QuEChERS法结合HPLC-MS/MS检测人参中氟吗啉和戊唑醇残留及储藏稳定性  

QuEChERS Method Combined with HPLC-MS/MS to Detect Flumorph and Tebuconazole Residues in Ginseng and Storage Stability

作　　者：朱宗利 陆洋 王欣茹 孙晓伟 尤庆航 宋雨桐 高玉雪 冷金蔓 逯忠斌 侯志广 ZHU Zong-li;LU Yang;WANG Xin-ru;SUN Xiao-wei;YOU Qing-hang;SONG Yu-tong;GAO Yu-xue;LENG Jin-man;LU Zhong-bin;HOU Zhi-guang(College of Plant Protection,Jilin Agricultural University,Changchun 130118,China)

机构地区：[1]吉林农业大学植物保护学院,长春130118

出　　处：《农药》2021年第7期512-516,共5页Agrochemicals

基　　金：吉林省参茸办人参产业发展专项资金人参中嘧菌酯等32种农药残留量的测定液相色谱-串联质谱法(201501);农业农村部行业标准制定双炔酰菌胺在人参中的残留限量标准(14202008)。

摘　　要：[目的]建立QuEChERS法与高效液相色谱-串联质谱法(HPLC-MS/MS)相结合测定人参样品中氟吗啉与戊唑醇残留量的分析方法,将该方法应用于人参中氟吗啉和戊唑醇储藏稳定性的研究。[方法]人参样品经乙腈提取,PSA与MgSO4净化,经HPLC-MS/MS测定。[结果] 2种农药在0.001~0.5 mg/L范围内线性良好,人参中氟吗啉和戊唑醇的添加水平为0.01、0.1、1.0 mg/kg,平均回收率分别为97.4%~99.9%和89.6%~100.5%,相对标准偏差分别为0.9%~1.7%和1.4%~4.3%。在-20℃下储藏的人参样品中氟吗啉和戊唑醇180 d内平均降解率均小于15%,而在25、4℃下储藏的人参样品中氟吗啉和戊唑醇180 d内平均降解率在15%~30%之间。[结论]人参样品中氟吗啉和戊唑醇在180 d内储存稳定,且随着温度的升高2种农药的降解率也呈现升高趋势。[Aims] This study aims to establish a QuEChERS method combined with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) for the determination of flumorph and tebuconazole residues in ginseng samples. The method was applied to study the storage stability of flumorpholine and tebuconazole in ginseng. [Methods] Ginseng sample was extracted with acetonitrile, purified by PSA and MgSO4, and finally determined by HPLC-MS/MS. [Results] The results showed that the two pesticides have good linearity in the range of 0.001-0.5 mg/L, when the addition levels of flumorph and tebuconazole in ginseng are 0.01, 0.1, 1.0 mg/kg, the average recoveries are 97.4-99.9 and 89.6-100.5%, respectively, the relative standard deviation is between 0.9-1.7 and 1.4-4.3%.The average degradation rate of flumorph and tebuconazole in ginseng samples stored at-20 ℃ is less than 15% within 180 d, while ginseng samples stored at 25 and 4 ℃ contain flumorph and tebuconazole for 180 d. The internal average degradation rate is between 15 and 30%. [Conclusions] Flumorph and tebuconazole in ginseng samples are stable in storage within 180 days, and the degradation rate of the two pesticides also shows an increasing trend with the increase of temperature.

关 键 词：氟吗啉 戊唑醇 人参 储藏稳定性 不同温度 

分 类 号：TQ450.2[化学工程—农药化工]