双水相萃取-高效液相色谱法分析红小豆中酰胺除草剂

doi:10.7506/spkx1002-6630-20200430-394

食品科学 ›› 2021, Vol. 42 ›› Issue (14): 301-307.doi: 10.7506/spkx1002-6630-20200430-394

双水相萃取-高效液相色谱法分析红小豆中酰胺除草剂

张丽媛，张悦，于润众，王长远,，张东杰,

（1.黑龙江八一农垦大学食品学院，黑龙江大庆 163319；2.黑龙江八一农垦大学电气与信息学院，黑龙江大庆 163319；3.北大荒现代农业产业技术省级培育协同创新中心，黑龙江大庆 163319；4.黑龙江省农产品加工与质量安全重点实验室，黑龙江大庆 163319；5.国家杂粮工程技术研究中心，黑龙江大庆 163319）

发布日期:2021-07-27
基金资助:
国际合作重点研发项目（2018YFE0206300）；地方高校改革发展资金优秀青年人才项目（2020YQ16）；黑龙江省高等教育教学改革研究项目（SJGY20180356）；黑龙江八一农垦大学三横三纵资助项目（ZRCQC201906）；黑龙江省农垦总局重点研发项目（HKKY190407）

Analysis of Acetanilide Herbicide Residues in Adzuki Beans (Vigna angularis) by Aqueous Two-Phase Extraction Coupled with High Performance Liquid Chromatography

ZHANG Liyuan, ZHANG Yue, YU Runzhong, WANG Changyuan, ZHANG Dongjie

(1. College of Food Science, Heilongjiang Bayi Agricultural University, Daqing 163319, China; 2. College of Electrical and Information, Heilongjiang Bayi Agricultural University, Daqing 163319, China; 3. Heilongjiang Province Cultivating Collaborative Innovation Center for The Beidahuang Modern Agricultural Industry Technology, Daqing 163319, China; 4. Key Laboratory of Agro-products Processing and Quality Safety of Heilongjiang Province, Daqing 163319, China;5. National Coarse Cereals Engineering Research Center, Daqing 163319, China)

Published:2021-07-27

摘要/Abstract

摘要： 建立以硫酸铵-乙醇为基础的双水相萃取法，在红小豆中萃取分离富集乙草胺、丁草胺、敌稗、异丙甲草胺4 种酰胺类除草剂的方法。采用高效液相色谱法对4 种除草剂进行分析测定。在双水相萃取过程中，上相富醇溶液的极性更接近于同一有机溶剂中除草剂的极性。下相盐溶液能有效沉淀蛋白质和脂肪。考察前处理条件，最终选择硫酸铵-乙醇体系双水相体系类型、25%乙醇、28%硫酸铵、35 ℃、1 min超声萃取时间为最佳前处理条件。由于避免了有毒有机溶剂，本方法是一种环境友好的方法。乙草胺、丁草胺、敌稗、异丙甲草胺的检测限分别为3.5、7.1、4.6、5.8 μg/kg。在加标量为10 μg/kg和100 μg/kg水平下，4 种酰胺除草剂的平均回收率范围为86.1%～95.9%，相对标准偏差≤4.5%。

关键词: 双水相；萃取；酰胺除草剂；高效液相色谱法；红小豆

Abstract: A method for the determination of four acetanilide herbicides including acetochlor, butachlor, propanil, and metolachlor in adzuki beans was established using ammonium sulfate-ethanol-based aqueous two-phase extraction combined with high performance liquid chromatography. In the aqueous two-phase extraction, the polarity of the alcohol-rich upper phase was more similar to that of the herbicides in the same organic solvent. The salt solution of the lower phase could effectively precipitate protein and fat. Based on the recoveries of the herbicides, the optimal pretreatment conditions were determined as follows: aqueous two-phase system containing 25% ethanol and 28% ammonium sulfate, and ultrasonic extraction for 1 min at 35 ℃. Avoiding the use of toxic organic solvents, the current method was environmentally friendly. The detection limits for acetochlor, butachlor, propanil, and metolachlor were 3.5, 7.1, 4.6 and 5.8 μg/kg, respectively. The average recoveries at spiked concentrations of 10 and 100 μg/kg ranged from 86.1% to 95.9%, with relative standard deviation equal to or lower than 4.5%.

Key words: aqueous two-phase extraction; acetanilide herbicides; high performance liquid chromatography; adzuki bean

中图分类号:

Q657

张丽媛，张悦，于润众，王长远,，张东杰,. 双水相萃取-高效液相色谱法分析红小豆中酰胺除草剂[J]. 食品科学, 2021, 42(14): 301-307.

ZHANG Liyuan, ZHANG Yue, YU Runzhong, WANG Changyuan, ZHANG Dongjie. Analysis of Acetanilide Herbicide Residues in Adzuki Beans (Vigna angularis) by Aqueous Two-Phase Extraction Coupled with High Performance Liquid Chromatography[J]. FOOD SCIENCE, 2021, 42(14): 301-307.

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双水相萃取-高效液相色谱法分析红小豆中酰胺除草剂

Analysis of Acetanilide Herbicide Residues in Adzuki Beans (Vigna angularis) by Aqueous Two-Phase Extraction Coupled with High Performance Liquid Chromatography

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