分散液液微萃取-气质联用检测葡萄酒中的有机氯农药残留

Determination of Organochlorine Pesticides Residues in Wine by GC-MS with Dispersive Liquid-Liquid Microextraction

建立了分散液液微萃取-气相色谱-质谱法(DLLME-GC-MS)的同步检测红葡萄酒样品中α-BHC、β-BHC、δ-BHC、林丹(γ-BHC)、p,p'-DDE、p,p'-DDT、p,p'-DDD和o,p'-DDT 8种有机氯农药(OCPs)残留的快速、高效和经济的新方法。在样品中添加1mg/L浓度的农药,分别以氯苯、二硫化碳、二氯甲烷和四氯化碳为萃取剂,以丙酮、乙腈、甲醇为分散剂,进行农药提取,平行3次,取平均值,考察农药加标回收率和富集倍数。结果表明,以80μμL二硫化碳和四氯化碳(3:1,V/V)为提取剂、1mL丙酮为分散剂时,提取效果最佳,在0.10—20.0μg/mL线性范围内,回收率在85%—110%之间,方法对所有待测农药的检测灵敏度均低于0.01mg/L,最低可至0.1μg/L。

A rapid-efficient-economic method was established to determine 8 organochlorine pesticides（OCPs） includingα-BHC,β-BHC,δ-BHC,7-BHC,p,p＇-DDE,p,p＇-DDT,p,p＇-DDD and o,p′-DDT in wine by liquid-liquid microextraction-gas chromatography-mass spectrometry （GC-MS）.The residues of organochlorine pesticides in wine were extracted by the agent （chlorobenzene,carbon disulfide,methylene chloride and carbon tetrachloride） with methanol, acetone,acetonitrile as dispersion agent,the average results were obtained for 3 parallel times.The results showed that 80μL carbon disulfide-carbon tetrachloride（3：1,V/V） was used as extraction agent and 1mL acetone as dispersing agent with the best extracting effect.The linear range was from 0.10μg/mL to 20.0μg/mL,and recoveries were in the range of 85%—110%.The detection limits of organochlorine pesticides were less than 0.01mg/L,and the lowest was 0.1μg/L.