QuEChERS-超高效液相色谱-串联质谱法快速测定小麦及土壤中环丙唑醇的残留

Rapid detection of cyproconazole in wheat and soil by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

目的建立Qu ECh ERS-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)快速测定小麦及土壤中环丙唑醇的残留的方法。方法小麦籽粒与秸秆及土壤经纯水浸泡、乙腈振荡提取并离心后,上清液加乙二胺-N-丙基硅烷(primary-secondary amine,PSA)和硫酸镁混合净化,高速离心后取净化上清液用流动相定容,经0.22μm尼龙膜过滤后上机检测。结果本方法在0.001~0.400 mg/L浓度范围内线性响应均良好,相关系数在0.9994~0.9997之间。环丙唑醇在小麦籽粒中的添加水平为0.010~1.000mg/kg,平均回收率为92%~98%,相对标准偏差(relative standard deviations,RSDs)均不超过1.6%(n=5);在小麦秸秆中的添加水平为0.010~5.000 mg/kg,平均回收率为72%~104%,RSDs均不超过1.7%(n=5);在土壤中的添加水平为0.010~5.000 mg/kg,平均回收率为91%~103%,RSDs均不超过2.1%(n=5)。结论本方法简单快速、灵敏度高、准确度和精密度好,能满足小麦及土壤中环丙唑醇残留分析的需要。

Objective To establish a method for the rapid determination of cyproconazole residues in wheat and soil by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods After wheat seeds,straw and soil were soaked in pure water,extracted by acetonitrile oscillation and centrifuged,the supernatant was mixed with primary secondary amine(PSA) and magnesium sulfate for purification.After high-speed centrifugation,the purified supernatant was fixed to volume with mobile phase and purified by 0.22 μm nylon membrane and tested for on-line detection Results This method had good linear responses in the range of 0.001-0.400 mg/L,and the correlation coefficients were 0.9994-0.9997.When the addition levels of cyproconazole were 0.010-1.000 mg/kg in wheat grain,the average recoveries were 92%-98%,and relative standard deviations(RSDs) were no more than 1.6%(n=5);when the addition levels were 0.010-5.000 mg/kg in wheat straw,the average recoveries were 72%-104%,and RSDs were no more than 1.7%(n=5);when the addition levels were 0.010-5.000 mg/kg in wheat straw,the average recoveries were 91%-103%,and RSDs were no more than 2.1%(n=5).Conclusion This method is simple,fast,sensitive,accurate and reliable,which is suitable for the detection of cyproconazole residues in wheat and soil.