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摘要: |
为开发甲鱼油,对其副产物高值化利用,针对传统加热辅助解吸附(HAD)在顶空固相微萃取-气质联用法(HS-SPME-GC/MS)检测甲鱼油的挥发性成分耗时长、解吸附不充分等不足,利用激光促进挥发性物质快速释放的优势,建立新型高效、简便的激光辅助(LID)方法,使甲鱼油挥发性成分在较短时间内获得释放。结果表明,该方法的最佳操作技术参数为:激光功率10 W,照射时间5 min,样品添加量3 g。从甲鱼油中共检测出53种挥发性物质,主要特征风味化合物有壬醛、己醛、庚醛、2-壬酮、2-十一酮、1-戊烯-3-醇、己醇等。与HAD相比,该方法的萃取时间从原来的30 min缩短至5 min,且检测到的有效挥发性成分种类与含量多。方法可行性验证表明,该方法具有良好的灵敏度、精密度及回收率。本研究结果对快速检测液体样品中的挥发性成分具有参考价值。 |
关键词: 激光辅助 固相微萃取 气相质谱 甲鱼油 挥发性成分 |
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基金项目:浙江省公益技术研究计划项目(LGN18C 200001,LGF19H180013); 舟山市科技计划项目(2018C31096) |
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Analysis of Volatile Components in Turtle Oil Based on Laser-assisted Headspace Solid Phase Microextraction |
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Abstract: |
The exploitation and utilization of turtle oil has a significant effect on the rational use of the by-product. In this study, referring to the drawbacks of traditional heating-assisted desorption in headspace solid phase microextraction-gas chromatography-mass spectrometry (HAD-HS-SPME-GC/MS) analysis of turtle oil volatile components, including long time heating, insufficient desorption, etc., utilizing the benefits of laser technology in promoting the fast release of volatile components, a novel, fast, efficient and convenient laser-assisted desorption method was built, which was conducive to efficient release in a shorter period of time during the analysis of volatile components of turtle oil. The results showed that the experimental parameters were optimized, including laser power (10 W), irradiation time (5 min), sample addition amount (3 g). A total of 53 volatile substances in the turtle oil were detected, and the main characteristic flavor compounds were nonanal, hexanal, heptanal, 2-nonanone, 2-undecone, 1-penten-3-ol, hexanol and so on. Compared with the conventional HAD-HS-SPME-GC/MS, the LID-HS-SPME could significantly reduce the extraction time to 5 min from a previous demand of 30 min, with similar fingerprint profiles and more volatile molecular species. Afterwards, the method was validated in terms of sensitivity, precision, and recovery, which indicated the LID-HS-SPME GC/MS method was efficient and remarkable. The results of this study had the reference value for rapid detection of volatile components in liquid samples. |
Key words: laser irradiation desorption headspace solid phase microextraction gas chromatography mass spectrometry turtle oil volatile components |