赵桦林, 邱静, 王敏, 杨曙明, 柴婷婷, 叶小兰. 加速溶剂萃取-液相色谱-串联质谱法同步检测白菜中的丁硫克百威及其代谢物残留[J]. 农药学学报, 2013, 15(2): 204-210.
    引用本文: 赵桦林, 邱静, 王敏, 杨曙明, 柴婷婷, 叶小兰. 加速溶剂萃取-液相色谱-串联质谱法同步检测白菜中的丁硫克百威及其代谢物残留[J]. 农药学学报, 2013, 15(2): 204-210.
    ZHAO Hualin, QIU Jing, WANG Min, YANG Shuming, CHAI Tingting, YE Xiaolan. Simultaneous determination of carbosulfan and its metabolites in Chinese cabbage by ASE-LC-MS/MS[J]. Chinese Journal of Pesticide Science, 2013, 15(2): 204-210.
    Citation: ZHAO Hualin, QIU Jing, WANG Min, YANG Shuming, CHAI Tingting, YE Xiaolan. Simultaneous determination of carbosulfan and its metabolites in Chinese cabbage by ASE-LC-MS/MS[J]. Chinese Journal of Pesticide Science, 2013, 15(2): 204-210.

    加速溶剂萃取-液相色谱-串联质谱法同步检测白菜中的丁硫克百威及其代谢物残留

    Simultaneous determination of carbosulfan and its metabolites in Chinese cabbage by ASE-LC-MS/MS

    • 摘要: 建立了白菜中丁硫克百威及其代谢物克百威、3-羟基克百威和3-酮基克百威的同步检测方法。白菜样品匀浆后用硅藻土混合分散,经加速溶剂萃取仪(ASE)用二氯甲烷萃取,固相萃取柱净化,在液相色谱-串联质谱(LC-MS/MS)仪上采用正电离方式以多反应监测模式(MRM)检测,内标法定量。丁硫克百威及其3种代谢物在白菜中的平均回收率在85%~122%之间,相对标准偏差为2.3%~12.5%,检出限为0.002~0.01 mg/kg,定量限为0.005~0.02 mg/kg。采用该方法测定的消解动态结果表明:丁硫克百威在白菜中的消解半衰期为0.9 d,代谢物克百威在施药当天即达到最大值,并在1 d内消解70%以上,而3-羟基克百威与3-酮基克百威的浓度则在1 d时达到最大值,然后呈现快速降低的趋势。

       

      Abstract: An analytical method was developed for simultaneous determination of carbosulfan and other metabolites in Chinese cabbage.The analytes were extracted from the dispersed samples with diatomite by accelerated solvent extraction (ASE) using methylene chloride as solvent,purified with solid phase extraction column (SPE),analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive electro-spray ionization (ESI+) with multi-reaction monitoring (MRM) mode,and quantified by matrix internal standard method.The recoveries ranged from 85% to 122% with relative standard deviations (RSD) varying between 2.3% and 12.5%.The limits of detection (LOD) were from 0.002 to 0.01 mg/kg and the limits of quantification (LOQ) from 0.005 to 0.02 mg/kg.The developed method was successfully applied to study dissipation of carbosulfan in Chinese cabbage,the short half-life of 0.9 d showed that carbosulfan can be quickly degraded to its three metabolites.The maximum residue of carbofuran was exhibited in the day of application,and dissipated about 70% in 1 d.However,the maximum residues of 3-hydroxycarbofuran and 3-keto-carbofuran were exhibited 1 d after application,and were quickly dissipated in Chinese cabbage.

       

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