摘要
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0.01~0.05μg/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, di-methrin, 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 concentrations of 0.01 mg/kg were between 80%~120%. A good linearity was observed for all compounds in the concentration range inves-tigated 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 de-termination of various pesticide residues.
出处
《食品安全质量检测学报》
CAS
2014年第6期1757-1764,共8页
Journal of Food Safety and Quality
