GC Determination of 18 Organochlorine Pesticides and 7 Polychloro-Biphenyls in Rough Rice with Ultrasonic Extraction of Samples
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5.00~200.0 μg·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0.01~0.20 μg·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。
Abstract
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 5.00-200.0 μg·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%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201609023
所属栏目 专题报道(食品分析)
基金项目 国土资源地质大调查项目(12120113014800)
收稿日期 2015/10/26
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联系人作者时磊(njdkssl@163.com)
备注时 磊(1983-)男,江苏南京人,工程师,硕士,主要从事环境有机污染物检测。
引用该论文: SHI Lei,CHEN Hai-ying,CAI Xiao-hu,HU Jing-ke,L Ai-juan,SHEN Xiao-ming,SUN Yan-yan. GC Determination of 18 Organochlorine Pesticides and 7 Polychloro-Biphenyls in Rough Rice with Ultrasonic Extraction of Samples[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(9): 1090~1094
时磊,陈海英,蔡小虎,胡璟珂,吕爱娟,沈小明,孙艳艳. 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[J]. 理化检验-化学分册, 2016, 52(9): 1090~1094
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【5】郝玉红,吴建军.气相色谱-质谱法测定硅凝胶中两种硅氧烷[J].理化检验-化学分册, 2015,51(6):818-820.
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【9】李春风,沈伟健,蒋原,等.分散固相萃取气相色谱-负化学离子源质谱法测定大豆和玉米中20种农药的残留量[J].色谱, 2009,27(2):176-180.
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