小金丸脂溶性和水溶性部位的HPLC指纹图谱分析  

HPLC Fingerprint Analysis of Liposoluble and Water-soluble Fractions of Xiaojinwan

作　　者：冯碧 宋娇 慈志敏[1] 曹波 许洪 杜晓娟 林俊芝 张定堃[1] 韩丽[1] 许润春[1] FENG Bi;SONG Jiao;CI Zhi-min;CAO Bo;XU Hong;DU Xiao-juan;LIN Jun-zhi;ZHANG Ding-kun;HAN Li;XU Run-chun(School of Pharmacy,Chengdu University of Traditional Chinese Medicine(TCM),Chengdu 611137,China;Chengdu Yonkon Pharmacy Co.Ltd.,Chengdu 610041,China;Teaching Hospital of Chengdu University of TCM.Chengdu 610075,China)

机构地区：[1]成都中医药大学药学院,成都611137 [2]成都永康制药有限公司,成都610041 [3]成都中医药大学附属医院,成都610075

出　　处：《中国实验方剂学杂志》2020年第18期139-144,共6页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家自然科学基金面上项目(81873232);成都中医药大学中药学学科特色创新科研团队项目(CXTD2018006);成都中医药大学附属医院院基金项目(2017-D-YY-46)。

摘　　要：目的:建立小金丸脂溶性部位、水溶性部位的高效液相色谱法(HPLC)指纹图谱并进行指纹图谱相似度评价,探讨小金丸的质量一致性。方法:采用Welch Ultimate AQ-C18色谱柱(4.6 mm×250 mm,5μm),流动相选择0.1%磷酸水溶液(A)-乙腈(B)梯度洗脱(脂溶性部分:0~5 min,40%B;5~10 min,40%~50%B;10~20 min,50%~60%B;20~30 min,60%~65%B;30~40 min,65%~70%B;40~50 min,70%~80%B;50~60 min,80%~90%B;60~65 min,90%~95%B;65~75 min,95%~100%B;75~80 min,100%B。水溶性部分:0~20 min,2%~5%B;20~30 min,5%~10%B;30~37 min,10%~20%B;37~45 min,20%~30%B;45~50 min,30%~40%B;50~58 min,40%B),流速1 mL·min-1,柱温30℃,脂溶性部位和水溶性部位的检测波长分别设定为202,250 nm,进样量依次为10,20μL。对5个厂家共30批市售小金丸进行HPLC检测,使用主成分分析(PCA)对各部位色谱峰进行分析,并对色谱峰进行指认。结果:指纹图谱共检测出55个色谱峰,30批小金丸指纹图谱相似度差异较大。小金丸脂溶性部位、水溶性部位的指纹图谱相似度RSD分别为21.5%和32.8%,厂家间与厂家内样品质量差异较大,且脂溶性部位成分主导小金丸化学一致性评价结果,其中,来自枫香脂的成分是影响该制剂化学差异的主要原因。结论:市售小金丸质量一致性较差。双部位指纹图谱的建立为小金丸整体质量评控提供了新思路,可为传统丸剂的质量一致性评价提供参考。Objective:High performance liquid chromatography(HPLC)fingerprints of liposoluble and water-soluble fractions of Xiaojinwan were established and the similarity of fingerprints was evaluated,so as to explore the quality consistency of Xiaojinwan.Method:Chromatographic separation was carried out on Welch Ultimate AQ-C18 column(4.6 mm×250 mm,5μm)with the mobile phase of 0.1%phosphoric acid solution(A)-acetonitrile(B)for gradient elution(liposoluble fraction of 0-5 min,40%B;5-10 min,40%-50%B;10-20 min,50%-60%B;20-30 min,60%-65%B;30-40 min,65%-70%B;40-50 min,70%-80%B;50-60 min,80%-90%B;60-65 min,90%-95%B;65-75 min,95%-100%B;75-80 min,100%B;water-soluble fraction of 0-20 min,2%-5%B;20-30 min,5%-10%B;30-37 min,10%-20%B;37-45 min,20%-30%B;45-50 min,30%-40%B;50-58 min,40%B),the flow rate was 1 mL·min-1,the column temperature was 30℃.The detection wavelengths of the liposoluble and water-soluble fractions were 202,250 nm,and their injection volumes were 10,20μL,respectively.A total of 30 batches of Xiaojinwan from five manufacturers were detected by HPLC,the chromatographic peaks of each part were analyzed by principal component analysis(PCA)and identified.Result:A total of 55 chromatographic peaks were detected in the fingerprints,and the similarity of fingerprint of 30 batches of Xiaojinwan was quite different.The relative standard deviations(RSDs)of fingerprint similarity of liposoluble and water-soluble fractions of Xiaojinwan were 21.5%and 32.8%,respectively.There were significant differences in the quality of samples from different manufacturers and the same manufacturer,and the chemical consistency evaluation results were dominated by liposoluble fraction,and the main reason for the chemical difference of this preparation was the composition of Liquidambaris Resina.Conclusion:The quality consistency of Xiaojinwan is poor.The establishment of two-fraction fingerprint provides a new idea for the overall quality evaluation and control of Xiaojinwan,and can provide a reference for the quality consistency evaluatio

关 键 词：小金丸 脂溶性部位 水溶性部位 指纹图谱 相似度 主成分分析(PCA) 高效液相色谱法(HPLC) 

分 类 号：R22[医药卫生—中医基础理论] R94[医药卫生—中医学]