超高效液相色谱-串联质谱法测定海水悬浮颗粒物中的8种典型脂溶性藻毒素

引用本文: 王艳龙, 陈军辉, 高莉媛, 王帅, 郑晓玲, 孙承君, 王小如. 超高效液相色谱-串联质谱法测定海水悬浮颗粒物中的8种典型脂溶性藻毒素[J]. 分析化学, 2016, 44(3): 335-341. doi: 10.11895/j.issn.0253-3820.150714 shu

Citation: WANG Yan-Long, CHEN Jun-Hui, GAO Li-Yuan, WANG Shuai, ZHENG Xiao-Ling, SUN Cheng-Jun, WANG Xiao-Ru. Determination of Eight Typical Lipophilic Algae Toxins in Particles Suspended in Seawater by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2016, 44(3): 335-341. doi: 10.11895/j.issn.0253-3820.150714 shu

超高效液相色谱-串联质谱法测定海水悬浮颗粒物中的8种典型脂溶性藻毒素

王艳龙 ^1, ,
陈军辉 ^{1,2,
,} ,
高莉媛 ^1, ,
王帅 ^1,2, ,
郑晓玲 ^1, ,
孙承君 ^1, ,
王小如 ^1,

1.
¹ 国家海洋局第一海洋研究所, 海洋生态研究中心, 青岛 266061;
2.
² 青岛海洋科学与技术国家实验室, 海洋生态与环境科学功能实验室, 青岛 266071

通讯作者: 陈军辉

基金项目:
本文系国家基金委-山东省联合基金项目(No.U1406403) (No.U1406403)

中央级公益性科研院所基本科研业务费专项(No.2014T05) (No.2014T05)

山东省自然科学基金(No.ZR2015PD003) (No.ZR2015PD003)

2012泰山学者海外人才项目资助

摘要: 海水悬浮颗粒物对海洋环境中污染物的迁移转化有着重要的影响,在海水悬浮颗粒物上富集的脂溶性藻毒素会严重的毒害海洋滤食性生物。本研究建立了海水悬浮颗粒物中8种典型脂溶性藻毒素同步测定的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。海水悬浮颗粒物样品经甲醇超声辅助提取后,以5 mmol/L 乙酸铵水溶液和乙腈为流动相,经1.7微米C₁₈色谱柱分离,采用电喷雾串联质谱(ESI-MS/MS)多反应监测 (MRM )模式检测,外标法定量。结果表明,在最佳实验条件下,8种目标物在5 min内分离良好,加标回收率在83.8%~110.4%之间,方法具有良好的精密度(相对标准偏差(RSD)≤14.1%)和灵敏度(检出限介于2.9~103 pg/g之间),在线性范围内,相关系数(R²)均大于0.996,能满足海水悬浮颗粒物中8种典型脂溶性藻毒素同步检测的要求。采用本方法初步分析了青岛沿岸海域海水悬浮颗粒物中的脂溶性藻毒素,其中PTX2被检出,含量最高可达790 pg/g(干重)。

关键词:

English

Determination of Eight Typical Lipophilic Algae Toxins in Particles Suspended in Seawater by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

1.
¹ Research Center for Marine Ecology, The First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China;
2.
² Laboratory of Marine Ecology and Environmental Science, Qingdao National Laboratory for Marine Science and Technology, Qingdao 266071, China

Corresponding author: 陈军辉

Received Date: 09 September 2015
Fund Project:
本文系国家基金委-山东省联合基金项目(No.U1406403)

中央级公益性科研院所基本科研业务费专项(No.2014T05)

山东省自然科学基金(No.ZR2015PD003)

2012泰山学者海外人才项目资助

Abstract: The particles suspended in seawater have great influence on pollutant migration and transformation in marine environment, while the lipophilic algae toxins enriched by the particles suspended in seawater will lead more serious toxicity to marine filter feeders. In this study, a new method was developed for the simultaneous determination of eight lipophilic algae toxins in suspended particles by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). After extracted with methanol by ultrasonic-assisted extraction, the sample was separated on an Acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 μm) using gradient elution of acetonitrile and water containing 5 mmol/L ammonium acetate as eluent modifiers. The qualitative and quantitative analyses were carried out by electrospray ionization (ESI) tandem mass spectrometry in multiple reaction monitoring (MRM) mode. Under the optimal conditions, satisfactory precision (relative standard deviations (RSD≤14.1%), recoveries (83.8%-110.4%) and detection limits (2.9-103 pg/g) of the method were achieved. Good linearity (R²≥0.99) was also obtained for all studied analytes. Then, the method was applied to determine the amounts of the eight lipophilic marine toxins in authentic suspended particle samples collected from Qingdao near-shore area. Pectenotoxin 2 (PTX2) was detected in the samples from Shilaoren beach and No. 3 bathing beach with concentration ranges of 717 and 790 pg/g, respectively.

Key words:

Ultra performance liquid chromatography-tandem mass spectrometry
/ Lipophilic algae toxins
/ Seawater
/ Suspended particles
/ Pectenotoxin 2

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

超高效液相色谱-串联质谱法测定海水悬浮颗粒物中的8种典型脂溶性藻毒素

通讯作者: 陈军辉

English

Determination of Eight Typical Lipophilic Algae Toxins in Particles Suspended in Seawater by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: 陈军辉

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

超高效液相色谱-串联质谱法测定海水悬浮颗粒物中的8种典型脂溶性藻毒素

通讯作者: 陈军辉

English

Determination of Eight Typical Lipophilic Algae Toxins in Particles Suspended in Seawater by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: 陈军辉

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

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