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  

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

作　　者：贾福艳[1,2] 黄鑫 杨沛文[1,2] 丁琦 刘良月 杨雪葳[1,2] 刘修园 张双 黄成田 JIA Fu-yan;HUANG Xin;YANG Pei-wen;DING Qi;LIU Liang-yue;YANG Xue-wei;LIU Xiu-yuan;ZHANG Shuang;HUANG Cheng-tian(Shenyang Research Institute of Chemical Industry Co.,Ltd.,Shenyang 110021,China;Shenyang SYRICI Testing Co.,Ltd.,Shenyang 110021,China)

机构地区：[1]沈阳化工研究院有限公司,沈阳110021 [2]沈阳沈化院测试技术有限公司,沈阳110021

出　　处：《农药》2021年第2期135-138,共4页Agrochemicals

基　　金：辽宁省自然科学基金(20180550210)。

摘　　要：[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。[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.

关 键 词：小麦 脱硫丙硫菌唑 戊唑醇 高效液相色谱串联质谱 

分 类 号：TQ450.2[化学工程—农药化工]