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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。
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.
丹七软胶囊脂溶性成分气相色谱-质谱联用指纹图谱
Danqi soft capsuleLiposoluble constituentsGC-MSFingerprint
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