黄 武,章晶晶,刘 辉,孙良娟,孙艳波,庞晓林.QuEChERS结合在线凝胶渗透色谱-气相色谱- 质谱联用法快速检测水产品中农药残留[J].食品安全质量检测学报,2016,7(2):746-754 |
QuEChERS结合在线凝胶渗透色谱-气相色谱- 质谱联用法快速检测水产品中农药残留 |
Rapid determination of pesticide residues in aquatic products by QuEChERS and on-line gel permeation chromatography-gas chromatography-mass spectrometry |
投稿时间:2015-12-01 修订日期:2016-02-01 |
DOI: |
中文关键词: 凝胶渗透色谱-气相色谱-质谱联用法 QuEChERS 农药残留 水产品 |
英文关键词:gel permeation chromatography-gas chromatography-mass spectrometry QuEChERS pesticide residues aquatic products |
基金项目:广东检验检疫局科技项目(2014GDK09,2016GDK30)、国家质量监督检验检疫总局科技项目(2013IK192, 2013QK272) |
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中文摘要: |
目的 建立水产品中32种农药残留的快速筛查分析方法。方法 样品采用改进的QuEChERS方法提取净化, 通过在线凝胶渗透色谱-气相色谱-质谱联用技术检测。结果 32种农药在0.01~0.5 mg/L范围内具有良好的线性关系, 相关系数为0.9956~0.9999; 对于5.00 g样品的32种农药残留的检出限范围为0.05~3.14 μg/kg, 3个添加水平的回收率范围为74.5%~104.1%; 相对标准偏差范围4.2%~15.6%。结论 本方法具有操作简便、快速等特点, 同时结合筛选和确证两个过程, 灵敏度理想, 可靠性强, 符合分析要求。 |
英文摘要: |
Objective To establish a method for the rapid determination of 32 pesticide residues in aquatic products. Methods The samples were extracted and purified by a modified QuEChERS method, and then the supernatant was analyzed by on-line gel permeation chromatography-gas chromatography-mass spectrometry. Results The linear range was from 0.01 to 0.5 mg/L with a good correlation coefficients (r=0.9956~0.9999) for 32 pesticides. The detection limits were 0.05~3.14 μg/kg for all compounds based on a 5.0 g sample. Overall recoveries and relative standard deviations (RSD) were ranged from 74.5% to 104.1% and from 4.2% to15.6%, respectively. Conclusion The method has the advantages of simple and convenient operation, and the combination of screening and identification of the two processes. The sensitivity and reliability of this method is useful for the quality surveillance of 32 pesticides in aquatic products. |
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