色谱

色谱 ›› 2012, Vol. 30 ›› Issue (01): 51-55.DOI: 10.3724/SP.J.1123.2011.09003

• 研究论文 • 上一篇    下一篇

固相萃取-超高效液相色谱-电喷雾串联质谱法同时测定地表水中9种微囊藻毒素

张明*, 唐访良, 陈峰, 徐建芬, 张丽娜   

  1. 杭州市环境监测中心站, 浙江 杭州 310007
  • 收稿日期:2011-09-03 修回日期:2011-10-03 出版日期:2012-01-28 发布日期:2012-03-01
  • 通讯作者: 张明,硕士,工程师,主要从事环境监测技术及方法研究. Tel: (0571)87998257,
  • 基金资助:

    杭州市环境保护科技项目(No.2011002).

Simultaneous determination of nine microcystins in surface water by solid phase extraction and ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry

ZHANG Ming*, TANG Fangliang, CHEN Feng, XU Jianfen, ZHANG Lina   

  1. Hangzhou Environmental Monitoring Central Station, Hangzhou 310007, China
  • Received:2011-09-03 Revised:2011-10-03 Online:2012-01-28 Published:2012-03-01

PDF

381

被引次数

50

摘要： 建立了固相萃取-超高效液相色谱-电喷雾串联三重四极杆质谱(SPE-UPLC-ESI-MS/MS)联用技术分析水中9种微囊藻毒素的方法。样品经SPE提取和净化后,以Waters ACQUITY UPLCTM BEH C18色谱柱为分离柱,以含0.1%甲酸乙腈和含0.1%甲酸水作为流动相进行梯度洗脱,电喷雾离子源电离、正离子多反应监测模式质谱进行定性和定量分析。9种微囊藻毒素在0.1～50 μg/L或0.5～100 μg/L质量浓度范围内线性良好,相关系数为0.9990～0.9998,方法的检出限(以3倍信噪比计)为0.1～0.5 ng/L;高、中、低3个添加水平的回收率为75.8%～109%,相对标准偏差为0.49%～10.0%。结果表明,该方法灵敏、准确,检测范围广,分析速度快。应用该方法检测了杭州市两处水库水样中的微囊藻毒素,分别检出了3种和8种微囊藻毒素。

关键词: 超高效液相色谱-电喷雾串联质谱, 地表水, 固相萃取, 微囊藻毒素

Abstract: A method has been developed for the simultaneous determination of nine microcystins (MCs) in surface water by solid phase extraction-ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (SPE-UPLC-ESI-MS/MS). The samples were enriched and purified by an HLB solid phase extraction column. The separation was performed on an ACQUITY UPLCTM system with a BEH C18 column with the gradient elution of acidified acetonitrile and water (both containing 0.1%(v/v) formic acid). The nine MCs were determined in the modes of electrospray positive ionization (ESI+) and multiple reaction monitoring (MRM). Good linearities were observed in the ranges of 0.1~50 μg/L for MC-RR and 0.5~100 μg/L for the others with correlation coefficients over 0.9990 and the limits of detection for the nine MCs were in the range of 0.1~0.5 ng/L. The recoveries were in the range of 75.8%~109% in the three spiked levels of 1.0, 10 and 50 μg/L with the relative standard deviations of 0.49%~10.0%. The method is characterized by high sensitivity and precision, extensive analytical range and quick analytical rate. This method was used in the analysis of water samples from two reservoirs situated in Hangzhou, and the 3 and 8 microcystins were detected individually.

Key words: microcystins, surface water, ultra performance liquid chromatography-electro- spray ionization tandem mass spectrometry (UPLC-ESI-MS/MS), solid phase extraction (SPE)