| 搅拌棒吸附萃取-气相色谱-质谱法测定化妆水中多氯联苯 |
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| 引用本文： | 曹小吉,王丽萍,江南,郑乐斌,乔婧芳,叶学敏,莫卫民.搅拌棒吸附萃取-气相色谱-质谱法测定化妆水中多氯联苯[J].理化检验(化学分册),2012(6):705-708. |
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| 作者姓名： | 曹小吉 王丽萍 江南 郑乐斌 乔婧芳 叶学敏 莫卫民 |
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| 作者单位： | 浙江工业大学分析测试中心;浙江工业大学化学工程与材料学院 |
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| 基金项目： | 浙江省科技计划资助项目(2010C33074和2011C37020) |
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| 摘 要： | 提出了搅拌棒吸附萃取(SRAE)-气相色谱-质谱法测定化妆水中7种多氯联苯含量的方法。采用正交试验方法研究了萃取时间、分散剂种类及体积、热脱附时间及冷阱收集温度对萃取效率的影响。分析中采用DB-5MS毛细管色谱柱作为分离柱,质谱条件为电子轰击电离源全扫描监测模式。7种多氯联苯的峰面积与其质量分数在一定范围内呈线性关系,测定下限(10S/N)在5～60ng.kg-1之间。分别在3个浓度水平对方法的回收率和精密度进行了试验,测得回收率在74%～107%之间,测定值的相对标准偏差(n=6)在1.1%～16.9%之间。
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| 关 键 词： | 搅拌棒吸附萃取 气相色谱-质谱法 多氯联苯 化妆水 |
GC-MS Determination of Polychloro Biphenyls in Cosmetic Lotion with Stirring Rod Adsorptive Extraction |
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| CAO Xiao-ji,WANG Li-ping,JIANG Nan,ZHENG Le-bin,QIAO Jing-fang,YE Xue-min,MO Wei-min.GC-MS Determination of Polychloro Biphenyls in Cosmetic Lotion with Stirring Rod Adsorptive Extraction[J].Physical Testing and Chemical Analysis Part B:Chemical Analgsis,2012(6):705-708. |
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| Authors: | CAO Xiao-ji WANG Li-ping JIANG Nan ZHENG Le-bin QIAO Jing-fang YE Xue-min MO Wei-min |
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| Institution: | 1,2(1.Center of Analysis and Testing; 2.College of Chemical Engineering and Material Science,Zhejiang University of Industry, Hangzhou 310014,China) |
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| Abstract: | A method of GC-MS with stirring rod adsorptive extraction for the determination of 7 polychloro biphenyls(PCB′s) in cosmetic lotion was proposed.Influential factors of the extraction process,including extraction time,extraction solvent and its amount,thermodesorption time and cold injection temperature were studied by orthogonal testing.DB-5MS capillary chromatographic column was used in GC,and the full scanning monitoring with electron impact ionization source was adopted in MS.Linear relationship between values of peak area and mass fraction of PCB′s was obtained in definite ranges,with lower limits(10S/N) of determination in the range of 5-60 ng·kg-1.Tests for recovery and precision were made at 3 concentration levels,giving results of recovery in the range of 74%-107%,with values of RSD′s(n=6) in the range of 1.1%-16.9%. |
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| Keywords: | Stirring rod adsorptive extraction GC-MS PCB′s Cosmetic lotion |
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