牛胆粉高效液相色谱法特征图谱研究

目的:探求比较黄牛胆粉和水牛胆粉的HPLC特征图谱,为建立牛胆粉的特征图谱提供依据。方法:采用梯度洗脱技术进行HPLC分离分析。色谱柱为Lichrospher C18(4.6 mm×250 mm,5μm),以乙腈-0.001 mol.L-1 KH2PO4溶液为流动相,梯度洗脱(0～20 min,乙腈30%→30%;20～40 min,乙腈30%→40%;40～70 min,乙腈40%→50%;70～80 min,乙腈50%→50%),流速1.0mL.min-1;柱温30℃;DAD检测器,检测波长210 nm。用聚类分析方法处理色谱特征信息,比较色谱以胆酸为参照色谱峰的22个特征峰的信息。结果:通过分析10批黄牛胆粉和水牛胆粉样品,确定了22个共有峰,建立了牛胆粉的HPLC特征图谱。结论:黄牛胆粉和水牛胆粉的色谱指纹特征比较相近,但特征成分含量有一定差异。

Study on HPLC fingerprint characteristic of the ox bile powder

OBJECTIVE To investigate HPLC fingerprint characteristic for the bile powder of Bos Taurus domesticus Gmelin and the Bubalus Linnaeus,and provide basis for the establishment of chromatographic fingerprint of ox bile powder.METHODS The HPLC was run on Lichrospher C18(4.6 mm×250 mm,5 μm) column with acetonitrile-water(0.1% potassium dihydrogen phosphate) as mobile phase in gradient elution(0-20 min acetonitrile 30%→30%,20-40 min acetonitrile 30%→40%,40-70 min acetonitrile 40%→50%;70-80 min,acetonitrile 50%→50%) at a flow rate of 1.0 mL·min-1.The temperature of column was 30 ℃.The detection wavelength and reference wavelength were 210 nm with DAD detector.The information of 22 fingerprint peaks compared with cholic acid was treated by cluster analysis.RESULTS Through the analysis of 10 batches samples of the bile powder of Bos Taurus domesticus Gmelin and the Bubalus Linnaeus,22 peaks were identified,and the HPLC fingerprint of the ox bile powder was established.CONCLUSION HPLC fingerprint characteristic for the bile powder of Bos Taurus domesticus Gmelin and the Bubalus Linnaeus are similarity,but there is a certain difference in content among the characteristic ingredients.