HS-SPME-GC-MS法分析不同产地菟丝子中的挥发性成分
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篇名: HS-SPME-GC-MS法分析不同产地菟丝子中的挥发性成分
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摘要: 目的:建立分析菟丝子中挥发性成分的方法,并比较不同产地菟丝子中挥发性成分的差异。方法:采用顶空固相微萃取-气相色谱-质谱联用法(HS-SPME-GC-MS)。HS-SPME条件:取样量为1.0 g,萃取纤维头种类为65 μm PDMS/DVB,平衡温度为120 ℃,平衡时间为15 min,萃取时间为30 min,解析时间为3 min;GC条件:色谱柱为HP-5MS石英毛细管柱,程序升温,进样口温度为230 ℃,载气为高纯氦气,载气流速为1.0 ml/min,不分流进样;MS条件:离子源为电子轰击离子源,离子源温度为230 ℃,四极杆温度为150 ℃,电子能量为70 eV,倍增管电压为1.2 kV,接口温度为 280 ℃,质谱扫描范围为m/z 35~550。结合惠普化学工作站对不同产地菟丝子中的挥发性成分进行定性分析,以峰面积归一化法计算各成分的相对含量,采用主成分分析法和聚类分析法对数据进行分析。结果:共鉴定出52 种挥发性成分,其中9 种为不同产地菟丝子中的共有成分,分别为叶醇、1-辛烯-3-醇、3-辛醇、麦芽醇、酞酸二乙酯、石竹烯、壬醛、正辛醇、棕榈酸。样品1、2、3聚为一类后再与样品4、5、6聚为一类,7、8、9聚为一类后再与样品10、11、12聚为一类,样品13、14、15单独聚为一类。结论:该方法稳定可靠,适用于菟丝子中挥发性成分的快速分析;不同产地菟丝子中挥发性成分差异较大。
ABSTRACT: OBJECTIVE: To establish a method for analyzing the volatile components in Cuscuta chinensis, and compare the difference of the volatile components in C. chinensis. METHODS: HS-SPME-GC-MS was adopted: sampling amount was 1.0 g, extracting fibers was 65 μm PDMS/DVB, equilibrium temperature was 120 ℃, equilibrium time was 15 min, extraction time was 30 min, resolution time was 3 min; GC conditions: the column was HP-5MS quartz capillary column, programmed temperature, inlet temperature was 230 ℃, carrier gas was high purity helium, the flow rate was 1.0 ml/min, splitless injection; MS conditions: ion source was electron ionization, temperature was 230 ℃, quadrupole temperature was 150 ℃, electron energy was 70 eV, photomultiplier tube voltage was 1.2 kV, the interface temperature was 280 ℃, and scanning range was m/z 35-550. Combined with the qualitative analysis for volatile components of C. chinensis from different habitats by HP ChemStation, the relative content was calculated by peak area normalization, and the data was analyzed by principal component analysis and cluster analysis. RESULTS: Totally 52 components were identified, 9 of which were the common components in C. chinensis, namely leaf alcohol, 1-octene-3-ol, 3-octanol, malt alcohol, diethyl phthalate, caryophyllene, nonaldehyde, octanol and palmitic acid. sample 1, 2, 3 were clustered into a group, then clustered with 4, 5, 6 into a group, sample 7, 8, 9 was clustered into a group, then clustered with 10, 11, 12 into a group, and sample 13, 14, 15 clustered into a group individually. CONCLUSIONS: The method is stable and reliable, and suitable for the rapid analysis of volatile components in C. chinensis; and differences of volatile components in C. chinensis from diflerent habitats are discernible.
期刊: 2016年第27卷第21期
作者: 裴学军,卢金清,黎强,郭胜男
AUTHORS: PEI Xuejun,LU Jinqing,LI Qiang,GUO Shengnan
关键字: 菟丝子;挥发性成分;顶空固相微萃取;聚类分析;主成分分析
KEYWORDS: Cuscuta chinensis; Volatile components; Headspace solid phase micro extraction; Cluster analysis; Principal component analysis
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