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作 者:刘媛 刘佳 唐道邦[2] 涂勇刚[1] 臧建威 吴雨青 陈继光[1] 张清峰[1] 尹忠平[1] LIU Yuan;LIU Jia;TANG Daobang;TU Yonggang;ZANG Jianwei;WU Yuqing;CHEN Jiguang;ZHANG Qingfeng;YIN Zhongping(Jiangxi Key Laboratory of Natural Products Functional Foods,Jiangxi Agro-processing and Safety Control Engineering Laboratory,College of Food Science and Engineering,Jiangxi Agricultural University,Nanchang 330045,China;Key Laboratory of Functional Foods,Ministry of Agriculture and Rural Affairs,Guangdong Key Laboratory of Agricultural Products Processing,Sericultural&Agri-Food Research Institute,Guangdong Academy of Agricultural Sciences,Guangdong 510610,China)
机构地区:[1]江西农业大学食品科学与工程学院,江西省天然产物与功能食品重点实验室,江西省农产品加工与安全控制工程实验室,江西南昌330045 [2]广东省农业科学院蚕业与农产品加工研究所,农业农村部功能食品重点实验室,广东省农产品加工重点实验室,广东广州510610
出 处:《食品科学》2022年第20期343-351,共9页Food Science
基 金:广东省农科院农产品加工国家重点实验室培育基地开放基金项目(202109);江西省食品药品监督管理局科技项目(2017SP05);广州市科技计划项目(201909020001)。
摘 要:以4-(二乙氨基)水杨醛为原料,经缩合成环、水解反应合成一种结构新颖的香豆素类荧光衍生试剂7-(二乙氨基)-2-氧-2H-色酮-3-羧酸(记为L1);建立并优化L1与氟虫腈衍生化反应体系,优化后条件如下:催化缩合剂为1-(3-二甲基氨基丙基)-3-乙基碳二亚胺盐酸盐/4-二甲氨基吡啶,反应溶剂为二氯甲烷,L1与氟虫腈用量比为11∶1,反应时间为60 min,衍生温度为45℃;对衍生产物N-(3-氰基-1-(2,6-二氯-4-(三氟甲基)苯基)-4-((三氟甲基)亚磺酰基)-1H-吡唑-5-基)-7-(二乙氨基)-2-氧-2H-色酮-3-甲酰胺(记为SF1)进行分离和鉴定;在此基础上,建立氟虫腈柱前衍生化高效液相色谱-荧光检测方法,方法的检出限达到0.01μg/L,定量限为0.036μg/L。该方法具有较好的灵敏度、精确性和可靠性,可应用于农产品中氟虫腈残留的检测。A novel fluorescent coumarin derivatization reagent,7-(diethylamino)-2-oxo-2H-chromone-3-carboxylic acid(named as L1),was synthesized by condensation-cyclization and hydrolysis reactions using 4-(diethylamino)salicylaldehyde as the raw material.The derivatization reaction system of L1 and fipronil was established and optimized.The optimal reaction conditions were obtained as follows:condensation catalyst,1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride/4-dimethylaminopyridine;reaction solvent,dichloromethane;ratio of L1 to fipronil,11:1;reaction time,60 min;and derivatization temperature,45℃.The derivative of fipronil,N-(3-cyano-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-4-(trifluoromethyl)sulfonyl)-1H-pyrazole-5-yl)-7-(diethylamino)-2-oxo-2H-chromone-3-formamide(named as SF1),was isolated and identified.On this basis,a high performance liquid chromatography-fluorescence detection method(HPLC-FLD)based on pre-column derivatization was established for fipronil determination,with a detection limit of 0.01μg/L and quantitative limit of 0.036μg/L.In summary,the HPLC-FLD method presented good sensitivity,accuracy and reliability,and therefore could be applied to the detection of fipronil residue in agricultural products.
关 键 词:香豆素类荧光衍生试剂 氟虫腈 柱前衍生化 高效液相色谱-荧光检测
分 类 号:TS207.3[轻工技术与工程—食品科学]
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