澳門大學碩士論文 Abstract Head-space solid phase microextraction (HS-SPME) has become one of the preferred techniques in aroma analysis, offering solvent free, rapid sampling with low cost and ease preparation. HS-SPME is sensitive, selective and compatible with low detection limits, which has been intensively used for the analysis of Chinese medicines. However, its application in the quantitative analysis was limited due to its complex transition of the volatile analytes. Although multiple HS-SPME has been used for the quantitative analysis, its application still restricted because of the inconvenient of multiple HS-SPМЕ. In present study, a one-step HS-SPME coupled to gas chromatography-mass spectrometry (GC-MS) method was developed for the analysis of volatile components in dry Pogostemon cablin. 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 incubating at 80 °C for 40 min with stirring speed of 250 r/min, PDMS-DVB coated fiber was inserted and extracted for 40 min at 80 °C with the same stirring speed. Then the fiber was inserted into the injection port and desorption for 100 seconds at 250 °C. DB-5MS capillary with the flow rate of ImL/min was used for GC-MS analysis. Column temperature program: initial temperature was 90 'C, and then programmed at 0.8 'C/min to 110 °C and held for 5 min at the temperature of 110 °C, then at 1.0°C/min to 134 °C and held for 5 min at the temperature of 134 'C, and finally, at 5.0 °C/min to 143 °C, and held for 10 min at the temperature of 143 °C. The average recovery of patchouli alcohol under the optimum conditions was 91.8 % with RSD 3.0 %. Then the content of patchouli alcohol in ten samples of Pogostemon cablin from different areas were determined, the other main volatile components in Pogostemon were also estimated by using patchouli alcohol as reference standard. The results showed that the developed method is simple, rapid and reliable, which is suitable for qualitative and quantitative analysis of volatile compounds in Pogostemon cablin. Key words: Head-space solid phase microextraction (HS-SPME), gas chromatography-mass spectrometry (GC-MS), Pogostemon cablin, Patchouli alcohol III

澳門大學碩士論文 摘要 固相微萃取技術(Solid Phase Micro-extraction, SPME)集取樣、萃取及富 集於一體,操作簡便,而且具有萃取速度快、操作成本低以及便於實現自動化等優 點,在中藥揮發性成分分析中得到了廣泛的應用。頂空固相微萃取(head-space solid phase microextraction, HS-SPME)在萃取過程中纖維頭不與樣品直接接 觸,大大延長了萃取頭的使用壽命。另外,在分析中藥材揮發性成分的過程 中, HS-SPME 可以對固態樣品直接進行採樣,消除了在溶劑提取過程中由於揮發 性成分的丟失及副產物的產生等對分析結果準確性的影響。但由於揮發性組分間 的基質效應及較為複雜的擴散和吸附過程, HS-SPME 定量分析尚存在許多技術問 題。本文利用較少樣品量情況下,被測物1次萃取量近似等於其總量,建立了外標 法1次HS-SPME 定量分析廣 香 Pogostemon cablin (Blanco) Benth. 中揮發性 成分,並與多次萃取結果進行比較,探討一次萃取 HS-SPME/GC-MS 法定量分析中 藥揮發性成分的可行性。本文共分為三個章節: 第一章 固相微萃取的發展概況,主要介紹它的原理,裝置,應用等方面情況。另 外,對廣霍香的研究現狀進行了分析,主要在廣香的藥理研究、化學成 分及其定性定量分析等方面進行了論述 第二章 建立了頂空固相微萃取的方法並對此方法進行了條件的優化,採用 PDMS-DVB 萃取頭 HS-SPME/GC/MS 法測得百秋裏醇的平均回收率為 91.8%,RSD為3.0%。通過與多次萃取 HS-SPME/GC/MS 法測定百秋裏 醇的對比結果可以看出,在較少取樣量的情況下,一次萃取即可達到定量 的要求。並對10個廣香樣品進行了檢測。 第三章 對本研究進行了總結。 關鍵字 頂空固相微萃取,氣相色譜質譜法,廣 香,百秋裏醇 II