| 高效液相色谱-串联质谱法测定蔬菜中氟虫腈及其代谢物残留 |
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| 引用本文： | 肖国军,蔡超海,王生,覃玲,蔡雅清.高效液相色谱-串联质谱法测定蔬菜中氟虫腈及其代谢物残留[J].现代预防医学,2019,0(7):1260-1263. |
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| 作者姓名： | 肖国军 蔡超海 王生 覃玲 蔡雅清 |
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| 作者单位： | 茂名市疾病预防控制中心,广东 茂名 525000 |
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| 摘 要： | 目的 建立了蔬菜中氟虫腈及其代谢物氟甲腈、氟虫腈砜和氟虫腈亚砜的高效液相色谱-串联质谱法。方法 用乙腈超声提取样品中的氟虫腈及其代谢物,高速离心后,提取液经QuChERS净化管净化,过0.22μm滤膜,经Waters Acquity UPLC HSS T3色谱柱分离,以乙腈-0.1%甲酸水(含5mmol/L乙酸铵)做流动相,梯度洗脱,采用电喷雾离子源负离子检测模式(ESI-)和多重反应监测(MRM)模式测定,基质匹配标准曲线定量。结果 在蔬菜基质中,被测物在1.0 μg/L～100 μg/L内相关系数均>0.999,平均回收率范围为97.8%～109%,相对标准偏差(RSD)为1.0%～7.7%,检出限为0.02μg/kg～0.10μg/kg,定量限为0.06μg/kg～0.30μg/kg。结论 该方法操作简单、准确、快速、灵敏度高,适用于蔬菜中氟虫腈及其代谢物残留的检测。
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| 关 键 词： | 氟虫腈 高效液相色谱串联质谱法 QuChERS 蔬菜 |
Determination of fipronil and its metabolites residues in vegetables by high-performance liquid chromatography-tandem mass spectrometry |
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| XIAO Guo-jun,CAI Chao-hai,WANG Sheng,QIN Ling,CAI Ya-qing.Determination of fipronil and its metabolites residues in vegetables by high-performance liquid chromatography-tandem mass spectrometry[J].Modern Preventive Medicine,2019,0(7):1260-1263. |
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| Authors: | XIAO Guo-jun CAI Chao-hai WANG Sheng QIN Ling CAI Ya-qing |
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| Affiliation: | Maoming Center for Disease Control and Prevention,Maoming,Guangdong 525000,China |
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| Abstract: | Objective To establish a method for the determination of fipronil and its metabolites(fluoro formonitrile,fipronil sulfone and fipronil sulfoxide)residues in vegetables by high-performance liquid chromatography-tandem mass spectrometry.Methods The fipronil and its metabolites were extracted ultrasonically with acetonitrile.After high-speed centrifugation,the extract was purified by QuChERS purification tube,and then filtrated with 0.22 m filter membrane,and finally separated with a Waters Acquity UPLC HSS T3 chromatographic column gradient elution mode.Acetonitrile-0.1% formic acid water(containing 5mmol/L ammonium acetate)was used as a mobile phase.Gradient elution was carried out using electrospray ion source negative ion detection mode(ESI-)and multiple reactions monitoring(MRM)mode,and the quantifications were based on matrix matching standard curves.Results The method had a good linearity in the range of 1.0μg/L-100μg/L with the correlation coefficients greater than 0.999.The average recovery rates of the method were 97.8%-100% with the relative standard deviations(RSDs)of 1.0%-7.7%.The limits were 0.02μg/kg-0.10μg/kg,and the limits of quantification were 0.06μg/kg-0.30μg/kg.Conclusion The method is simple,accurate,rapid and sensitive.It is suitable for the determination of fipronil and its metabolites residues in vegetables. |
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| Keywords: | Fipronil High-performance liquid chromatography-tandem mass spectrometry QuChERS Vegetables |
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