不同产地苍艾挥发油的GC-MS指纹图谱研究

Study on GC-MS fingerprints of Cangai volatile oil from different origins

目的:建立苍艾挥发油的气相色谱-质谱(GC-MS)指纹图谱,分析苍艾挥发油的化学组成,为其质量控制提供方法和依据。方法:Agilent DB-5MS石英毛细管色谱柱(30 m×0.25 mm×0.25μm),柱温40℃(保持1 min),以10℃·min^(-1)速率升至130℃(保持5 min),以8℃·min^(-1)速率升至250℃(保持5 min);进样口温度为280℃,载气为高纯氦气,柱流量1 mL·min^(-1);分流比40∶1,进样量1μL;总分离时间35 min,溶剂延迟时间4 min;电离方式El,离子源温度230℃,电子能量70 eV,四级杆温度150℃,辅助加热温度290℃,质荷比(m/z)为50~600。建立14批苍艾挥发油的GC-MS指纹图谱,通过“中药色谱指纹图谱相似度评价系统(2004版)”进行相似度评价,确定共有峰,分析其化学组成及结构,结合NIST11.L数据库对样品中成分进行匹配定性,并利用面积归一化法计算各成分相对含量。结果:14批苍艾挥发油的GC-MS指纹图谱共确定21个共有峰,主要有丁香酚、1,8-桉叶素、β-石竹烯、4-松油醇、α-蒎烯等成分。14批样品指纹图谱与对照图谱的相似度为0.981~0.998。结论:所建立的苍艾挥发油GC-MS指纹图谱共有模式特征性及专属性强,能为苍艾挥发油的质量评价提供参考。

OBJECTIVE To establish the GC-MS fingerprints and analyze the chemical components of Cangai volatile oil from different origins in order to provide the method and basis for its quality control.METHODS The analysis was achieved by using an Agilent DB-5MS(30 m×250 mm×0.25μm)silica capillary chromatographic column(40℃for 1 min,10℃·min^(-1)to 130℃for 5 min,8℃·min^(-1)to 250℃for 5 min).The injector temperature was 280℃and the carrier gas was high purity helium at the flow rate of 1.0mL·min^(-1),the shunt ratio was 40∶1 and the injection volume was 1μL.The total separation time was 35 min and solvent delay time was 4 min.MS conditions were as follows:electron impact(EI)ion source,ion source temperature of 230℃,electronic energy of 70 eV,quadrupole temperature of 150℃,auxiliary heating temperature of 290℃,and mass charge ratio of 50-600.The GC-MS fingerprints of 14 batches of Cangai volatile oil were established,and the similarity was evaluated by"Similarity Evaluation System of Chromatographic Fingerprint of Traditional Chinese Medicine(2004 edition)".The common peaks were determined,and their chemical composition and structure were analyzed.Combined with NIST11.L database,the components in the sample were matched qualitatively,and the relative content of each component was calculated by area normalization method.RESULTS There were 21 common peaks in the GC-MS fingerprints of 14 batches of Cangai volatile oil,mainly including eugenol,1,8-eucalyptol,β-caryophyllene,4-terpineol andα-pinene.The similarities of 14 batches of samples compared with reference fingerprint were 0.981-0.998.CONCLUSION The established GC-MS fingerprint of Cangai volatile oil has strong characteristics and specificity,which can provide reference for the quality evaluation of Cangai volatile oil.