高效液相色谱串联质谱法测定小麦中脱硫丙硫菌唑和戊唑醇残留量

目的]建立一种小麦籽粒和秸秆中脱硫丙硫菌唑和戊唑醇的定量分析方法。方法]小麦籽粒和秸秆样品经过乙腈研磨提取,PSA和C18净化后高效液相色谱串联质谱联用仪测定。脱硫丙硫菌唑和戊唑醇采用电喷雾源正离子扫描模式,外标法定量。结果]脱硫丙硫菌唑和戊唑醇在0.0001~0.01 mg/L范围内具有较好的线性关系,相关系数r>0.9990,小麦籽粒和秸秆中脱硫丙硫菌唑和戊唑醇的平均回收率为87%~105%,相对标准偏差为2.1%~6.1%,定量限均为0.01 mg/kg。结论]该方法操作简单,快速,选择性好,灵敏度高,适用于小麦中脱硫丙硫菌唑和戊唑醇的残留分析。

Determination of Prothioconazole-Desthio and Tebuconazole in Wheat by HPLC-MS/MS

Aims] This study aims to establish a HPLC-MS/MS method for the quantitative determination of prothioconazole-desthio and tebuconazole in wheat grain and straw. Methods] The samples of wheat grain and straw were ground and extracted with acetonitrile, purified with PSA and C18, and determined with HPLC-MS/MS.Prothioconazole-desthio and tebuconazole were quantified by electrospray positive ion source mode and external standard method. Results] The results showed that all the correlation coefficient of calibration curves were over0.9990 in ranged of 0.0001 to 0.01 mg/L. The average recoveries of prothioconazole-desthio and tebuconazole in wheat grain and straw were 87-105%. The relative standard deviations were 2.1-6.1%. The limits of quantification were0.01 mg/kg. Conclusions] The method is simple and fast, with good separation effect and high sensitivity, which is suitable for residue analysis of prothioconazole-desthio and tebuconazole in wheat.