固相萃取-毛细管液相色谱测定食品和水样中有机磷和氨基甲酸酯类杀虫剂残留

doi:10.3724/SP.J.1123.2017.09023

色谱 ›› 2018, Vol. 36 ›› Issue (1): 30-36.DOI: 10.3724/SP.J.1123.2017.09023

固相萃取-毛细管液相色谱测定食品和水样中有机磷和氨基甲酸酯类杀虫剂残留

刘洁^1,2, 鹿文慧², 崔荣¹, 孙西艳², 李金花², 陈令新²

1. 烟台大学环境与材料工程学院, 山东烟台 264005;
2. 中国科学院烟台海岸带研究所中国科学院海岸带环境过程与生态修复重点实验室, 山东烟台 264003

收稿日期:2017-09-12 出版日期:2018-01-08 发布日期:2018-01-22
通讯作者: 陈令新,Tel:(0535)2109130,E-mail:lxchen@yic.ac.cn;崔荣,Tel:(0535)6706038,E-mail:glorytre@163.com.
基金资助:
国家自然科学基金（21477160）.

Determination of organophosphorus and carbamate insecticide residues in food and water samples by solid phase extraction coupled with capillary liquid chromatography

LIU Jie^1,2, LU Wenhui², CUI Rong¹, SUN Xiyan², LI Jinhua², CHEN Lingxin²

1. School of Environment and Materials Engineering, Yantai University, Yantai 264005, China;
2. Key Laboratory of Coastal Environmental Processes and Ecological Remediation, Yantai Institute of Coastal Zone Research, Chinese Academy of Sciences, Yantai 264003, China

Received:2017-09-12 Online:2018-01-08 Published:2018-01-22
Supported by:
National Natural Science Foundation of China (No. 21477160).

摘要/Abstract

摘要：

采用乙腈提取、固相萃取（SPE）富集浓缩技术结合自行研制开发的毛细管液相色谱（CLC）仪，同时分离测定了食品和水样中1种有机磷和3种氨基甲酸酯类杀虫剂残留。对影响SPE效率和CLC分离检测的各类因素进行了优化，包括固相萃取柱种类、样品pH、洗脱剂种类和体积、上样速率、盐效应、上样体积、检测波长、流动相种类和比例等。结果表明，4种杀虫剂在6 min内达到完全分离，检出限为0.35~1.20 μg/kg，定量限为1.17~4.00 μg/kg。使用该SPE-CLC法对西红柿、黄瓜、苹果样品和自来水、湖水水样进行加标回收测定，得到食品中加标回收率为72.41%~107.15%，相对标准偏差≤8.12%；水样中加标回收率为71.45%~109.25%，相对标准偏差≤9.28%。该法能够满足农药多残留分析要求。

关键词: 氨基甲酸酯, 固相萃取, 毛细管液相色谱, 杀虫剂残留, 食品, 水样, 有机磷

Abstract:

A method was established for the simultaneous separation and determination of one organophosphorus and three carbamate insecticide residues in food and water samples by solid phase extraction (SPE) followed by analysis using a home-made capillary liquid chromatogram. Various parameters possibly affecting the efficiencies of capillary liquid chromatography (CLC) and SPE were investigated in detail, such as type of SPE column, pH value of samples, type and volume of elution solvent, flow rate of loading sample, salt effect, loading volume, detection wavelength, and type and ratio of mobile phases. Under the optimized experimental conditions, the four insecticides were separated completely within 6 min. The limits of detection and limits of quantification were 0.35-1.20 μg/kg and 1.17-4.00 μg/kg, respectively. Satisfactory recoveries of the SPE-CLC method were achieved for spiked food samples of tomato, cucumber and apple ranging from 72.41% to 107.15% with the relative standard deviations (RSDs) no more than 8.12%, and for spiked tap/lake water samples ranging from 71.45% to 109.25% with the RSDs no more than 9.28%. The method can meet the requirements for multi-residue analysis of insecticides.

Key words: capillary liquid chromatography (CLC), carbamate, food, insecticide residues, organophosphorus, solid phase extraction (SPE), water samples

中图分类号:

O658

刘洁, 鹿文慧, 崔荣, 孙西艳, 李金花, 陈令新. 固相萃取-毛细管液相色谱测定食品和水样中有机磷和氨基甲酸酯类杀虫剂残留[J]. 色谱, 2018, 36(1): 30-36.

LIU Jie, LU Wenhui, CUI Rong, SUN Xiyan, LI Jinhua, CHEN Lingxin. Determination of organophosphorus and carbamate insecticide residues in food and water samples by solid phase extraction coupled with capillary liquid chromatography[J]. Chinese Journal of Chromatography, 2018, 36(1): 30-36.

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固相萃取-毛细管液相色谱测定食品和水样中有机磷和氨基甲酸酯类杀虫剂残留

Determination of organophosphorus and carbamate insecticide residues in food and water samples by solid phase extraction coupled with capillary liquid chromatography

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