[关键词]
[摘要]
目的 采用顶空固相微萃取(HS-SPME)结合气相色谱质谱法(GC-MS)分析检测海南产黄皮不同部位的挥发油成分。方法 在对5种不同性质的萃取头考察优化后,选用L16(45)正交表进行正交试验优化其他5个影响HS-SPME萃取的因素(水的体积、萃取温度、平衡时间、萃取时间、NaCl添加量),最终采用GC-MS相似度检索结合保留指数对黄皮叶、果皮和种子中的挥发性成分进行分析与鉴定。结果 最终确定的萃取条件为采用50/30 μm DVB/CAR/PDMS萃取头,取样品粉末10.0 mg于20 mL顶空瓶中,加水2.0 mL和NaCl 0.2 g,萃取温度80℃,平衡时间30 min,萃取时间60 min。在此条件下从海南产黄皮叶、果皮和种子中分别鉴定出83、96和106种挥发性成分,分别占挥发油总量的95.24%、92.15%和95.92%,含量较高的均为倍半萜类成分,其成分和含量在不同部位中差异较大。结论 HS-SPME-GC-MS法灵敏度高,样品用量少,操作简便,无需有机溶剂,谱库相似度检索结合保留指数提高了分析鉴定的准确性,为海南产黄皮的进一步研究提供了科学依据。该方法能对中药中高沸点及微量成分进行富集分析,更全面、科学地对中药的质量进行表征及评估。
[Key word]
[Abstract]
Objective A headspace-solid phase microextraction-gas chromatography-mass spectrometry method (HS-SPME-GC-MS) was adopted for analyzing the volatile components of different parts of Clausena lansium in Hainan Province. Methods Five different fibers were investigated and optimized. Other five experimental parameters such as volume of water, extraction temperature, equilibrium time, extraction time, and salt concentration had been evaluated and optimized by means of the orthogonal design with L16(45) table. Finally, the volatile components of C. lansium leaves, pericarps, and seeds in Hainan were analyzed and identified by GC-MS combined with retention index (RI). Results The optimum extraction conditions were as follows:a 50/30 μm DVB/CAR/PDMS fiber, 10 mg sample powders, 2.0 mL water, 0.2 g NaCl, extraction temperature 80℃, equilibrium time 30 min, extraction time 60 min. A total of 83 chemical components were identified from leaves, 96 from pericarps, and 106 from seeds, representing the relative contents of 95.24%, 92.15%, and 95.92% of the total composition. The highest contents were sesquiterpenes in all of the parts, but there were obviously different both in components and contents. Conclusion The HS-SPME-GC-MS method is rapid and sensitive, with a small sample size, without any organic solvents. GC-MS combined with RI has improved the accuracy of analysis and identification. The results may provide experimental basis for further exploitation of C. lansium in Hainan. This method can be used to perform enrichment analysis of the components with high-boiling point and micro-components, which can comprehensively and scientifically characterize and evaluate the quality of Chinese materia medica.
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[基金项目]
海南省自然科学基金项目(20163076);海南医学院科研培育基金项目(HY2015-15);海南医学院大学生创新训练计划项目(HYCX2018046)