QuEChERS法联合在线凝胶过滤色谱-气相色谱-质谱联用法快速测定鱼肉中16种农药残留量
目的 采用QuEChERS 前处理方法和在线凝胶过滤色谱-气相色谱-质谱(GPC-GC/MS) 联用法对鱼肉样品中的16 种有机磷、菊酯和氨基甲酸酯等农药残留进行测定。方法 首先用QuEChERS 方法进行样品前处理, 即乙腈提取, 提取溶液经脱水后离心, 用分散性吸附剂去除离心提取液中的干扰基质(如油脂和色素等), 然后直接进行在线GPC-GC/MS联用法分析。结果 在线GPC-GC/MS系统中的GPC能弥补QuEChERS方法去除干扰物质不彻底的问题, 从而降低了分析背景, 改善了峰形, 提高了分析结果的准确性和相关质谱图的匹配性。在加标0.01 mg/kg情况下, 鱼肉样品的回收率为80%~120%, 相对标准偏差(RSD)均小于20%。线性范围0.01~0.05 μg/mL, 相关系数0.9961~0.9998。结论 本研究建立的方法步骤简单、可操作性强、仪器自动化程度高, 具有检出限低、准确度高、精密度好的特点, 应用于日常检测可大大降低检测成本, 缩短分析周期。
Objective To determine 16 pesticide residues including organophosphorus pesticides, dimethrin, and carbamates pesticides in fish were determined by online gel permeation chromatography-gas chromatography mass spectrometry (GPC-GC/MS) coupled with QuEChERS method. Methods The samples were cleaned up by QuEChERS with extracting by acetontrile and wiping pigment out with GPC. Results GPC of online GPC-GC/MS system can effectively remove chromatographic interferences that QuEChERS pretreating method can not effectively removed. Compared with GC/MS, online GPC-GC/MS has the lower interfered background and better peak shape. Identification and quantization of pesticide residues with online GPC-GC/MS can be well performed. The recoveries of 16 pesticides at the spiked con-centrations of 0.01 mg/kg were between 80%~120%. A good linearity was observed for all compounds in the concentration range investigated with correlation coefficients of 0.9961~0.9998. Conclusion The good sensitivity, precision, accuracy, simple operation and short analytical period of this method could satisfy the requirement of simultaneous determination of various pesticide residues.
标题：QuEChERS法联合在线凝胶过滤色谱-气相色谱-质谱联用法快速测定鱼肉中16种农药残留量
英文标题：Determination of pesticide residues in fish by application of QuEChERS method coupled with online gel permeation chromatography-gas chromatography mass spectrometry
作者：
苏明明 辽宁出入境检验检疫局技术中心
董振霖 辽宁出入境检验检疫局技术中心
徐静 辽宁出入境检验检疫局技术中心
孙兴权 辽宁出入境检验检疫局技术中心
董伟峰 辽宁出入境检验检疫局技术中心
曹际娟 辽宁出入境检验检疫局技术中心
中文关键词:农药残留,在线凝胶过滤色谱-气相色谱-质谱,QuEChERS前处理,食品安全,
英文关键词:pesticide residues,gel permeation chromatography-gas chromatography mass spectrometry,QuEChERS pretreating method,food safety,
发表日期：2014-04-15
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