双环磺草酮在稻田环境中的残留分析

Residual analysis of benzobicyclon in paddy field

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

中文摘要:

      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。

英文摘要:

      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.