固相萃取-高效液相色谱-串联质谱法同时测定蔬菜中8种磺胺类抗生素

吴小莲; 包艳萍; 向垒; 严青云; 姜元能; 李彦文; 黄献培; 莫测辉

doi:10.7524/j.issn.0254-6108.2013.06.018

环境化学

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吴小莲, 包艳萍, 向垒, 严青云, 姜元能, 李彦文, 黄献培, 莫测辉. 固相萃取-高效液相色谱-串联质谱法同时测定蔬菜中8种磺胺类抗生素[J]. 环境化学, 2013, 32(6): 1038-1044. doi: 10.7524/j.issn.0254-6108.2013.06.018

引用本文:

WU Xiaolian, BAO Yanping, XIANG Lei, YAN Qingyun, JIANG Yuanneng, LI Yanwen, HUANG Xianpei, MO Cehui. Simultaneous determination of eight sulfonamide antibiotics in vegetables using solid phase extraction and high performance liquid chromatography coupled with mass spectrometry[J]. Environmental Chemistry, 2013, 32(6): 1038-1044. doi: 10.7524/j.issn.0254-6108.2013.06.018

Citation:

WU Xiaolian, BAO Yanping, XIANG Lei, YAN Qingyun, JIANG Yuanneng, LI Yanwen, HUANG Xianpei, MO Cehui. Simultaneous determination of eight sulfonamide antibiotics in vegetables using solid phase extraction and high performance liquid chromatography coupled with mass spectrometry[J]. Environmental Chemistry, 2013, 32(6): 1038-1044. doi: 10.7524/j.issn.0254-6108.2013.06.018

固相萃取-高效液相色谱-串联质谱法同时测定蔬菜中8种磺胺类抗生素

1.
暨南大学环境工程系, 广东省高校水土环境毒害性污染物防治与生物修复重点实验室, 广州, 510632;
2.
暨南大学水生生物研究所, 广州, 516032
基金项目:
国家自然科学基金项目(41173101)

广东省自然科学基金重点项目(20110200003196)

广东高校高层次人才项目资助.

Simultaneous determination of eight sulfonamide antibiotics in vegetables using solid phase extraction and high performance liquid chromatography coupled with mass spectrometry

1.
Key Laboratory of water/soil toxic pollutants control and bioremediation of Guangdong Higher Education Institutions, Department of Environmental Engineering, Jinan University, Guangzhou, 510630;
2.
National Key Disicpline of Hydrobiology, Jinan University, Guangzhou, 510632
Fund Project:

摘要: 建立了固相萃取-高效液相色谱-串联质谱同时测定蔬菜中8种磺胺类抗生素(SAs)的分析方法.以10 mL乙腈(添加2 g无水硫酸钠、0.1 g乙酸钠、0.1 g Na2EDTA)进行提取,HLB柱净化富集.采用RESTEK Pinnacle Ⅱ C18色谱柱,以水(含0.1%甲酸)和乙腈(含0.1%甲酸)为初始流动相进行梯度洗脱.在电喷雾-多反应检测离子模式下,进行定性定量分析.SMZ的方法定量限为0.2 μg·kg-1,其它7种化合物的定量限均为0.1 μg·kg-1.不同加标浓度(5-100 μg·kg-1)下8种SAs的回收率大部分约在70%以上,相对标准偏差(RSD)多数小于10%,表明该方法能够满足实际样品的分析要求.利用该方法对某无公害蔬菜基地进行分析,蔬菜中检出3种以上磺胺类抗生素,含量在0.20-17.43 μg·kg-1 (干重)之间,总含量在2.42-27.60 μg·kg-1之间.
- 磺胺类抗生素(SAs) /
- 高效液相色谱-串联质谱法(HPLC-MS/MS) /
- 蔬菜
Abstract: An analytical method for the simultaneous determination of eight sulfonamide antibiotics(sulfadimethoxine, sulfpyride, sulfamethazine, sulfathiazole, sulfamerazine, sulfamethoxazole, sulfameter and sulfadiazine)in vegetables was presented using solid phase extraction and high performance liquid chromatography coupled with mass spectrometry. Vegetable samples were extracted by acetonitrile (containing 2 g anhydrous sodium sulfate, 0.1 g sodium acetate and 0.1 g disodium ethylenediamine tetraacetate), then purified and enriched by the HLB column. The sulfonamide antibiotics were separated on RESTEK Pinnacle Ⅱ C18 column with mobile phase containing 0.1% acetic acid and acetonitrile (0.1% acetic acid) and then determined by electrospray ionization mass spectrometry(ESI-MS). The quantitative limits of method were 0.2 μg·kg-1 for SMZ and 0.1 μg·kg-1 for the other seven analytes. Recoveries were mostly above 70% and relative standard deviation (RSD) was mostly under 10% at various spiking levels The method was successfully applied to test sulfonamides in vegetable samples with total content from 2.42 μg·kg-1 to 27.60 μg·kg-1.
- sulfonamide antibiotics /
- HPLC-MS/MS /
- vegetables

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WU Xiaolian, BAO Yanping, XIANG Lei, YAN Qingyun, JIANG Yuanneng, LI Yanwen, HUANG Xianpei, MO Cehui. Simultaneous determination of eight sulfonamide antibiotics in vegetables using solid phase extraction and high performance liquid chromatography coupled with mass spectrometry[J]. Environmental Chemistry, 2013, 32(6): 1038-1044. doi: 10.7524/j.issn.0254-6108.2013.06.018

固相萃取-高效液相色谱-串联质谱法同时测定蔬菜中8种磺胺类抗生素

1. 暨南大学环境工程系, 广东省高校水土环境毒害性污染物防治与生物修复重点实验室, 广州, 510632;
2. 暨南大学水生生物研究所, 广州, 516032

收稿日期: 2012-09-18

基金项目:

国家自然科学基金项目(41173101)

广东省自然科学基金重点项目(20110200003196)

广东高校高层次人才项目资助.

关键词:

摘要: 建立了固相萃取-高效液相色谱-串联质谱同时测定蔬菜中8种磺胺类抗生素(SAs)的分析方法.以10 mL乙腈(添加2 g无水硫酸钠、0.1 g乙酸钠、0.1 g Na2EDTA)进行提取,HLB柱净化富集.采用RESTEK Pinnacle Ⅱ C18色谱柱,以水(含0.1%甲酸)和乙腈(含0.1%甲酸)为初始流动相进行梯度洗脱.在电喷雾-多反应检测离子模式下,进行定性定量分析.SMZ的方法定量限为0.2 μg·kg-1,其它7种化合物的定量限均为0.1 μg·kg-1.不同加标浓度(5-100 μg·kg-1)下8种SAs的回收率大部分约在70%以上,相对标准偏差(RSD)多数小于10%,表明该方法能够满足实际样品的分析要求.利用该方法对某无公害蔬菜基地进行分析,蔬菜中检出3种以上磺胺类抗生素,含量在0.20-17.43 μg·kg-1 (干重)之间,总含量在2.42-27.60 μg·kg-1之间.

English Abstract

Simultaneous determination of eight sulfonamide antibiotics in vegetables using solid phase extraction and high performance liquid chromatography coupled with mass spectrometry

1. Key Laboratory of water/soil toxic pollutants control and bioremediation of Guangdong Higher Education Institutions, Department of Environmental Engineering, Jinan University, Guangzhou, 510630;
2. National Key Disicpline of Hydrobiology, Jinan University, Guangzhou, 510632

Received Date: 2012-09-18

Fund Project:

Keywords:

Abstract: An analytical method for the simultaneous determination of eight sulfonamide antibiotics(sulfadimethoxine, sulfpyride, sulfamethazine, sulfathiazole, sulfamerazine, sulfamethoxazole, sulfameter and sulfadiazine)in vegetables was presented using solid phase extraction and high performance liquid chromatography coupled with mass spectrometry. Vegetable samples were extracted by acetonitrile (containing 2 g anhydrous sodium sulfate, 0.1 g sodium acetate and 0.1 g disodium ethylenediamine tetraacetate), then purified and enriched by the HLB column. The sulfonamide antibiotics were separated on RESTEK Pinnacle Ⅱ C18 column with mobile phase containing 0.1% acetic acid and acetonitrile (0.1% acetic acid) and then determined by electrospray ionization mass spectrometry(ESI-MS). The quantitative limits of method were 0.2 μg·kg-1 for SMZ and 0.1 μg·kg-1 for the other seven analytes. Recoveries were mostly above 70% and relative standard deviation (RSD) was mostly under 10% at various spiking levels The method was successfully applied to test sulfonamides in vegetable samples with total content from 2.42 μg·kg-1 to 27.60 μg·kg-1.

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固相萃取-高效液相色谱-串联质谱法同时测定蔬菜中8种磺胺类抗生素

Simultaneous determination of eight sulfonamide antibiotics in vegetables using solid phase extraction and high performance liquid chromatography coupled with mass spectrometry

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固相萃取-高效液相色谱-串联质谱法同时测定蔬菜中8种磺胺类抗生素

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Simultaneous determination of eight sulfonamide antibiotics in vegetables using solid phase extraction and high performance liquid chromatography coupled with mass spectrometry

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