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丹七软胶囊脂溶性成分的GC-MS指纹图谱研究
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| 篇名： | 丹七软胶囊脂溶性成分的GC-MS指纹图谱研究 |
| TITLE： | |
| 摘要： | 目的：建立丹七软胶囊脂溶性成分的气相色谱-质谱（GC-MS）指纹图谱。方法：采用GC-MS 法。色谱柱为DB-5 ms毛细管色谱柱，载气为高纯度氦（99.999％），程序升温，流速为1.0 mL/min， 进样口温度为250 ℃，进样量为1 μL，分流比为1 ∶ 40，分流进样；电离方式为电子轰击离子源，离子源温度为280 ℃， 接口温度为300 ℃，电子能量为 70 eV，溶剂延迟时间为3 min，质荷比（m/z）为50～550。以棕榈酸乙酯为参照，测定11批样品的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，并采用LC Solution 2工作站标准质谱图库（NIST05.LIB和NIST05s.LIB）确定共有峰成分。结果：11批样品相似度均大于0.90；经验证，11批样品的GC-MS图谱均与对照图谱具有较好的一致性。11批样品的GC-MS图谱有49个共有峰，鉴定出38个化学成分（占总峰面积的94.94％）。结论：所建指纹图谱可为丹七软胶囊质量评价提供参考。 |
| ABSTRACT： | OBJECTIVE： To establish GC-MS fingerprints of liposoluble constituents from Danqi soft capsule. METHODS： GC-MS method was adopted. GC chromatogram column was DB-5 ms capillary column with high purity helium （99.999％） as carrier gas at the flow rate of 1.0 mL/min， with temperature programming. The injector temperature was 250 ℃.The sample size was 1 μL. The shunt ratio was 1∶40， with distributary injection. Ionization mode was as follows as electron bombardment ion source， ion source temperature of 280 ℃， injector temperature of 300 ℃， electronic energy of 70 eV， solvent delay time of 3 min， mass charge ratio （m/z） of 50-550. Using ethyl palmitate as reference， MS spectrums of 11 batches of samples were determined. Similarity evaluation was conducted by using TCM Fingerprint Chromatogram Similarity Evaluation System （2004 A edition） to determine common peak. The common peaks were determined by LC Solution 2 workstation standard mass spectrometry Library （NIST05.LIB or NIST05s.LIB）. RESULTS： The similarity of 11 batches of samples was higher than 0.90. After validation， GC-MS chromatograms of 11 batches of samples were in good agreement with control fingerprint. There were 49 common peaks in GC-MS chromatogram， and 38 chemical constituents were identified， accounting for 94.94％ of total peak areas. CONCLUSIONS： Established fingerprint can provide evidence for quality evaluation of Danqi soft capsule. |
| 期刊： | 2018年第29卷第6期 |
| 作者： | 庞颖，刘汉伟，高峰，杨健 |
| AUTHORS： | PANG Ying，LIU Hanwei，GAO Feng，YANG Jian |
| 关键字： | 丹七软胶囊；脂溶性成分；气相色谱-质谱联用；指纹图谱 |
| KEYWORDS： | Danqi soft capsule； Liposoluble constituents； GC-MS； Fingerprint |
| 阅读数： | 322 次 |
| 本月下载数： | 6 次 |
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