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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 for the simultaneous determination of a variety of common toxicants in food by GC-MS, including 18 kinds of organophosphorus, 8 kinds of organochlorine pesticides and rat warfarin and fluoroacetamide, and to optimize the extraction and Purification conditions. Methods: The samples of pesticide residues were classified and extracted. The samples containing less fat were concentrated and nearly dried after extraction with acetonitrile. The samples were dissolved with acetone and dichloromethane, dehydrated with anhydrous Na2SO4, purified with Carb / NH2 column and silica gel column, Concentration to be determined; containing more fat samples, first with petroleum ether to extract the fat content, and then use acetonitrile and petroleum ether liquid-liquid separation of fat in the pesticide residues separated anhydrous Na2SO4 dehydration, with different volume ratio Dichloromethane, acetonitrile, n-hexane as eluent, after Florisil column, Carb / NH2 column sample was concentrated to be determined. Samples containing rodenticides were extracted with ethyl acetate, dehydrated with anhydrous Na2SO4 and eluted with ethyl acetate. After purification by silica gel column, the concentration was determined. Results: The results showed that the minimum detectable limit of 18 organophosphates was 0.01 mg / L ~ 0.05 mg / L, that of 8 organochlorines was 0.001 mg / L ~ 0.01 mg / L, that of tetramine was 0.03 mg / L, Acetaminophen 0.05 mg / L, the recoveries were 67.7% -83.2%, 68.6% -85.3%, 89.6% -92.7%, 81.5% -83.6%, RSD were 1.3% ~ 7.9%, 1.8% ~ 3.7 %, 4.5%, 2.5%. Conclusion: This method is able to conduct a good separation and determination of a variety of common toxicants in food, accurate qualitative and quantitative, the experimental results show good sensitivity, reproducibility, accuracy and precision, can be used for the actual test analysis .