超声提取-气相色谱法同时测定稻谷中18种有机氯农药和7种多氯联苯  

GC Determination of 18 Organochlorine Pesticides and 7 Polychloro-Biphenyls in Rough Rice with Ultrasonic Extraction of Samples

作　　者：时磊[1] 陈海英[1] 蔡小虎[1] 胡璟珂[1] 吕爱娟[1] 沈小明[1] 孙艳艳 

机构地区：[1]中国地质调查局南京地质调查中心,南京210016 [2]南京市产品质量监督检验院,南京210028

出　　处：《理化检验（化学分册）》2016年第9期1090-1094,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国土资源地质大调查项目(12120113014800)

摘　　要：以正己烷-二氯甲烷(3+2)混合液作提取溶剂,对稻谷样品进行超声提取,所得提取液经硅酸镁载体层析柱净化,选择正己烷-丙酮(9+1)混合液作淋洗液。用气相色谱法测定了稻谷中18种有机氯农药和7种多氯联苯的含量。结果表明:此25种化合物的质量浓度均在5.00~200.0μg·L^(-1)范围内与其相应的峰面积之间呈线性关系。方法的检出限(3S/N)在0.01~0.20μg·L^(-1)之间。以空白样品作基体进行加标回收试验,测得回收率在71.8%~102%之间,测定值的相对标准偏差(n=6)在2.2%~11%之间。Sample of rough rice was extracted ultrasonically with a mixture of n hexane and dichloromethane （3＋2）. The extract obtained was purified on a chromatographic column filled with florisil, and eluted by a mixture of n-hexane and acetone （9＋1）. 18 organochlorine pesticides （OCPs） and 7 polychlorobiphenyls （PCBs） in rough rice sample were determined by GC. Linear relationships between values of peak area and mass concentration of the 25 compounds were found in the same range of 5.00-200. 0μg·L^-1, with detection limits （3S/N） ranged from 0. 01 to 0. 20 μg·L^-1. Using a blank sample as the matrix, recovery was tested by standard addition method, giving values of recovery in the range of 71.8 %-102%, RSDs （n= 6） found were in the range of 2.2 %- 11 %.

关 键 词：气相色谱法 超声提取 有机氯农药 多氯联苯 稻谷 

分 类 号：O657.7[理学—分析化学]