枳壳药材挥发油的GC-MS指纹图谱研究

Study on GC-MS Fingerprint of Volatile Oil from Citrus aurantium

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 m L/min,分流比为10∶1,进样量为1μL(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。

OBJECTIVE:To establish GC-MS fingerprint of volatile oil from Citrus aurantium. METHODS:GC-MS method was adopted. The determination was performed on RTX-5 MS capillary column with injector temperature of 250 ℃,high pure helium as carrier gas(≥99.999%),flow rate of 1.0 m L/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 of250 ℃,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 NIST05 s.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.