枳殼藥材揮發(fā)油的GC—MS指紋圖譜研究

　　中圖分類號 R927.2 文獻標志碼 A 文章編號 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毛細管柱，進樣口溫度為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 ℃，檢測器溫度為250 ℃，溶劑延遲時間為3 min，掃描范圍為m/z 35～550。以月桂烯為參照，測定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價系統(tǒng)》（2004 A版）進行相似度評價，確定共有峰，采用LC Solution 2質(zhì)譜庫（NIST05.LIB和NIST05s.LIB）確定共有峰成分，并采用面積歸一化法測定共有峰的相對含量。結(jié)果：21批藥材揮發(fā)油樣品的GC-MS圖譜有20個共有峰，相似度均>0.90；經(jīng)驗證，21批藥材揮發(fā)油樣品GC-MS圖譜與對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)量評價提供參考。
　　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[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)代藥理學研究表明，枳殼具有抗炎、抗菌、抗病毒、抗腫瘤、抗?jié)�瘍、減少毛細血管脆性等作用[3]。
　　我國枳殼藥材3個道地產(chǎn)區(qū)為湖南沅江、江西新干和重慶江津，市場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，主要用于評價中藥材以及中藥制劑半成品質(zhì)量的真實性、優(yōu)良性和穩(wěn)定性[4-5]�，F(xiàn)有研究對枳殼藥材的氣相色譜-質(zhì)譜（GC-MS）指紋圖譜報道較少，本試驗收集了全國不同產(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)量控制提供科學依據(jù)。

相關(guān)熱詞搜索：枳殼 揮發(fā)油 圖譜 指紋 藥材