解郁温胆颗粒工艺中间体及制剂的高效液相色谱指纹图谱建立与含量测定OA

Objective To establish a high-performance liquid chromatography(HPLC)fingerprint and content determination method for intermediate and preparation of Jieyu Wendan Granules.Methods The chromatographic column was Kromasil 100-5 C18 column(250 mm×4.6 mm,5 μm),the mobile phase was methanol-0.1%formic acid solution(gradient elution),the detection wavelengths were 318 nm(qualitative analysis)and 283 nm(quantitative analysis),the flow rate was 0.6 mL/min,the column temperature was 25 °C,and the injection volume was 5 μL.The Similarity Evaluation Software for Chromatographic Fingerprint of Traditional Chinese Medicine(2012 edition)was used to establish HPLC fingerprints of the traditional decoction,extract solution,thick paste,dry extract,and preparation of the Jieyu Wendan formula.Common peaks were identified,common components were identified,and similarity evaluation was performed.The contents of naringin and hesperidin in the granules were determined.Results A total of 23 common peaks were identified in the HPLC fingerprint of 13 batches of samples,and 14 components were identified by comparison with the reference substances.Except for three batches of dry extract showing relatively low similarity,the similarities of other samples were all above 0.90.The linear ranges of naringin and hesperidin were 21.06-1 053 μg and 20.78-1 039 μg,respectively(r>0.999 9).The RSDs of precision,stability,and repeatability test results were all lower than 2%(n=6).The average recovery rates were 102.76%(RSD=0.87%)and 96.80%(RSD=0.82%),respectively.The average contents were 5.437 mg/g and 5.734 mg/g,respectively.Conclusion The established HPLC fingerprint method exhibits good stability.The established content determination method is simple,sensitive,reproducible,and accurate,which can be used for the quality control of Jieyu Wendan Granules.