超高效液相色谱-串联质谱法同时检测贝类中13种麻痹性贝类毒素  

Simultaneous detection of 13 kinds of paralytic shellfish poisoning toxins in bivalve by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：何明珠 袁冠湘 秦逍云[2] 刘红河[2] 姜杰[2] 杨胜园[1] 刘桂华 HE Ming-Zhu;YUAN Guan-Xiang;QIN Xiao-Yun;LIU Hong-He;JIANG Jie;YANG Sheng-Yuan;LIU Gui-Hua(College of Public Health,University of South China,Hengyang 421001,China;Shenzhen Center for Disease Control and Prevention,Shenzhen 518055,China)

机构地区：[1]南华大学公共卫生学院,衡阳421001 [2]深圳市疾病预防控制中心,深圳518055

出　　处：《食品安全质量检测学报》2021年第9期3465-3475,共11页Journal of Food Safety and Quality

基　　金：国家重点研发计划项目(2019YFC1605100);国际原子能机构合作研究基金项目(CRPD5203918859);深圳市医学重点学科建设经费;深圳市三名工程项目(SZSM201811070)。

摘　　要：目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定双壳贝类中13种麻痹性贝类毒素(paralytic shellfish poisoning toxins,PSTs)的方法。方法用乙酸水溶液提取贝类中的PSTs,经乙酸乙酯除杂,然后用石墨化碳黑固相萃取柱净化,采用UPLC BEH Amide色谱柱(100 mm×2.1 mm,1.7μm)分离,电喷雾正、负离子多反应监测模式同时检测,基质匹配曲线外标法定量。结果13种PSTs的线性方程相关系数(r)均大于0.998,定量限为2~20μg/kg,贻贝基质、牡蛎基质、扇贝基质的平均回收率为92.2%~122%、106%~129%、107%~144%,相对标准偏差均小于11%。将该方法应用于100份贝类样品中PSTs的检测,共有30份样品、5种PSTs检出,总毒性当量(saxitoxin equivalent,STXeq)为10.0~159μg/kg。结论本方法灵敏度高,具有良好的重现性,可以准确定性定量13种PSTs,适用于贝类中PSTs的日常监测。Objective To establish a method for simultaneous determination of 13 kinds of paralytic shellfish toxins(PSTs)in bivalve by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods PSTs in shellfish were extracted with aqueous acetic acid aqueous solution,purified by ethyl acetate,and then it was purified with a graphitized carbon black solid phase extraction column.The samples were separated by UPLC BEH Amide column(100 mm×2.1 mm,1.7μm),simultaneously detected in negative ion multiple reaction monitoring mode(MRM),and quantified by matrix curve external standard method.Results The linear correlation coefficients(r)of 13 PSTs were all greater than 0.998,and the limits of quantitation were 2-20μg/kg.The average recoveries of PTS in the shellfish matrix,oyster matrix and scallop matrix were 92.2%-122%,106%-129%and 107%-144%.The relative standard deviations were less than 11%.The method was applied to the detection of PSTs in 100 shellfish samples.A total of 30 samples and 5 kinds of PSTs were detected.The total toxicity(STXeq)was 10.0-159μg/kg.Conclusion This method has high sensitivity and good reproducibility,can accurately qualitatively quantify 13 kinds of PSTs,and is suitable for daily monitoring of PSTs in shellfish.

关 键 词：麻痹性贝类毒素 超高效液相色谱-串联质谱法 基质效应 贝类 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]