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分散固相萃取-分散液液微萃取/高效液相色谱法测定西瓜中氟唑菌酰羟胺残留 预览 被引量:3

Determination of Pydiflumetofen Residues in Watermelon by High Performance Liquid Chromatography with Dispersive Solid-phase Extraction and Dispersive Liquid- Liquid Microextraction
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摘要 采用分散固相萃取和分散液液微萃取联用的方法,建立了高效液相色谱快速检测西瓜中氟唑菌酰羟胺残留的分析方法。使用乙腈和水混合溶液作为萃取溶剂,经N-丙基-乙二胺硅烷(PSA)固相萃取吸附剂净化提取液,分散液液微萃取将目标物富集到1,1,2,2-四氯乙烷溶剂中,采用高效液相色谱进行分析。考察了萃取溶剂的种类与体积、分散剂体积及盐浓度等因素对分散液液微萃取萃取效率的影响。结果表明:分析物的质量浓度在0.01—5mg/L范围内与峰面积的线性关系良好,相关系数(r)为0.9999,定量下限(S/N=10)为0.01mg/kg。加标水平为0.01、0.1、1mg/kg时,平均回收率为89.2%~94.5%,相对标准偏差(n=5)为3.0%~8.7%。该方法简单、高效、灵敏度高,适用于西瓜中氟唑菌酰羟胺的残留检测。 A high performance liquid chromatography method for the determination of pydiflumetofen residues in watermelon was developed using dispersive solid-phase extraction and dispersive liquid - liquid microextraction as sample preparation methods. The samples were extracted with acetonitrile and water solution, purified with primary secondary amine as sorbents, and concentrated into 1, 1, 2, 2-tetrachloroethane by dispersive liquid - liquid microextraction. The extracts were analyzed by high performance liquid chromatography. The conditions affecting the purification efficiency of the dispersed solid phase extraction, including the extraction solvent and the type of adsorbent were optimized. Factors affecting the extraction efficiency such as type and volume of extraction solvent, volume of dispersive solvent and salt concentration, were investigated. The results indicated that the calibration curves for the analytes were linear in the concentration range of 0.01 - 5 mg/L with the correlation coefficients of 0. 999 9. The limits of quantification ( S/N = 10 ) were 0.01 mg/kg. The mean recoveries at three concentration levels of 0. 01, 0. 1, 1 mg/kg were in the range of 89. 2% - 94. 5% with the relative standard deviations below 8.7%. With the advantages of simplicity, high efficiency and sensitivity, the proposed method was applicable for the analysis of pydiflumetofen residues in watermelon samples.
作者 智沈伟 李兴海 赵尔成 贾春虹 朱晓丹 ZHI Shen-wei1,2, LI Xing-hai1, ZHAO Er-cheng2, JIA Chun-hong2, ZHU Xiao-dan2 (1.Institute of Plant Protection, Shenyang Agriculture University, Shenyang 110866, China; 2. Institute of Plant Protection and Environment Protection, Beijing Academy of Agriculture and Forestry Science, Beijing 100097, China)
出处 《分析测试学报》 CSCD 北大核心 2017年第10期1265-1268,共4页 Journal of Instrumental Analysis
基金 国家自然科学基金项目(31301649) 辽宁省自然科学基金(2015020766) 辽宁省教育厅科学研究项目(LSNYB201611)
关键词 氟唑菌酰羟胺 分散固相萃取 分散液液微萃取 西瓜 高效液相色谱 pydiflumetofen dispersive solid-phase extraction dispersive liquid -liquid microex-traction watermelon high performance liquid chromatography
作者简介 通讯作者:李兴海,博士,副教授,研究方向:新农药创制与合成,E-mail:xinghai30@163.com
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