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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

摘    要
取干紫菜样品2.00 g置于50 mL离心管中,加入1.00 mg·L-1内标混合溶液100 μL,加入4 mL水浸润。再加入10 mL正己烷均质20 s,加入4.0 g无水硫酸镁、1.0 g氯化钠,涡旋混匀2 min,离心,向1 mL上清液中加入100 mg N-丙基乙二胺(PSA)和100 mg无水硫酸镁,涡旋混匀1 min,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0.57~3.8 μg·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%。
标    签 气相色谱-质谱法   分散固相萃取   多环芳烃   干紫菜   gas chromatography-mass spectrometry   dispersive solid phase extraction   polycyclic aromatic hydrocarbon   dry prophyra  
 
Abstract
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%.

中图分类号 O657.63   DOI 10.11973/lhjy-hx201810013

 
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所属栏目 工作简报

基金项目 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)

收稿日期 2017/11/8

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备注范广宇,工程师,主要从事食品理化检测工作,gyfan@foxmail.com

引用该论文: FAN Guangyu,WU Jin,MENG Xianglong,DUAN Rui,DUAN Hongan,LIANG Zhengang. Determination of 16 Polycyclic Aromatic Hydrocarbons in Dry Prophyra by Gas Chromatography-Mass Spectrometry with Dispersive Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(10): 1182~1187
范广宇,吴琎,孟祥龙,段蕊,段宏安,梁振纲. 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[J]. 理化检验-化学分册, 2018, 54(10): 1182~1187


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