色谱

色谱 ›› 2017, Vol. 35 ›› Issue (8): 794-800.DOI: 10.3724/SP.J.1123.2017.04018

• 研究论文 • 上一篇    下一篇

通过型固相萃取-液相色谱-串联质谱法同时快速测定鱼肉中7种微囊藻毒素

李诗言1,2, 王扬1, 王鼎南1, 吴洪喜1, 丁雪燕1, 崔益玮2, 沈清2   

  1. 1. 浙江省水产质量检测中心, 浙江 杭州 310023;
    2. 浙江工商大学海洋食品研究院, 浙江 杭州 310012
  • 收稿日期:2017-04-17 出版日期:2017-08-08 发布日期:2013-11-25
  • 通讯作者: 王扬,Tel:85029759,E-mail:wangyangruanfeng@163.com;沈清,Tel:88071024,E-mail:leonqshen@163.com
  • 基金资助:

    浙江省水产品质量安全技术支撑团队项目（QS2016001）.

Rapid and simultaneous determination of seven microcystins in fish meat by liquid chromatography-tandem mass spectrometry coupled with pass-through solid phase extraction

LI Shiyan1,2, WANG Yang1, WANG Dingnan1, WU Hongxi1, DING Xueyan1, CUI Yiwei2, SHEN Qing2   

  1. 1. Aquatic Products Quality Inspection Center of Zhejiang Province, Hangzhou 310023, China;
    2. Institute of Seafood, Zhejiang Gongshang University, Hangzhou 310012, China
  • Received:2017-04-17 Online:2017-08-08 Published:2013-11-25
  • Supported by:

    Zhejiang Province Technical Team Projects for Quality and Safety of Aquatic Products (No. QS2016001).

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摘要：

采用通过型固相萃取净化去除样品基质中脂类物质的干扰，建立了鱼肉中7种微囊藻毒素的液相色谱-串联质谱快速分析方法。样品经80℃水浴热处理后用体积分数为90%的甲醇水溶液进行提取，使用Oasis PRiME HLB通过型固相萃取柱净化。净化后的样品采用Waters XSelect HSS T3色谱柱分离，以0.1%（体积分数）甲酸乙腈溶液和0.1%（体积分数）甲酸水溶液为流动相，梯度洗脱，多反应监测正离子模式扫描，采用基质匹配溶液外标法定量。研究了7种微囊藻毒素的质谱离子化特征，结果表明，酸能显著增加双电荷离子的响应强度。7种目标物在相关范围内线性关系良好，相关系数不低于0.99，定量限为0.30~2.0 μ g/kg，基质加标回收率为70.6%~96.1%，相对标准偏差为3.4%~9.6%。该方法前处理操作简便，灵敏度和准确度高，可实现鱼肉中多种微囊藻毒素的同时快速测定。

关键词: 双电荷离子, 通过型固相萃取, 微囊藻毒素, 液相色谱-串联质谱, 鱼肉

Abstract:

An analytical method was developed for the simultaneous and rapid determination of seven microcystins in fish meat by liquid chromatography-tandem mass spectrometry (LC-MS/MS) coupled with pass-through solid phase extraction (SPE). The samples were extracted with methanol-water (90:10, v/v) after heat treatment by water bath at 80℃, and then cleaned up with an Oasis PRiME HLB pass-through SPE column. The samples were analyzed directly on a Waters XSelect HSS T3 column using 0.1% (v/v) aqueous formic acid and acidified acetonitrile (0.1% formic acid, v/v) as mobile phases. Qualitative and quantitative analysis of the analytes was carried out under the multiple reaction monitoring mode with positive electrospray ionization. The matrix matching external standard method was used for quantitation analysis. To solve the problem of parent ion selection of the microcystins, the ionization characteristics of microcystins were evaluated under different mobile phase conditions. Finally, the results showed that the acid could promote the intensity of the doubly charged ions significantly. The calibration curves were linear well in the corresponding concentration ranges, with correlation coefficient ≥ 0.99. The limits of quantification ranged from 0.30 to 2.0 μ g/kg. The average spiked recoveries for the seven microcystins were between 70.6% and 96.1% with the relative standard deviations of 3.4%-9.6%. The proposed method is sensitive, accurate, and efficient. It is applicable for the determination of microcystins in fish meat.

Key words: doubly charged ions, fish meat, liquid chromatography-tandem mass (LC-MS/MS), microcystin (MC), pass-through solid-phase extraction

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