分子印迹固相萃取-气相色谱-串联质谱法测定油茶籽油中16种多环芳烃
Determination of 16 polycyclic aromatic hydrocarbons in oil-tea camellia seed oil using molecularly imprinted solid-phase extraction coupled with GC-MS/MS
  
DOI:
中文关键词:  油茶籽油  多环芳烃  分子印迹固相萃取  气相色谱-串联质谱法
英文关键词:oil-tea camellia seed oil  polycyclic aromatic hydrocarbons  molecularly imprinted solid-phase extraction  GC-MS/MS
基金项目:
Author NameAffiliation
ZHONG Donglian1,YU Ninghua2,WANG Meijuan1, MO Runhong1, DUAN Junmin2, TANG Fubin1 1.Research Institute of Subtropical Forestry, Chinese Academy of Forestry, Hangzhou 311400, China
2.Hunan Quality Inspection and Testing Center for Forestry Products, Changsha 410004, China 
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中文摘要:
      为稳定可靠地分析油茶籽油中多环芳烃,建立了分子印迹固相萃取-气相色谱-串联质谱测定油茶籽油中16种多环芳烃方法。样品经正己烷溶解后,分别采用反相固相萃取HLB小柱、弗罗里硅土小柱和分子印迹固相萃取小柱对16种多环芳烃进行净化。以回收率和基质效应为考察指标评估3种固相萃取柱的净化,在此基础上,对净化液进行低温低速氮吹浓缩,多反应监测扫描模式下进行气相色谱-串联质谱检测,外标法定量。结果表明:分子印迹固相萃取小柱对16种多环芳烃的净化效果最佳;16种多环芳烃在质量浓度1~50 μg/L范围内线性关系良好(R2≥0.995 1),检出限为0.01~ 0.20 μg/kg,在2、10 μg/kg和20 μg/kg加标水平下的回收率为71.5%~116.3%,相对标准偏差为1.5%~13.8%。该方法具有灵敏度高、检出限低、重复性好等特点,适用于油茶籽油中16种多环烃的测定。
英文摘要:
      In order to analyze polycyclic aromatic hydrocarbons(PAHs) in oil-tea camellia seed oil stably and reliably, a method for the determination of 16 PAHs in oil-tea camellia seed oil was developed by molecularly imprinted solid-phase extraction(MIP-SPE)-gas chromatography-tandem mass spectrometry(GC-MS/MS). The samples were dissolved by n-hexane, then purified by reversed-phase solid-phase extraction HLB column, Florisil column and MIP-SPE column, respectively, and the recovery and matrix effect were used as the investigation indexes to evaluate the purification effect. On this basis, the purification solution was concentrated by low-temperature and low-speed nitrogen blowing, detected by GC-MS/MS in multiple reaction monitoring scan mode, and quantified by external standard method.The results showed that the MIP-SPE column had the best purification effect on 16 PAHs.The linearity of the 16 PAHs was good in the range of mass concentration from 1 μg/L to 50 μg/L (R2≥0.995 1), and the limits of detection (LODs) range from 0.01 μg/kg to 0.20 μg/kg. The recoveries varied from 71.5% to 116.3% with relative standard deviation of 1.5% to 13.8% at spiked levels of 2, 10 μg/kg and 20 μg/kg. The method has the characteristics of high sensitivity, low detection limit and good precision, and is suitable for rapid and accurate quantitative detection of 16 PAHs in oil-tea camellia seed oil.
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