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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0.02mol/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0.002~10mg/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0.002mg/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 the determination of bicyclovlosulamone in paddy field by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods After the sample was soaked in 0.02mol / L hydrochloric acid, the sample was extracted with acetonitrile. The extract was purified by carbonized carbon black powder and eluted with acetonitrile and 0.1% formic acid as mobile phase. The mass spectrometry (ESI) The quantitative ion and qualitative ions of belcontamone are monitored. Results The target was linear in the range of 0.002 ~ 10 mg / L with the correlation coefficient greater than 0.9999. The results showed that the average recoveries were about 78.5% -100% with RSDs of 0.8% ~ 6.5%. The minimum detectable concentration of bicyclovlosulazone was 0.002 mg / kg. Conclusion The sensitivity, accuracy and precision of this method are in line with the requirements of pesticide residue analysis.