目的 比较直接粉碎成细粉和挥发油测定法提取天麻丸中的挥发性成分的差异.方法 利用顶空进样气相色谱-质谱联用(GC-MS)仪进行鉴定分析,GC-MS条件:HP-5MS石英毛细管柱(30 m×0.25 mm,0.25μm);起始温度为40℃,保持1 min后以3℃/min的速率升温至195℃,并保持2 min,再以5℃/min的速率升温至240℃,保持6 min至完成分析;载气为氦气;柱流量为1.1 mL/min;分流比为10:1;进样口温度为250℃;EI电离源能量为70 eV;离子源温度为230℃;扫描范围为m/z 45~500.结果 在天麻丸粉末中检测出37种成分,鉴定出26种成分,占总挥发性成分的83.48%;在天麻丸挥发油中检测出32种成分,鉴定出21种成分,占总挥发性成分的87.25%.结论 采用直接粉碎成细粉和挥发油测定法提取得到的天麻丸中挥发性成分有较大差异,为进一步阐明该药的活性物质基础提供了实验数据.该方法为天麻丸气相色谱指纹图谱的研究及其质量控制提供了依据.%Objective To compare the differences of the volatile components of the Tianma Pill were extracted by direct pulverized into fine powder and steam distillation method. Methods The structures were analyzed and identified by headspace GC-MS. The GC-MS conditions were set as follows:HP-5MS quartz capillary column(30 m × 0. 25 mm,0. 25 μm),the initial temperature was 40 ℃ and maintained for 1 min,the temperature was heating to 195 ℃ at a rate of 3 ℃ /min and maintained for 2 min,then heating to 240 ℃at a rate of 5 ℃ /min and maintained for 6 min until completion of analysis. The carrier gas was helium,the column flow rate was 1. 1 mL/min,the split ratio was 10:1,the inlet temperature was 250 ℃,the EI ionization source was 70 eV,the ion source tempera-ture was 230 ℃,the scan range of m/ z 45-500. Results Totally 37 compounds were detected from Tianma Pill powder,among them,only 26 compounds were identified,which accounted for 83. 48% of total volatile composition. Totally 32 compounds were detected from Tianma Pill volatile oil,among them,only 21 compounds were identified,which accounted for 87. 25% of total volatile composition. Conclusion The type of constituents contained in the volatile oil extracted by direct pulverized into fine powder and steam distillation methods are totally different,and GC-MS can be used to identify the structures and relative content of volatile components,the results of this study can provide an experimental basis for development and utilization of Tianma Pill. The proposed method could provide useful information for the basic study on gas chromatography fingerprint and the quality evaluation of Tianma Pill.
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