GC-MS/MS国标法检测稻谷中11种农药残留存在的问题及改进  

Problems and improvements of GC-MS/MS national standard method for determination of 11 pesticide residues in rice

作　　者：徐明雅 丰文燕 申屠婉铃 周旭 XU Ming-ya;FENG Wen-yan;SHENTU Wan-ing;ZHOU Xu(Hangzhou Grain Security Service Center,Hangzhou 310003,Zhejiang,China;Hangzhou Grain Purchase and Storage Co.,Ltd.,Hangzhou 310003,Zhejiang,China)

机构地区：[1]杭州市粮食保障服务中心,浙江杭州310003 [2]杭州市粮食收储有限公司,浙江杭州310003

出　　处：《粮食与油脂》2024年第4期140-144,157,共6页Cereals & Oils

摘　　要：研究国标法检测稻谷中11种农药残留时存在的问题,并建立改进方法。样品粉碎后经水浸润,乙腈-乙酸溶液(体积比99:1)提取,分散固相萃取净化,丙酮替换乙酸乙酯作溶剂,自动加标替换手动加标,仍采用气相色谱-串联质谱(GC-MS/MS)进行内标法定量。结果表明:丙酮替换乙酸乙酯可以有效解决无法准确定量的问题。在进样时采用自动加标可以解决手动加标的繁琐。用改进后的方法检测稻谷中11种农药残留量,在0.005~0.5 mg/L范围内线性关系良好,相关系数均大于0.999,检出限均小于0.01 mg/kg,定量限均小于0.02 mg/kg,平均回收率为72.7%~109.1%,相对标准偏差为0.8%~7.2%,符合农药残留定量的分析要求。The problems encountered in the application of the national standard method in the determination of 1l pesticides residues in rice were studied and the improved solutions were established.The crushed samples were soaked with water,extracted with acetonitrile-acetic acid solution(volume ratio 99:1),purified by dispersive solid phase extraction,and acetone replaced ethyl acetate as solvent.Automatic adding internal standard was used instead of manual adding,and internal standard quantification was still performed by gas chromatography-tandem mass spectrometry(GC-MS/MS).The results showed that replacing ethyl acetate with acetone could effectively solve the problem of inaccurate quantification.Automatic adding internal standard during sample injection could solve the cumbersome manual adding.The improved method was used to detect 11 pesticide residues in rice,and the linear relationship was good within the range of 0.005-0.5 mg/L,with correlation coefficients greater than 0.999,detection limits less than 0.01 mg/kg,and quantification limits less than 0.02 mg/kg.The average recovery rate was 72.7%-109.1%,and the relative standard deviation was 0.8%-7.2%,meeting the analysis requirements for pesticide residue quantification.

关 键 词：稻谷 农药残留量 丙酮 

分 类 号：TS207.53[轻工技术与工程—食品科学]