枳殼藥材揮發(fā)油的GC—MS指紋圖譜研究
發(fā)布時(shí)間:2019-08-30 來源: 歷史回眸 點(diǎn)擊:
中圖分類號(hào) R927.2 文獻(xiàn)標(biāo)志碼 A 文章編號(hào) 1001-0408(2018)04-0461-05
DOI 10.6039/j.issn.1001-0408.2018.04.08
摘 要 目的:建立枳殼藥材揮發(fā)油的氣相色譜-質(zhì)譜(GC-MS)指紋圖譜。方法:采用GC-MS法,色譜柱為RTX-5MS毛細(xì)管柱,進(jìn)樣口溫度為250 ℃,載氣為高純氦氣(≥99.999%),流速為1.0 mL/min,分流比為10 ∶ 1,進(jìn)樣量為1 μL(程序升溫);采用電子轟擊離子源,離子源溫度為230 ℃,檢測(cè)器溫度為250 ℃,溶劑延遲時(shí)間為3 min,掃描范圍為m/z 35~550。以月桂烯為參照,測(cè)定21批藥材揮發(fā)油樣品的GC-MS圖譜,采用《中藥色譜指紋圖譜相似度評(píng)價(jià)系統(tǒng)》(2004 A版)進(jìn)行相似度評(píng)價(jià),確定共有峰,采用LC Solution 2質(zhì)譜庫(kù)(NIST05.LIB和NIST05s.LIB)確定共有峰成分,并采用面積歸一化法測(cè)定共有峰的相對(duì)含量。結(jié)果:21批藥材揮發(fā)油樣品的GC-MS圖譜有20個(gè)共有峰,相似度均>0.90;經(jīng)驗(yàn)證,21批藥材揮發(fā)油樣品GC-MS圖譜與對(duì)照指紋圖譜具有較好的一致性。枳殼藥材揮發(fā)油主要成分為檸檬烯、萜品烯、月桂烯和D-Cadinene。結(jié)論:所建指紋圖譜可為枳殼藥材揮發(fā)油的真?zhèn)舞b別和質(zhì)量評(píng)價(jià)提供參考。
關(guān)鍵詞 枳殼;揮發(fā)油;氣相色譜-質(zhì)譜指紋圖譜;道地藥材
ABSTRACT OBJECTIVE: To establish GC-MS fingerprint of volatile oil from Citrus aurantium. METHODS: GC-MS method was adopted. The determination was performed on RTX-5MS capillary column with injector temperature of 250 ℃, high pure helium as carrier gas(≥99.999%), flow rate of 1.0 mL/min, split ratio of 10 ∶ 1, and sample size of 1 μL (temperature programming). Mass spectrum condition included electron bombardment ion source, ion source temperature of 230 ℃, detector temperature of 250 ℃, 3 min solvent delay, scanning range of m/z 35-550. GC-MS chromatograms of 21 batches of volatile oil samples were determined using Laurene as reference. The similarity of them was evaluated by using TCM Chromatographic Fingerprint Similarity Evaluation System (2004 A edition), and common peak was determined. The components of common peak were determined by LC Solution 2 mass database (NIST05.LIB and NIST05s.LIB). Relative content of common peak was determined with area normalization. RESULTS: There were 20 common peaks in GC-MS chromatograms of 21 batches of volatile oil samples, and the similarity was higher than 0.90. After validation, GC-MS chromatograms of 21 batches of volatile oil samples were in good agreement with control fingerprint. The main constituents of the volatile oil of C. aurantium were Limonene,Terpinene, Laurene and D-Cadinene. CONCLUSIONS: Established fingerprint can provide reference for identification and quality evaluation of volatile oil of C. aurantium.
KEYWORDS Citrus aurantium; Volatile oil; GC-MS fingerprint; Genuine regional drug
枳殼為蕓香科植物酸橙(Citrus aurantium L.)及其栽培變種的干燥未成熟果實(shí)[1],有理氣寬中之功效,多用于食積不化、脘腹脹滿等癥狀[2],F(xiàn)代藥理學(xué)研究表明,枳殼具有抗炎、抗菌、抗病毒、抗腫瘤、抗?jié)、減少毛細(xì)血管脆性等作用[3]。
我國(guó)枳殼藥材3個(gè)道地產(chǎn)區(qū)為湖南沅江、江西新干和重慶江津,市場(chǎng)多以藥材出處加以區(qū)分,分別稱為湘枳殼、江枳殼和川枳殼。中藥指紋圖譜是一種綜合的、可量化的鑒定手段,主要用于評(píng)價(jià)中藥材以及中藥制劑半成品質(zhì)量的真實(shí)性、優(yōu)良性和穩(wěn)定性[4-5],F(xiàn)有研究對(duì)枳殼藥材的氣相色譜-質(zhì)譜(GC-MS)指紋圖譜報(bào)道較少,本試驗(yàn)收集了全國(guó)不同產(chǎn)地的21批枳殼藥材,采用GC-MS法建立了其揮發(fā)油指紋圖譜,旨在為枳殼藥材的鑒別和中成藥的質(zhì)量控制提供科學(xué)依據(jù)。
相關(guān)熱詞搜索:枳殼 揮發(fā)油 圖譜 指紋 藥材
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