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固相萃取/超高效液相色谱-串联质谱法测定贝类中3种短裸甲藻毒素
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作者单位
严忠雍,张小军,陈思,李佩佩,龙举,张虹 1.浙江省海洋水产研究所2.浙江工商大学食品与生物工程学院 
基金项目:浙江省科技计划项目(2017C37009)
中文摘要:建立了同时测定贝类中3种短裸甲藻毒素的超高效液相色谱-串联质谱法。样品采用丙酮提取、C18固相萃取柱净化;以5 mmol/L 乙酸铵(含0.1%甲酸)-乙腈为流动相,ACQUITYTM UPLC BEH C18色谱柱进行分离,在多反应监测模式下进行测定,外标法定量。结果表明,3种目标物在1.0~100 μg/L质量浓度范围内线性良好,相关系数(r2)不小于0.996,方法定量下限为3.0 μg/kg,回收率为80.0%~87.5%,相对标准偏差为1.3%~5.4%。该方法前处理简单,灵敏度高,稳定性好,适用于贝类中3种短裸甲藻毒素的同时测定。
中文关键词:固相萃取  超高效液相色谱-串联质谱(UPLC-MS/MS)  贝类  短裸甲藻毒素
 
Determination of Three Brevetoxins in Shellfish by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction
Abstract:An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the determination of 3 kinds of brevetoxins(BTX) in shellfish.The samples were extracted with acetone,and purified on a C18 solid phase extraction column.The separation of the analytes was performed on an ACQUITYTM UPLC BEH C18 column with 5 mmol/L ammoumium acetate containing 0.1% formic acid-acetonitrile as mobile phase,and detected in multiple reaction monitoring(MRM) mode.The external standard method was used for quantitation.Results showed that there were good linear relationships for BTXs in the range of 1.0-100 μg/L with correlation coefficients(r2) not less than 0.996.The quantitation limits of the method were 3.0 μg/kg.The recoveries for the brevetoxins ranged from 80.0% to 87.5% with relative standard deviations of 1.3%-5.4%.The method was suitable for the determination of brevetoxins in shellfish with advantages of simple processing,high sensitivity and good stability.
Key Words:solid phase extraction  ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  shellfish  brevetoxin
引用本文:严忠雍,张小军,陈思,李佩佩,龙举,张虹.固相萃取/超高效液相色谱-串联质谱法测定贝类中3种短裸甲藻毒素[J].分析测试学报,2019,(2):224-228.
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