柱前衍生HPLC法测定2甲4氯异辛酯及代谢物在玉米中的残留  

Determination of MCPA-isooctyl and its metabolite residues in corn with pre-column derivatization by HPLC

作　　者：聂春林[1,2] 梁贵平 欧晓明[1,2] 曾利红 欧将[1,2] 晏姣 陈力华 NIE Chun-lin;LIANG Gui-ping;OU Xiao-ming;ZENG Li-hong;OU Jiang;YAN Jiao;CHEN Li-hua(Hunan Research Institute of Chemical Industry,National Engineering Research Center for Agrochemicals,Hunan Province Key Laboratory for Agrochemicals,Changsha 410014,China;Hunan Research Institute of Chemical Industry Testing Technology Co.,Ltd.,Changsha 410014,China)

机构地区：[1]湖南化工研究院国家农药创制工程技术研究中心,湖南省农用化学品重点实验室,长沙410014 [2]湖南化研院检测技术有限公司,长沙410014

出　　处：《农药》2022年第3期203-207,共5页Agrochemicals

摘　　要：[目的]为了监测2甲4氯异辛酯及代谢物2甲4氯在玉米等农产品中的残留及环境安全评价,建立了柱前衍生高效液相色谱检测玉米中2者残留量的分析方法。[方法]样品中2者先用甲醇-氢氧化钠溶液反应提取,水相用盐酸-水溶液调节pH值至2,混合层析柱萃取,浓缩定容后净化,采用HPLC-PDAD进行检测。[结果]在0.1~20 mg/L质量浓度范围内,2者的峰面积与质量浓度之间呈现出良好的线性关系;在添加质量分数为0.05~1.0 mg/kg时,2甲4氯异辛酯在成熟玉米籽粒、鲜食玉米中的添加回收率分别为90%~102%和85%~104%,相对标准偏差分别为1.2%~3.1%和0.9%~4.3%;在添加质量分数为0.05~1.0 mg/kg时,2甲4氯在成熟玉米籽粒、鲜食玉米的添加回收率分别为89%~99%和90%~104%,相对标准偏差分别为1.5%~3.1%和1.8%~2.3%;在添加质量分数为0.1~1.0 mg/kg时,2者在秸秆中的添加回收率为92%~101%,相对标准偏差为1.2%~3.4%。该方法的最小检出量(LOD)均为2.0 ng。2者在成熟玉米籽粒、鲜食玉米中的最低检测浓度(LOQ)均为0.05 mg/kg,在秸秆中的最低检测浓度(LOQ)均为0.1 mg/kg。[结论]该分析方法将2种目标物同时碱液衍生提取、混合层析柱萃取、高效液相测定,具有灵敏度精确度和准确度良好、分离度佳等特点,符合农药残留检测分析的要求,已应用于玉米中2甲4氯异辛酯及2甲4氯的农残监测。[Aims]This study aims to establish an analytical method for determining MCPA-isooctyl and its metabolite MCPA residues in corn and other agricultural products and the environmental safety assessment with pre-column derivatization by using high performance liquid chromatography. [Methods]Both of them in corn samples first were extracted with methanol-sodium hydroxide solution, the pH value of aqueous phase were adjusted to 2 with hydrochloric acid-aqueou solution, further extracted by mixed chromatographic column. The concentrated solutions were purified before analysis by HPLC-PDAD. [Results]The results showed that there were a good linearity between the concentration of two residues and their corresponding response values within the mass concentration of 0.1-20 mg/L.When the spiked level ranged from 0.05-1.0 mg/kg, the fortified recoveries of MCPA-isooctyl in mature corn grain and fresh corn were 90-102 and 85-104%, respectively, with their corresponding relative standard deviation(RSD) of 1.2-3.1 and 0.9-4.3%. When the spiked level ranged from 0.05-1.0 mg/kg, the fortified recoveries of MCPA in mature corn grain and fresh corn were 89-99 and 90-104%, respectively, with their corresponding relative standard deviation(RSD)was 1.5-3.1 and 1.8-2.3%. When the spiked level ranged from 0.1-1.0 mg/kg, the average spiked recoveries of two residues in straw were 92-101%, respectively, with their corresponding RSD of 1.2-3.4%. The limit of detection(LOD)of the method was 2.0 ng, and the LOQ of two residues in mature corn grain and fresh corn samples were 0.05 mg/kg,the LOQ of two residues mature in straw samples were 0.1 mg/kg. [Conclusions]Two objects were picked up with lye at the same time, extracted by mixed chromatographic column, and determined by HPLC. The method had the characteristics of high sensitivity, good precision, good accuracy, fine resolution etc, met with the requirements for pesticide residue analysis, which already be applied for monitoring the residue of MCPA-isooctyl and MCPA in the corn products.

关 键 词：2甲4氯异辛酯 2甲4氯 残留 高效液相色谱 玉米 

分 类 号：TQ450.2[化学工程—农药化工]