高效液相色谱-串联质谱法测定环境水样中多种杀菌剂残留量

引用本文: 王岩松, 贺明睿, 张春野, 范世华, 马吉, 李华锋. 高效液相色谱-串联质谱法测定环境水样中多种杀菌剂残留量[J]. 分析化学, 2012, 40(11): 1764-1771. doi: 10.3724/SP.J.1096.2012.20100 shu

Citation: WANG Yan-Song, HE Ming-Rui, ZHANG Chun-Ye, FAN Shi-Hua, MA Ji, LI Hua-Feng. Determination of Multiresidual Fungicides in Environmental Water Samples by High Performance Liquid Chromatography Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2012, 40(11): 1764-1771. doi: 10.3724/SP.J.1096.2012.20100 shu

高效液相色谱-串联质谱法测定环境水样中多种杀菌剂残留量

王岩松 ^{1,2,
,} ,
贺明睿 ^2, ,
张春野 ^2, ,
范世华 ^1, ,
马吉 ^2, ,
李华锋 ^2,

通讯作者: 王岩松

摘要: 建立了环境水样中多种杀菌剂残留量的高效液相-串联质谱(LC-MS/MS)分析方法。通过氟吗啉和烯酰吗啉的光照实验,研究了其顺反异构体的转化规律,确定了它们的色谱行为。优化了固相萃取(SPE)过程参数,选择HLB为固相萃取柱,4 mL甲醇-水(12:88, V/V)为淋洗液,3 mL甲醇为洗脱液。分析了环境水样中多种杀菌剂的基质效应影响,采用基质匹配曲线消除了基质效应。采用液相色谱分离,正离子多反应监测模式进行质谱分析。多种杀菌剂的方法定量限为0.003-0.03 μg/L (环酰菌胺0.3 μg/L)。在各自分析物的线性范围内, 回收率为70.2%-108.9%,相对标准偏差均小于16.7%。本方法具有快速、准确、灵敏度高、选择性好等特点。在辽宁地区环境水样检测中,蒲河水检出嘧菌酯0.051 μg/L、精甲霜灵0.217 μg/L和烯酰吗啉0.015 μg/L,浑河水检测出烯酰吗啉0.004 μg/L。

关键词:

English

Determination of Multiresidual Fungicides in Environmental Water Samples by High Performance Liquid Chromatography Tandem Mass Spectrometry

1.
¹ College of Sciences, Northeastern University, Shenyang 110004, China;

Corresponding author: 王岩松

Received Date: 09 February 2012

Abstract: A sensitive multiresidual analytical method for simultaneous analysis of multiresidual fungicides in environmental water samples was developed. The method was based on solid phase extraction (SPE) followed by high performance liquid chromatography tandem mass spectrometry (LC-MS/MS). Qualitative and quantitative detection for the analytes was carried out under the multiple reaction monitoring (MRM) in positive ionization mode after chromatography separation. In this method we have studied the conversion rule, identified the chromatogram retention time of Z-isomer and E-isomer of flumorph and dimethomorph, confirmed their chromatographic behavior by monitoring concentrations of two isomers of them at room temperature under sunlight and optimized parameters that may affect the SPE procedure efficiency: the column type, the wash solvent and the elution solvent. The recoveries of the SPE gave levels ranged from 70.18% to 108.87%, all recoveries were acceptable, with relative standard deviation (RSD) ≤16.7%. The limit of quantification (LOQ, S/N=10) varied between 0.003 and 0.03 μg/L (except for fenhexamid 0.3 μg/L). The developed method was applied for the determination of multiresidual fungicides in 100 tap water samples and 6 environmental samples collected from Liaoning province in China. Total fungicides were not found in tap water samples. Azoxystrobin (0.051 μg/L), metalaxyl (0.217 μg/L) and dimethomorph (Z, E) (0.015 μg/L) were found in Pu river sample, dimethomorph (Z, E) (0.004 μg/L) was found in Hun river sample, the highest concentration level of metalaxyl was 0.217 μg/L in Pu river, the rest of fungicides remained undetected in river samples.

Key words:

Liquid chromatography-tandem mass spectrometry
/ Multiresidual fungicides
/ Solid phase extratione
/ Modifier
/ Environmental water

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

高效液相色谱-串联质谱法测定环境水样中多种杀菌剂残留量

通讯作者: 王岩松

English

Determination of Multiresidual Fungicides in Environmental Water Samples by High Performance Liquid Chromatography Tandem Mass Spectrometry

Corresponding author: 王岩松

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

高效液相色谱-串联质谱法测定环境水样中多种杀菌剂残留量

通讯作者: 王岩松

English

Determination of Multiresidual Fungicides in Environmental Water Samples by High Performance Liquid Chromatography Tandem Mass Spectrometry

Corresponding author: 王岩松

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

中国化学会秘书处

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