世界中医药

目的:基于气相色谱-质谱研究方法检测分析加味逍遥丸中的挥发性成分。方法:首先采用水蒸气蒸馏法提取加味逍遥丸供试品溶液中的挥发性成分,以正十八烷为内标物进行参照,通过正交试验设计研究,将提取时间9 h、固液比1:15、浸泡时间10 h时是水蒸馏法提取加味逍遥丸中挥发性成分的最佳提取条件,进一步分析加味逍遥丸中挥发性成分的气相色谱-质谱图及具体化学成分,GC-MS色谱质谱研究方法色谱条件:选择直径为0.25 μm的Rxi-5ms的色谱柱(规格:30 m×0.25 mm),柱流量为1 mL/min;以氦气(He)为载气,采用30:1的分流比;进样量:0.5 μL,以260 ℃为进样口温度,升温程序:首先保持初始柱温60 ℃ 3 min,随后以10 ℃/min的升温速率升至175 ℃,再下降10倍升温速率以1 ℃/min缓慢升温至195 ℃,最后增加5倍升温速率以5 ℃/min升温至240 ℃,维持15 min后再缓慢升至250 ℃的接口温度;溶剂延迟时间为3 min。质谱条件:电子轰击离子源的轰击能量设置为70 eV,离子源温度设置为200 ℃;以0.7KV为检测电压;采用全谱扫描,其质量扫描范围为m/z 40~550 amu。结果:气相色谱-质谱研究方法严谨性精密度、重复性和稳定性试验结果均良好。加味逍遥丸在气相色谱-质谱研究中以正十八烷(S)为内标物,检测到53中挥发性成分。将总离子流色谱图中所检测出的色谱峰与NIST标准质谱数据库中的标准谱图进行参照比较,分析53个挥发性成分的具体化学成分信息,其中芳香族类和萜烯类挥发性成分均有11种,萜醇类挥发性成分有8中种,醛类挥发性成分有6种。结论:气相色谱-质谱方法研究加味逍遥丸中挥发性物质,分析其具体化学成分,为加味逍遥丸的质量控制提供依据。

English Summary:

To detect the volatile components in Modified Xiaoyao Pills by gas chromatography mass spectrometry.Methods:The volatile components in the solution of Modified Xiaoyao Pills were extracted by steam distillation.N-octadecane was used as internal standard substance for reference.Through the design of the orthogonal experiment,it was found that when the extraction time was 9 hours,the solid-liquid ratio was 1:15,and the soaking time was 10 hours,it was the best time to extract the volatile components in Modified Xiaoyao Pills by water distillation.The gas chromatography-mass spectrum and the specific chemical components of volatile components in Modified Xiaoyao Pills were analyzed.The chromatography condition of GC-MS chromatogram mass spectrometric study:the Rxi-5ms chromatographic column (30 m×0.25 mm) was selected,the column flow rate was 1 mL/min; the flow ratio of helium gas (He) was used as the carrier gas,and the flow ratio of 30:1 was adopted; the sample volume was 0.5 μL,the inlet temperature was 260 ℃.The temperature rising procedure started.First the temperature of the initial column temperature was 60 ℃ for 3 minutes,the temperature rose to 175 ℃ by the heating rate of 10 ℃/min,and decreased by 10 times at the rate of 1 ℃/min to 195 ℃,and at last increased the heating rate 5 times to 240 ℃ at the rate of 5 ℃/min,and then slowly increased to 250 ℃ after 15 minutes,and the delay time of solvent was 3 minutes.Mass spectrum condition:the bombardment energy of the electronic bombardment ion source was set to 70eV,the temperature of the ion source was set to 200 c,and the voltage was detected by 0.7 KV; the scanning range of the total spectrum was m/z40-550amu.Results:The accuracy,repeatability and stability of the GC-MS method were good.In the GC-MS study,N-octadecane (S) was used as the internal standard substance in Modified Xiaoyao Pills to detect the volatile components in 53.By comparing the chromatographic peaks detected in the total ion flow chromatogram with the standard spectra of NIST standard mass spectrometry database,the specific chemical composition information of the 53 volatile components was analyzed,including 11 aromatic and terpene volatile components,8 species of terpene alcohols and 6 kinds of aldehydes.Conclusion:Gas chromatography-mass spectrometry (GC-MS) is used to study the volatile substances in Modified Xiaoyao Pills,and to analyze its specific chemical composition and provide the basis for the quality control of Modified Xiaoyao Pills.

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