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

中文关键词:  环丙唑醇  小麦  土壤  QuEChERS  超高效液相色谱-串联质谱法

英文关键词:cyproconazole  wheat  soil  QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立QuEChERS-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0.22 μm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0.010~1.000 mg/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。

英文摘要:

      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.