乙酸-甲醇-0. 1 mol/L EDTA-Mcllvaine缓冲溶液(2∶49∶49,V/V/V)溶液提取后,再经HLB固相萃取柱净化,氮吹浓缩,用甲醇-0. 04%甲酸(1∶1,V/V)溶解,0. 22μm微孔滤膜过滤后进样,BEH C_(18)柱(2. 1 mm×100 mm,1. 7μm)分离,串联质谱MRM模式检测。结果通过本研究的提取净化方法,能够同时测定水产品种9种微囊藻毒素,其质量浓度为5 ng/ml～200 ng/ml时,线性相关系数(r)均> 0. 998,9种微囊藻毒素的检出限(LOD)为0. 10μg/kg～2. 48μg/kg,定量限(LOQ)为0. 30μg/kg～8. 27μg/kg。3种加标水平10μg/kg、40μg/kg和100μg/kg下的回收率为71. 4%～79. 7%、72. 4%～80. 4%和70. 6%～82. 2%,相对标准偏差(RSD)为6. 4%～8. 4%、4. 9%～8. 7%和5. 8%～8. 4%(n=6)。结论该方法前处理简单、选择性强、灵敏度高,可同时测定水产品中9种微囊藻毒素。
        Objective To develop a method for the determination of 9 microcystins in aquatic products by solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS). Methods The microcystins were extracted with acetic acid-methanol-0. 1 mol/l EDTA-Mcllvaine( 2∶49∶49,V/V/V) and cleaned-up with HLB. The extract was dried-up with nitrogen. The residue was re-dissolved with MeOH-0. 04% fomic acid( 1∶1,V/V).The solution was filtered with 0. 22 μm membrane and then injected for analysis. Separation was performed with a BEH C_(18)column( 2. 1 mm × 100 mm,1. 7 μm) and the detection was performed using tandem mass spectrometer in MRM mode.Results Through the extraction and purification methods in this study,9 microcystins in aquatic products were detected. The method showed a good linearity in the range of 5 ng/ml-200 ng/ml,with correlation coefficients above 0. 998. The detection limits( LODs) of the method were within 0. 10 μg/kg-2. 48 μg/kg and the limits of quantification( LOQs) were within0. 30 μg/kg-8. 27 μg/kg. The mean recoveries spiked at levels of 10 μg/kg,40 μg/kg and 100 μg/kg were within 71. 4%-79. 7%,72. 4%-80. 4% and 70. 6%-82. 2%,with relative standard deviation( RSD) of 6. 4%-8. 4%,4. 9%-8. 7%and 5. 8%-8. 4%( n = 6). Conclusion This method is efficient,selective and sensitive. It can simultaneously determine 9microcystins in aquatic products.

引文

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