9%春雷霉素·噻霉酮可湿性粉剂在黄瓜上的残留分析  

Residue Analysis of 9%Kasugamycin and Benziothiazolinone Wettable Powder on Cucumber

作　　者：牛艺融 李晋津 宋淑荣[1] 郭永泽[1] 张玉婷[1] 李辉[1] NIU Yirong;LI Jinjin;SONG Shurong;GUO Yongze;ZHANG Yuting;LI Hui(Institute of Agro-product Safety and Nutrition,Tianjin Academy of Agricultural Sciences,Tianjin 300384,China)

机构地区：[1]天津市农业科学院农产品质量安全与营养研究所,天津300384

出　　处：《天津农业科学》2022年第S01期121-126,共6页Tianjin Agricultural Sciences

基　　金：天津市蔬菜现代农业产业技术体系创新团队(ITTVRS2021019);天津市农业科技成果转化与推广项目(201901040)。

摘　　要：为研究9%春雷霉素·噻霉酮可湿性粉剂在黄瓜上的残留情况及使用安全性,从提取溶剂、净化方式等方面优化了前处理方法,将黄瓜样品经有机溶剂提取后在电喷雾正离子(ESI+)模式下,应用超高效液相色谱-串联质谱联用仪采用多反应监测模式检测春雷霉素和噻霉酮的残留情况。结果显示:春雷霉素采用含1%甲酸的甲醇水溶液提取,经过阳离子交换固相萃取(MCX)SPE小柱净化,噻霉酮采用乙酸乙酯提取,可达到理想要求;春雷霉素和噻霉酮分别在0.025~1.25 mg·L^(-1),0.01~1 mg·L^(-1)浓度范围内线性良好,相关系数分别为0.9998,0.9999;春雷霉素添加水平为0.05,0.2,1 mg·kg^(-1)时,平均加标回收率在73%~81%之间,相对标准偏差不大于10%;噻霉酮添加水平为0.01,0.1,1 mg·kg^(-1)时,平均加标回收率在73%~94%之间,相对标准偏差不大于10%。田间试验结果显示:9%春雷霉素·噻霉酮可湿性粉剂,以47.25 g.a.i.·hm^(-2)的剂量施药3次,采收间隔期5,7 d,其残留量均低于定量限。综上,优化后的方法准确性好、灵敏度高、能简单快捷的分析出农药残留情况。9%春雷霉素·噻霉酮可湿性粉剂按照推荐方法使用,残留量符合我国相关限量标准要求,食用安全性好。In order to research the residue and safety of 9%kasugamycin and benziothiazolinone wettable powder on cucumber,the pretreatment methods were optimized from the aspects of extraction solvent and purification method.After the cucumber samples were extracted with organic solvent,the residues of kasugamycin and benziothiazolinone were detected by ultra-high performance liquid chromatography tandem mass spectrometry in the mode of electrospray ionization(ESI+).The results showed that kasugamycin was extracted with methanol aqueous solution of 1%formic acid,purified by cation exchange solid phase extraction(MCX)SPE column,and benziothiazolinone was extracted with ethyl acetate.The linearity of kasugamycin and benziothiazolinone was good in the concentration range of 0.025~1.25 mg·L^(-1) and 0.01~1 mg·L^(-1) respectively,and the correlation coefficients was 0.9998,0.9999.The kasugamycin average recoveries of two pesticides at the three levels of 0.05,0.2 and 1 mg·kg^(-1) were between 73%and 81%,with the relative standard deviation less than 10%.The benziothiazolinone average recoveries of two pesticides at the three levels of 0.01,0.1 and 1 mg·kg^(-1) were between 73%and 94%,with the relative standard deviation less than 10%.The results of field experiment showed that the residue of 9%kasugamycin and benziothiazolinone wettable powder was lower than the quantitative limit when it was applied three times at the dose of 47.25 g.a.i.·hm^(-2),and the harvest interval was 5 d and 7 d.In conclusion,the optimized method has good accuracy,high sensitivity and can analyze pesticide residues simply and quickly.9%kasugamycin and benziothiazolinone wettable powder is used according to the recommended method,and the residue meet the requirements of relevant limit standards in China,with good edible safety.

关 键 词：春雷霉素 噻霉酮 超高效液相色谱-串联质谱法 黄瓜 

分 类 号：O657.63[理学—分析化学] S481.8[理学—化学]