分散固相萃取-气相色谱-质谱法测定干紫菜中16种多环芳烃  

Determination of 16 Polycyclic Aromatic Hydrocarbons in Dry Prophyra by Gas Chromatography-Mass Spectrometry with Dispersive Solid Phase Extraction

作　　者：范广宇[1] 吴琎 孟祥龙[1] 段蕊[2] 段宏安[1] 梁振纲 FAN Guangyu;WU Jin;MENG Xianglong;DUAN Rui;DUAN Hongan;LIANG Zhengang(Lianyungang Entry-Exit Inspection and Quarantine Bureau,Lianyungang 222042,China;College of Marine Life and Fisheries,Huaihai Institute of Technology,Lianyungang 222005,China;Technology Center of Hainan Entry-Exit Inspection and Quarantine Bureau,Haikou 570311,China)

机构地区：[1]连云港出入境检验检疫局,连云港222042 [2]淮海工学院海洋生命与水产学院,连云港222005 [3]海南出入境检验检疫局技术中心,海口570311

出　　处：《理化检验（化学分册）》2018年第10期1182-1187,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：连云港检验检疫局科研项目(L2014KJ07);江苏检验检疫局科研项目计划(2017KJ12);国家质检总局科技计划(2017IK146)

摘　　要：取干紫菜样品2.00g置于50mL离心管中,加入1.00mg·L-1内标混合溶液100μL,加入4mL水浸润。再加入10mL正己烷均质20s,加入4.0g无水硫酸镁、1.0g氯化钠,涡旋混匀2min,离心,向1mL上清液中加入100mg N-丙基乙二胺(PSA)和100mg无水硫酸镁,涡旋混匀1min,离心。取上清液采用气相色谱-质谱法测定其中16种多环芳烃(PAHs)的含量。16种PAHs的质量浓度在一定范围内与其峰面积与内标峰面积的比值呈线性关系,检出限(3S/N)为0.57～3.8μg·kg-1。按标准加入法进行回收试验,回收率为78.3%～109%,测定值的相对标准偏差(n=6)为1.2%～14%。The sample （2.00 g） of the dry prophyra was placed into a 50 mL centrifuge tube, and 1.00 mg · L^-1 mixed solution （100 μL） of internal standards and 4 mL of water were added to wet the sample. And then 10 mL of n-hexane was added into the solution to homogenize for 20 s, and 4.0 g of anhydrous magnesium sulfate and 1.0 g of sodium chloride were added into the solution and the mixture was vortexed for 2 min. After centrifugation, 100 mg of N-propylethylenediamine （PSA） and 100 mg of anhydrous magnesium sulfate were added into 1 mL of the supernatant and the mixture was vortexed for 1 min. After centrifugation, 16 PHAs in the superanatant were determined by gas chromatography-mass spectrometry （GC-MS）. Linear relationships between the ratio of the Peak area of 16 PAHs to that of the internal standard and mass concentration of PAHs were obtained in definite ranges, with detection limits （3S/N） of 0.57-3.8 μg · kg^-1. Test for recovery was made by standard addition method, giving results in the range of 78.3%- 109%, and values of RSDs （n = 6） were in the range of 1.2%-14%.

关 键 词：气相色谱-质谱法 分散固相萃取 多环芳烃 干紫菜 

分 类 号：O657.63[理学—分析化学]