枳壳药材挥发油的GC—MS指纹图谱研究

发布时间:2019-08-30 来源: 历史回眸 点击:


  中图分类号 R927.2 文献标志码 A 文章编号 1001-0408(2018)04-0461-05
  DOI 10.6039/j.issn.1001-0408.2018.04.08
  摘 要 目的:建立枳壳药材挥发油的气相色谱-质谱(GC-MS)指纹图谱。方法:采用GC-MS法,色谱柱为RTX-5MS毛细管柱,进样口温度为250 ℃,载气为高纯氦气(≥99.999%),流速为1.0 mL/min,分流比为10 ∶ 1,进样量为1 μL(程序升温);采用电子轰击离子源,离子源温度为230 ℃,检测器温度为250 ℃,溶剂延迟时间为3 min,扫描范围为m/z 35~550。以月桂烯为参照,测定21批药材挥发油样品的GC-MS图谱,采用《中药色谱指纹图谱相似度评价系统》(2004 A版)进行相似度评价,确定共有峰,采用LC Solution 2质谱库(NIST05.LIB和NIST05s.LIB)确定共有峰成分,并采用面积归一化法测定共有峰的相对含量。结果:21批药材挥发油样品的GC-MS图谱有20个共有峰,相似度均>0.90;经验证,21批药材挥发油样品GC-MS图谱与对照指纹图谱具有较好的一致性。枳壳药材挥发油主要成分为柠檬烯、萜品烯、月桂烯和D-Cadinene。结论:所建指纹图谱可为枳壳药材挥发油的真伪鉴别和质量评价提供参考。
  关键词 枳壳;挥发油;气相色谱-质谱指纹图谱;道地药材
  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
  枳殼为芸香科植物酸橙(Citrus aurantium L.)及其栽培变种的干燥未成熟果实[1],有理气宽中之功效,多用于食积不化、脘腹胀满等症状[2]。现代药理学研究表明,枳壳具有抗炎、抗菌、抗病毒、抗肿瘤、抗溃疡、减少毛细血管脆性等作用[3]。
  我国枳壳药材3个道地产区为湖南沅江、江西新干和重庆江津,市场多以药材出处加以区分,分别称为湘枳壳、江枳壳和川枳壳。中药指纹图谱是一种综合的、可量化的鉴定手段,主要用于评价中药材以及中药制剂半成品质量的真实性、优良性和稳定性[4-5]。现有研究对枳壳药材的气相色谱-质谱(GC-MS)指纹图谱报道较少,本试验收集了全国不同产地的21批枳壳药材,采用GC-MS法建立了其挥发油指纹图谱,旨在为枳壳药材的鉴别和中成药的质量控制提供科学依据。

相关热词搜索:枳壳 挥发油 图谱 指纹 药材

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