色谱

色谱 ›› 2017, Vol. 35 ›› Issue (7): 772-777.DOI: 10.3724/SP.J.1123.2017.03046

• 技术与应用 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定水华样品中微囊藻毒素及其基质效应的消除

沈斐1,2, 许燕娟1, 姜晟3, 赵斌1, 石浚哲1, 陈静1   

  1. 1. 无锡市环境监测中心站, 江苏 无锡 214121;
    2. 江南大学环境与土木工程学院, 江苏 无锡 214122;
    3. 江苏省环境监测中心, 江苏 南京 210036
  • 收稿日期:2017-03-31 出版日期:2017-07-08 发布日期:2013-10-18
  • 通讯作者: 沈斐,E-mail:feirenlei911@aliyun.com
  • 基金资助:

    江苏省环境监测科研基金项目（1621）；江苏省普通高校学术学位研究生创新计划项目（KYLX16_0813）；城市河道环境监测技术系统集成研究和示范（WX03-04B0205-051600-07）.

Determination of microcystins in algal bloom samples by ultra performance liquid chromatography-tandem mass spectrometry and elimination of their matrix effects

SHEN Fei1,2, XU Yanjuan1, JIANG Sheng3, ZHAO Bin1, SHI Junzhe1, CHEN Jing1   

  1. 1. Wuxi Environmental Monitoring Central Station, Wuxi 214121, China;
    2. School of Environment and Civil Engineering, Jiangnan University, Wuxi 214122, China;
    3. Jiangsu Environmental Monitoring Center, Nanjing 210036, China
  • Received:2017-03-31 Online:2017-07-08 Published:2013-10-18
  • Supported by:

    Environmental Monitoring and Research Fund of Jiangsu Province (No.1621);Research and Innovation Project for Postgraduate of Higher Education Institutions of Jiangsu Province (No.KYLX16_0813);Research and Demonstration Project of Urban River Environment Monitoring Technology (No.WX03-04B0205-051600-07).

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122

被引次数

4

摘要：

超高效液相色谱-串联质谱法（UPLC-MS/MS）由于其快速、简便的特点，目前广泛应用于水中微囊藻毒素的测定。由于蓝藻水华样品基质比较复杂，UPLC-MS/MS在复杂基质的分析过程中容易发生基质效应问题，严重影响其定量分析结果的准确性。通过稀释样品、优化梯度洗脱程序、减少进样量等方法有效地降低或消除了基质干扰及基质效应问题。7种目标物在各自线性范围内线性关系良好，相关系数（r2）≥0.99；检出限和定量限分别为0.064~0.103 μ g/L和0.213~0.343 μ g/L。通过稀释样品、减少进样量等措施，成功测定了水华爆发时实际样品中的微囊藻毒素，并有效降低了基质效应的干扰。该法为微囊藻毒素的准确测定提供一定的参考，对保障饮用水源地的安全具有十分重要的意义。

关键词: 超高效液相色谱-串联质谱, 基质效应, 水华样品, 微囊藻毒素

Abstract:

A rapid and simple method was commonly used for the determination of microcystins by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The reliability, accuracy and sensitivity of LC-MS/MS determination were affected by the matrix effect because of the complex matrices in algal bloom samples. In this study, the matrix interference and matrix effect problems were effectively reduced or eliminated by diluting samples, optimizing gradient elution programs, and reducing injection volumes. The correlation coefficients (r2) of the seven microcystins were ≥ 0.99. The limits of detection and limits of quantification ranged from 0.064 μ g/L to 0.103 μ g/L and 0.213 μ g/L to 0.343 μ g/L, respectively. Algal bloom samples were determined by diluting 10 times and injecting 5 μ L of sample volume. The method provides some references for the determination of microcystins. It is of great significance for ensuring the safety of drinking water source.

Key words: algal bloom samples, matrix effect, microcystins, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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