GC-MS同时检测食品中多种常见毒物的方法研究  

Determination of various poisons in common in food by Gas Chromatography-Mass Spectrometry

作　　者：沈平[1] 彭进[1] 谢朝梅[1] 谢燕湘[1] 谢敏[1] 

机构地区：[1]湖南省常德市疾病预防控制中心,湖南常德415000

出　　处：《中国卫生检验杂志》2011年第4期781-784,787,共5页Chinese Journal of Health Laboratory Technology

基　　金：2011年常德市科技局重点项目

摘　　要：目的:建立用GC-MS同时检测食品中多种常见毒物的方法,包括18种有机磷、8种有机氯农药及杀鼠药毒鼠强和氟乙酰胺,并优化样品前处理中的提取及净化条件。方法:农残类样品进行分类提取,含油脂较少的样品用乙腈提取后浓缩近干,经丙酮和二氯甲烷混合液溶解,无水Na2SO4脱水,过Carb/NH2柱、硅镁柱净化,浓缩待测定;含油脂较多的样品,先用石油醚提取其脂肪的含量,再利用乙腈和石油醚液液分配的方法将脂肪中的农药残留分离,无水Na2SO4脱水后,以不同体积比例的二氯甲烷、乙腈、正己烷作为淋洗液,过弗罗里硅土柱、Carb/NH2柱净化样品后浓缩待测定。含杀鼠药的样品经乙酸乙酯提取,无水Na2SO4脱水后,以乙酸乙酯作为淋洗液,过硅镁柱净化后浓缩待测定。结果:实验结果显示18种有机磷的最低检出限为0.01 mg/L^0.05 mg/L,8种有机氯为0.001 mg/L^0.01 mg/L,毒鼠强为0.03 mg/L,氟乙酰胺0.05 mg/L,加标回收率分别为67.7%~83.2%、68.6%~85.3%、89.6%~92.7%、81.5%~83.6%,RSD分别为1.3%~7.9%、1.8%~3.7%、4.5%、2.5%。结论:该方法为能够将以上食品中常见的多种毒物进行良好的分离测定,准确的定性和定量,实验结果显示灵敏度、重现性良好,准确度和精密度较高,可用于实际检测分析。Objective：To establish a method with Gas Chromatography-Mass Spectrometry also detection of various common poisons in food in same conditions,including 18 kinds of organophosphorus,8 kinds of organochlorine pesticides,killing rat poisons fluoroacetamide and tetramine,and optimize the sample pretreatment of extraction and purification conditions.Methords： Extracted samples were classified pesticide category,containing fat fewer extracted using acetonitrile sample after nearly dry,concentrated extract by acetone and methylene chloride mixture dissolve,over Na2SO4 dehydration without water,had Carb/NH2 column and silicon magnesium column purification,concentrated to determine;Containing fat more samples,first with petroleum ether extract the fat content,using mixture of acetonitrile and petroleum ether liquid-liquid allocation methods will adipose the pesticide residue separation,over Na2SO4 dehydration without water,with different volume percentage of methylene chloride,acetonitrile and are hexane as eluent,over florisil column and Carb/NH2 column,samples to determination after purification and concentration.Containing killed of rat poison samples by ethyl acetate extracted,over Na2SO4 dehydration without water,with ethyl acetate as eluent,had silicon magnesium column purification then concentrated determination.Results： The results showed that 18 kinds of organophosphorus detection of limiting was 0.01 mg/L^0.05 mg/L,8 kinds of organochlorines in the 0.001 mg/L^0.01 mg/L,tetramine was 0.03 mg/L,Fluoroacetamide was 0.05 mg/l,the method recoveries were 67.7%~83.2%,68.6%~85.3%,89.6%~92.7%,81.5%~83.6%,and the RSD were 1.3%~7.9%,1.8%~3.7%,4.5%,2.5 %.Conclusion： This method is able to determinate various poisons in food for good separation and determination,accurate qualitative and quantitative,experimental results show that the method is sensitive and reproducibility,and high accuracy and precision,and can be used in the actual testing analysis.

关 键 词：有机磷 有机氯 GC/MS 毒鼠强 氟乙酰胺 

分 类 号：O657.63[理学—分析化学]