蒙药悬钩子木配方颗粒HPLC指纹图谱及含量测定方法研究

Study on HPLC Fingerprint and Content Determination of Rubus Sachalinensis Leveile Formula Granules

目的:建立悬钩子木配方颗粒HPLC指纹图谱及含量测定研究方法,为悬钩子木配方颗粒的质量评价提供依据。方法:采用高效液相色谱法,色谱柱为C_(18)(4.6 mm×250 mm,5μm),以乙腈-0.05%磷酸为流动相,流速1 mL·min^(-1),柱温30℃,检测波长270 nm,测定悬钩子木配方颗粒中鞣花酸和芦丁的含量。建立15批悬钩子木配方颗粒指纹图谱,利用《中药色谱指纹图谱相似度评价系统》进行相似度分析,对特征峰进行指认。结果:含量测定方法学考察鞣花酸和芦丁在一定质量浓度范围内线性关系良好,精密度、重复性、稳定性、加样回收率的RSD均<2%,15批悬钩子木配方颗粒含量测定结果为:鞣花酸0.603%~1.802%,芦丁0.088%~0.333%。建立了15批悬钩子木配方颗粒指纹图谱,共指认10个共有峰,相似度均大于0.900,并指认表儿茶素、鞣花酸、芦丁。结论:建立的悬钩子木配方颗粒HPLC含量测定方法精密度较高,稳定性较好;HPLC指纹图谱分析方法简单,重现性良好,专属性较优,可为蒙药悬钩子木配方颗粒的物质基础及质量控制研究提供参考。

Objective:To establish the HPLC fingerprint,determine the content of Rubus Sachalinensis Leveile formula granules,and provide the basis for the quality evaluation of Rubus Sachalinensis Leveile formula granules.Methods:HPLC was performed on C_(18)(4.6 mm×250 mm,5μm).Acetonitrile-0.05%phosphoric acid was used as the mobile phase,and the flow rate was 1.0 mL·min^(-1).The column temperature was 30℃,and the detection wavelength was 270 nm.The fingerprint of 15 batches of Rubus Sachalinensis Leveile formula granules was established,and the similarity analysis was carried out by the similarity Evaluation System of Traditional Chinese Medicine similarity valuation,and the characteristic peaks were identified.Results:The linear relationship between ellellic acid and rutin was good in a certain mass concentration range,and the RSD of precision,repeatability,stability and sample recovery were all less than 2%.The content of 15 batches of formula particles was determined as follows:ellellic acid 0.603%-1.802%,rutin 0.088%-0.333%.The HPLC fingerprint of Rubus Sachalinensis Leveile formula particles was established,and 10 common peakwere identified,and similarity were greater than 0.900,and identified epicatechin,ellagic acid and rutin.Conclusion:The HPLC method for the determination of Rubus Sachalinensis Leveile formula granules has high precision and good stability.The HPLC fingerprint analysis method is simple,good reproducibility and good specificity,which can provide reference for the material basis and quality control of Rubus Sachalinensis Leveile formula particles.