摘要
采用顶空固相微萃取-气相色谱质谱法(HS-SPME/GC-MS)定性定量分析广藿香药材中的挥发性成分。以百秋里醇的峰面积为指标,确定HS-SPME最佳的实验条件为:160目药材粉末用无水Na2SO4稀释10倍,称取30mg于15mL萃取瓶中,以250r/min速度搅拌预热(80℃)40min,插入65μm聚二甲基硅烷-二乙烯(PDMS-DVB)涂层的纤维头,在相同搅拌速度下80℃萃取40min,纤维头进入GC进样口在250℃下解吸100s。GC色谱条件:色谱柱为DB-5MS柱;载气流速为1mL/min;柱温的起始温度为90℃,以0.8℃/min升至110℃,保持5min;1.0℃/min升至134℃,保持5min;最后以5.0℃/min升至143℃,保持10min。结果:百秋里醇的平均回收率为91.8%,RSD为3.0%。运用本方法对10份不同产地广藿香中百秋里醇的含量进行测定,并以其为参比对照,测定了广藿香中其它主要挥发性成分的含量。
A head-space solid phase microextraction （HS-SPME） coupled to gas chromatography-mass spectrometry （GC-MS） was developed for the analysis of volatile components in dry Pogostemon. Based on the peak area of patchouli alcohol, the experimental conditions for HS-SPME were optimized. The optimum conditions were： 30 mg Pogostemon cablin powder, which was 10 times diluted using anhydrous sodium sulfate, was placed into a 15 mL extraction tube. After incubated at 80 ℃ for 40 min with stirring speed of 250 r/min, polydimethylsiloxane/divinylbenzene （PDMS-DVB） coated fiber was inserted and extracted for 40 min at 80 ℃ with the same stirring speed. Then the fiber was inserted into the injection port and desorption for 100 s at 250 ℃. DB-SMS capillary with a flow rate of 1 mL/min was used for GC separation. The average recovery of patchouli alcohol under the optimum conditions was 91.8% with a RSD of 3.0%. Then the content of patchouli alcohol in ten samples of Pogostemon cablin from different areas was determined, the other main volatile components in Pogostemon were also calculated by using patchouli alcohol as reference standard. The results show that the developed method is simple, rapid and reliable, which is suitable for qualitative and quantitative analysis of volatile compounds in Pogostemon cablin.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2009年第2期283-287,共5页
Chinese Journal of Analytical Chemistry
关键词
顶空固相微萃取
气相色谱质谱法
广藿香
百秋里醇
Head-space solid phase microextraction, gas chromatography-mass spectrometry, Pogostemon,patchouli alcohol
