| 钟冬莲1，喻宁华2，王玫鹃1，莫润宏1，段俊敏2，汤富彬1.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[J].中国油脂,2022,47(10):.[ZHONG Donglian1,YU Ninghua2,WANG Meijuan1, MO Ｒunhong1, DUAN Junmin2, TANG Fubin1.Determination of 16 polycyclic aromatic hydrocarbons in oil-tea camellia seed oil using molecularly imprinted solid-phase extraction coupled with GC-MS/MS[J].China Oils and Fats,2022,47(10):.] |
| 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 |
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| 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: |
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| Author Name | Affiliation | | 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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