枳壳药材挥发油的GC-MS指纹图谱研究

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/z35~550.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 Solution2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.%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.