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UM E-Theses Collection (澳門大學電子學位論文庫)

Title

龍血竭的化學成分及廣佛手的化學成分分析研究

English Abstract

In order to elucidate the active compounents of Resina Draconis, systematical study on chemical constituents of Resina Draconis were carried out, which led to the isolation of thirteen compounds. Based on physic-chemical characters and extensive spectroscopic methods , the structure of the compounds were identified as: pinostilbene (LXJ-01), pinosylvin (LXJ-02), (E)-4-methyl-5-styrylbenzene-1, 3-diol (LXJ-03), 7, 4'-dihydroxyflavone (LXJ-04), 7, 3'-dihydroxy-4'-methoxyflavone (LXJ-05), apigenin (LXJ-06), 7, 4'-dihydroxyflavan (LXJ-07), broussin (LXJ-08), methyl-p-hydroxybenzoate (LXJ-9), ethyl-p-hydroxybenzoate (LXJ-10), 7-hydroxy-3-(4-hydroxybenzyl)chroman (LXJ-11), cochinchinenin C (LXJ-12), β-sitosterol (LXJ-13), respectively. Among them, compound 3 is a new compound. In addition, 2 and 9 are purified for the first time in this genus, 1 and 6 are isolated from this plant for the first time. Meanwhile, as the second part of this thesis, a high performance liquid chromatography coupled with diode array detector (HPLC-DAD) method was estalblished for simultaneous quantification of eleven major bioactive components including six coumarins, three flavonoids and two limonoids in Fructus Citris Sarcodactylis. The analysis was performed on a Cosmosil 5 C18-MS-II column (4.6 mm × 250 mm, 5 μm) with water-acetonitrile gradient elution. The method was validated in terms of linearity, sensitivity, precision, stability and accuracy. It was found that the calibration curves for all analytes showed good linearity (R 2 >0.9993) within the test ranges. The overall limit of detection (LOD) and limit of quantification (LOQ) were less than 3.0 and 10.2 ng for DAD. The relative standard deviations (RSDs) for intra- and inter-day repeatability were no more than 4.99 % and 4.92 %, respectively. The sample was stable for at least 48 h. The recoveries of eleven components were 95.1 % to 104.9 %. The established method was successfully applied to determine eleven components in three samples from different locations. The results showed that the newly-developed HPLC-DAD method was linear, sensitive, precise and accurate, and could be used for quality control of Fructus Citris Sarcodactylis. vi

Chinese Abstract

為了探索龍血竭藥材中的活性成分,為其開發利用及質量控制提供科學依 據,本課題對龍血竭進行了系統的化學成分研究。綜合運用各種現代色譜技術, 從龍血竭中分離得到 15 個化合物,並根據理化常數和波譜数据分析的方法鑒定 了其中 13 個化合物的結構,分別為松茋 (LXJ-01)、赤松素 (LXJ-02)、2-甲基 赤松素 (LXJ-03)、7, 4'-二羥基黃酮 (LXJ-04)、4'-甲氧基-3', 7-二羥基黃酮 (LXJ-05)、芹菜素 (LXJ-06)、4', 7-二羥基黃烷 (LXJ-07)、構樹素 (LXJ-08)、對 羥基苯甲酸甲酯 (LXJ-9)、對羥基苯甲酸乙酯 (LXJ-10)、7-羥基-3-(4-羥基苄基)- 色原烷 (LXJ-11)、劍葉龍血素 C (LXJ-12)、β-穀甾醇 (LXJ-13)。其中 LXJ-03 為新化合物,LXJ-02、LXJ-09 為首次從本屬植物中分離得到,LXJ-01、LXJ-06 為首次從本種植物中分離得到。 本論文的第二部分為廣佛手中活性成分的含量測定。為此,通過建立 HPLC 測定方法,同時定量分析廣佛手(Fructus Citri Sarcodactylis)中 11 種活性成分,包 括 6 種香豆素(異莨菪亭、莨菪亭、7-羥基香豆素、6, 7-二甲氧基香豆素、5, 7- 二甲氧基香豆素與佛手柑內酯),3 種黃酮(橙皮苷、香葉木甙及 3, 5, 6-三羥基 -3', 4', 7-三甲氧基黃酮)以及2種檸檬苦素(檸檬苦素與諾米林)。色譜柱:Cosmosil 5 C18-MS-Ⅱ (4.6 mm × 250 mm, 5 μm);流動相:水 (A)-乙腈 (B);梯度洗脫 程式 (B):0-10 min,18-23 %;10-15 min,23 %;15-30 min,23-50 %;30-40 min, 50-100 %;流速:1.0 mL·min-1;檢測波長:210,254,280,320,340 nm。在 相應的線性範圍內,11 種化合物的標準曲線方程均 R 2 >0.9993,檢測限 (LOD) 與定量限 (LOQ)分別小於 3.0 與 10.2 ng,日內精密度與日間精密度 RSD 值分別 小於 4.99 %與 4.92 %,平均加樣回收率為 95.1 %-104.9 %,樣品在 48 h 內穩定。 並測量了來自不同採集地點的 10 個批次樣品中 11 種化合物的含量。該方法具有 線性良好,快速準確,重現性好等特點,為廣佛手質量評價寄質量控制提供了科 學依據。 關鍵字:龍血竭;黃酮;二苯乙烯;佛手;香豆素;HPLC-DAD;檸檬苦素

Issue date

2012.

Author

楚俊

Faculty

Institute of Chinese Medical Sciences

Degree

M.Sc.

Subject

Medicinal plants -- China -- Analysis.

藥用植物 -- 中國 -- 化學分析.

Herbs -- Therapeutic use.

草本植物 -- 治療用途.

Supervisor

張慶文

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