乳化液液微萃取结合超高效液相色谱法检测水、果汁、茶和醋中三唑酮和三唑醇残留量  

Determination of triadimefon and triadimenol in water,juice,tea,and vinegar by emulsive liquid-liquid microextraction combined with ultra performance liquid chromatography

作　　者：秦一帆 郭兴乐 卫娟娜 白冰 张高勤 辛国斌 荆旭 QIN Yi-Fan;GUO Xing-Le;WEI Juan-Na;BAI Bing;ZHANG Gao-Qin;XIN Guo-Bin;JING Xu(College of Food Science and Engineering,Shanxi Agricultural University,Taiyuan 030031,China;Key Laboratory of Forensic Toxicology Analysis,Ministry of Public Security,Beijing 100192,China;Institute of Forensic Science Public Security Bureau of Linfen,Linfen 041000,China;Institute of Criminal Science and Technology,Department of Public Security of Shanxi Province,Jinzhong 030601,China)

机构地区：[1]山西农业大学食品科学与工程学院,太原030031 [2]法庭毒物分析公安部重点实验室,北京100192 [3]临汾市公安司法鉴定中心,临汾041000 [4]山西省公安厅刑事科学技术研究所,晋中030601

出　　处：《食品安全质量检测学报》2024年第23期160-166,共7页Journal of Food Safety and Quality

基　　金：国家自然科学基金项目(32202161);法庭毒物分析公安部重点实验室开放基金项目(2023FTDWFX01)。

摘　　要：目的建立一种乳化液液微萃取技术结合超高效液相色谱法检测水、果汁、茶和醋中三唑酮和三唑醇残留的方法。方法使用己酸为环境友好型萃取剂,与纯水混合制备高浓度乳液,加入样品中在1 s内完成乳化和萃取。然后,加入电解质溶液无需离心即可完成破乳和分离。最后,使用超高效液相色谱仪分析含量。结果在0.02~2.00 mg/L范围内,三唑酮、三唑醇的线性关系良好,其决定系数大于0.997。定量限和检出限分别为0.020 mg/L和0.006 mg/L。萃取回收率为83.8%~100.3%,相对标准偏差为1.5%~4.8%。结论与传统的分散液液微萃取相比,乳化液液微萃取没有使用分散剂,从而减少了有毒溶剂的使用,同时避免了分散剂对分配系数的影响。乳化液液微萃取也不需要超声、涡旋、微波等仪器辅助萃取。所开发的乳化液液微萃取方法适用于水、果汁、茶和醋样品中的三唑酮和三唑醇的检测,并有可能作为分散液液微萃取的替代方法广泛应用于样品前处理领域。Objective To establish a method for the determination of triadimenol and triadimefon in water,juice,tea,and vinegar by emulsive liquid-liquid microextraction combined with ultra performance liquid chromatography.Methods Environmentally friendly hexanoic acid was used as an extractant,mixed with pure water to prepare a high-concentration emulsion.This emulsion was added to samples to complete the emulsification and extraction in 1 s.Afterward,an electrolyte solution was added to induce demulsification and separation without the need of centrifugation before the ultra performance liquid chromatography analysis.Results A good linear relationship of triadimenol and triadimefon was obtained in the concentration range of 0.02 mg/L to 2.00 mg/L,with coefficients of determination greater than 0.997.The limits of quantification and detection were 0.020 and 0.006 mg/L.The extraction recoveries ranged from 83.8%to 100.3%,with relative standard deviations of 1.5%to 4.8%.Conclusion Compared to the conventional dispersive liquid-liquid microextraction,the emulsive liquid-liquid microextraction method does not use dispersants thus reducing the volume of toxic solvents and avoiding the effect of dispersants on the partition coefficient.The emulsive liquid-liquid microextraction method does not require auxiliary extraction instruments such as ultrasound,vortex,or microwave.The emulsive liquid-liquid microextraction method effectively detects triadimenol and triadimefon in water,juice,tea,and vinegar samples and has the potential as an alternative to dispersive liquid-liquid microextraction for wide application in sample pretreatment.

关 键 词：液相微萃取 三唑类杀菌剂 样品前处理 食品安全 

分 类 号：O657.72[理学—分析化学] TS207.53[理学—化学]