双环磺草酮在稻田环境中的残留分析
目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定稻田环境中双环磺草酮的残留量分析方法。方法 样品经0.02 mol/L盐酸浸泡后, 用乙腈提取, 提取液经石墨化碳黑粉净化, 采用乙腈和0.1%甲酸作为流动相洗脱, 质谱(ESI+)采用多离子检测模式(MRM)对双环磺草酮的定量离子和定性离子进行监测。结果 在0.002~10 mg/L浓度范围内目标物线性良好, 相关系数大于0.9999。双环磺草酮在不同水平的添加回收试验中, 方法的平均回收率为78.5%~100%, 相对标准偏差为0.8%~6.5%, 双环磺草酮的最低检测浓度为0.002 mg/kg。结论 该方法灵敏度、准确度、精密度符合农药残留分析的要求。
Objective To establish a method for residual analysis of benzobicyclon in environment of rice paddies by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Samples were soaked in 0.02 mol/L hydrochloric acid and extracted with acetonitrile. The extracts were purified by graphitized carbon black, and then benzobicyclon residues in the extracts were separated on a reversed phase using elution program of acetonitrile and 0.1% formic acid aqueous solution. The quantitative ion and qualitative ion of benzobicyclon were monitored by UPLC-MS/MS (ESI+) with multiple reactions monitoring (MRM) model. Results The standard calibration curves for benzobicyclon showed high correlation coefficients within 0.002~10 mg/L, with the correlation coefficients more than 0.9999. The average recoveries of benzobicyclon at different spiked levels were between 78.5% and 100%, with the relative standard deviations (RSDs) between 0.8% and 6.5%. The minimum detectable concentration of benzobicyclon were 0.002 mg/kg. Conclusion This method is sensitivity, accuracy and precision, which is suitable for the requirements of the pesticide residue analysis.
标题：双环磺草酮在稻田环境中的残留分析
英文标题：Residual analysis of benzobicyclon in paddy field
作者：
李辉 天津市农业质量标准与检测技术研究所
刘磊 天津市农业质量标准与检测技术研究所
邵辉 天津市农业质量标准与检测技术研究所
李娜 天津市农业质量标准与检测技术研究所
李晶 天津市农业质量标准与检测技术研究所
宋淑荣 天津市农业质量标准与检测技术研究所
郭永泽 天津市农业质量标准与检测技术研究所
张玉婷 天津市农业质量标准与检测技术研究所
中文关键词:双环磺草酮,水稻,残留,分析,
英文关键词:benzobicyclon,paddy,residue,analysis,
发表日期：2017-06-01
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