免疫亲和净化-液相色谱-串联质谱法测定贝类中腹泻性贝类毒素

doi:10.7506/spkx1002-6630-201718047

食品科学 ›› 2017, Vol. 38 ›› Issue (18): 304-309.doi: 10.7506/spkx1002-6630-201718047

免疫亲和净化-液相色谱-串联质谱法测定贝类中腹泻性贝类毒素

严忠雍，张小军,，李奇富，陈思，李佩佩，祝银，刘文静

（1.浙江省海洋水产研究所，浙江?舟山 316021；2.浙江省海洋渔业资源可持续利用技术研究重点实验室，浙江?舟山 316021；3.江苏美正生物科技有限公司，江苏?无锡 214135；4.浙江海洋大学食品与医药学院，浙江?舟山 316021）

出版日期:2017-09-25 发布日期:2017-09-04
基金资助:
浙江省科研院所科技服务项目（2016F30020）；浙江省分析测试科技计划项目（2016C37026）

Determination of Diarrhetic Shellfish Poisons in Shellfish by Immunoaffinity Column Cleanup Coupled with Liquid Chromatography-Mass Spectrometry

YAN Zhongyong, ZHANG Xiaojun,, LI Qifu, CHEN Si, LI Peipei, ZHU Yin, LIU Wenjing

(1. Marine Fisheries Research Institute of Zhejiang, Zhoushan 316021, China;2. Key Laboratory of Sustainable Utilization of Technology Research for Fishery Resource of Zhejiang, Zhoushan 316021, China;3. Jiangsu Meizheng Biotechnology Co. Ltd., Wuxi 214135, China;4. School of Food Science and Pharmaceutics, Zhejiang Ocean University, Zhoushan 316021, China)

Online:2017-09-25 Published:2017-09-04

摘要/Abstract

摘要： 建立贝类中腹泻性贝类毒素的免疫亲和净化-液相色谱-串联质谱分析方法。样品采用80%甲醇溶液提取，选择磷酸盐缓冲液与提取液（4∶1，V/V）混合稀释后，免疫亲和选择专一净化，液相色谱-串联质谱分析。根据腹泻性免疫亲和柱的使用特性，对上样液、淋洗液、洗脱液等参数进行优化。质谱采用电喷雾负离子电离，多反应监测模式，外标法定量。3?种分析物在1.0～100?μg/L质量浓度范围内线性相关系数均大于0.996，对应的检出限和定量限均为0.3?μg/kg和1.0?μg/kg，平均回收率为82.7%～94.3%，相对标准偏差为0.70%～7.61%。本方法基质干扰小、净化效果强、灵敏度高，适合贝类中腹泻性贝类毒素的分析测定。

关键词: 免疫亲和, 液相色谱-串联质谱, 腹泻性贝类毒素

Abstract: A new method using immunoaffinity chromatography (IAC) combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established for the determination of diarrhetic shellfish poisons (DSP) such as okadaic acid (OA), dinophysistoxin-1 (DTX1), pectenotoxin-1 (PTX1) in shellfish. Samples were extracted with 80% methanol, diluted with phosphate buffer, cleaned up by immunoaffinity chromatography, and detected by LC-MS/MS. The major parameters affecting the performance of IAC, including loading amount, washing time and elution conditions, were investigated. Detection was carried out by electrospray ionization in the negative ion mode using multiple reaction monitoring (MRM). The linear range of the analytes was 1.0–100 μg/L with correlation coefficient more than 0.996. The limit of detection (LOD) and limit of quantification (LOQ) for the analytes were calculated as 0.3 and 1.0 μg/kg, respectively. The mean recoveries of the analytes were in the range of 82.7%–94.3% with a relative standard deviation (RSD) of less than 7.61%. Therefore, the method could be used to identify and quantify diarrhetic shellfish poisons in shellfish with less matrix interference and satisfactory sensitivity.

Key words: immunoaffinity chromatography (IAC), liquid chromatography-tandem mass spectrometry (LC-MS/MS), diarrhetic shellfish poison

中图分类号:

TS201.6

严忠雍，张小军,，李奇富，陈思，李佩佩，祝银，刘文静. 免疫亲和净化-液相色谱-串联质谱法测定贝类中腹泻性贝类毒素[J]. 食品科学, 2017, 38(18): 304-309.

YAN Zhongyong, ZHANG Xiaojun,, LI Qifu, CHEN Si, LI Peipei, ZHU Yin, LIU Wenjing. Determination of Diarrhetic Shellfish Poisons in Shellfish by Immunoaffinity Column Cleanup Coupled with Liquid Chromatography-Mass Spectrometry[J]. FOOD SCIENCE, 2017, 38(18): 304-309.

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免疫亲和净化-液相色谱-串联质谱法测定贝类中腹泻性贝类毒素

Determination of Diarrhetic Shellfish Poisons in Shellfish by Immunoaffinity Column Cleanup Coupled with Liquid Chromatography-Mass Spectrometry

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