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目的:建立当归六黄汤的HPLC指纹图谱分析方法,对色谱数据进行分析,并建立高效液相-质谱(LC-MS)法分析当归六黄汤汤剂中主要成分。方法:HPLC采用Agela Venusil XBP-C18色谱柱(4.6 mm×250 mm,5.0μm),流动相乙腈(A)-0.3%甲酸水溶液(B)梯度洗脱(0~10 min,5%~15%A;10~15 min,15%~20%A;15~35 min,20%~25%A;35~50 min,25%~31%A;50~62 min,31%~55%A;62~70 min,55%~60%A;70~75 min,60%~70%A),柱温30℃,体积流量0.8 m L·min-1;质谱采用电喷雾离子源,正负离子模式下全扫描检测,并通过[M-H]-,[M+H]+等离子信息推断化合物。结果:建立当归六黄汤汤剂的HPLC分析方法及指纹图谱,并建立当归六黄汤汤剂的LC-MS图谱,指认汤剂中主要的19个特征色谱峰。结论:当归六黄汤HPLC指纹图谱分析方法稳定可靠,具有较好的重复性;通过建立LC-MS图谱,更加有效的指认了当归六黄汤汤剂中的主要成分。
Objective: To establish an HPLC fingerprinting method for Angelica Liuhuang decoction, analyze the chromatographic data, and establish the HPLC-MS method to analyze the main components of Angelica Liuhuang decoction. METHODS: HPLC was performed on a Agela Venusil XBP-C18 column (4.6 mm × 250 mm, 5.0 μm) with a mobile phase of acetonitrile (A) -0.3% aqueous formic acid (B) A, 10-15 min, 15-20% A, 15-35 min, 20-25% A, 35-50 min, 25-31% A, 50-62 min, 31-55% A, 70-75 min, 60-70% A), column temperature was 30 ℃ and volume flow rate was 0.8 m L · min-1. Electrospray ionization (ESI) source, positive and negative ion mode Under full scan detection, compounds were extrapolated from [MH] -, [M + H] + plasma information. Results: HPLC method and fingerprint of Danggui Liuhuang decoction were established. The LC-MS spectrum of Danggui Liuhuang decoction was established, and the main 19 characteristic chromatographic peaks in decoction were identified. Conclusion: The HPLC fingerprinting method of Angelica Liuhuang decoction is stable and reliable with good reproducibility. By establishing LC-MS spectra, it is more effective to identify the main components of Angelica Liuhuang decoction.