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轻身调脂消渴片的指纹图谱建立、化学模式识别及含量测定
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| 篇名： | 轻身调脂消渴片的指纹图谱建立、化学模式识别及含量测定 |
| TITLE： | Establishment of fingerprint ，chemical pattern recognition and content determination for Qingshen tiaozhi xiaoke tablets |
| 摘要： | 目的 建立轻身调脂消渴片（QTXT）的指纹图谱，并进行化学模式识别分析，同时测定7种成分的含量。方法以盐酸黄连碱为参照，采用《中药色谱指纹图谱相似度评价系统（2012版）》建立13批QTXT的高效液相色谱（HPLC）指纹图谱并进行相似度评价；通过与混合对照品色谱图比对，确认共有峰；通过与各单味饮片样品溶液和各阴性样品溶液色谱图比对，确定共有峰的归属；采用SPSS22.0、SIMCA14.1软件进行聚类分析、主成分分析和正交偏最小二乘法-判别分析，以变量重要性投影（VIP）值大于1为标准筛选影响QTXT质量的标志性成分。以盐酸黄连碱为内参物，采用一测多评（QAMS）法测定柚皮苷、橙皮苷、新橙皮苷、盐酸小檗碱、盐酸巴马汀和洛伐他汀的含量，并与外标法测定结果（盐酸黄连碱除外）进行比较。结果13批QTXT中共有17个共有峰，相似度为0.987～0.999；共指认出7个共有峰，分别为柚皮苷（4号峰）、橙皮苷（5号峰）、新橙皮苷（6号峰）、盐酸黄连碱（8号峰）、盐酸巴马汀（9号峰）、盐酸小檗碱（10号峰）、洛伐他汀（14号峰）。7～10号峰为黄连的专属峰；3～6、11～13号峰为麸炒枳实的专属峰；14号峰为红曲的专属峰；1号峰为黄连和红曲的共有峰；2、15号峰为麸炒枳实和红曲的共有峰；16、17号峰为6味饮片的共有峰。聚类分析结果显示，13批QTXT可聚为3类，其中S2为一类，S1、S9、S10为一类，S3～S8、S11～S13为一类；主成分分析结果显示，前3个主成分的累计方差贡献率为85.120％，与聚类分析相比，主成分分析进一步将S1与S9、S10区分开；正交偏最小二乘-判别分析结果显示，有7个共有峰的VIP值大于1，依次为10号峰（盐酸小檗碱）、9号峰（盐酸巴马汀）、5号峰（橙皮苷）、11号峰、8号峰（盐酸黄连碱）、12号峰、6号峰（新橙皮苷）。QAMS法测得柚皮苷、橙皮苷、新橙皮苷、盐酸小檗碱、盐酸巴马汀、洛伐他汀的含量分别为40.198～77.552、6.138～13.413、71.823～125.868、11.274～49.951、3.303～5.367、1.821～3.185mg/g；外标法测得柚皮苷、橙皮苷、新橙皮苷、盐酸小檗碱、盐酸黄连碱、盐酸巴马汀和洛伐他汀的含量分别为41.454～79.976、6.404～13.993、74.068～129.081、11.627～51.512、5.922～12.020、3.158～5.131、1.901～3.325mg/g。两种方法所得含量测定结果（盐酸黄连碱除外）的偏差均小于3.00％。结论所建HPLC指纹图谱和QAMS法操作简单、准确、重复性好，结合化学模式识别分析可用于评价QTXT的整体质量。盐酸小檗碱、盐酸巴马汀等成分可能是影响该药质量的标志性成分。 |
| ABSTRACT： | OBJECTIVE To e stablish the fingerprint of Qings hen tiaozhi xiaoke tablets （QTXT）and carry out the analysis of chemical pattern recognition ，and determine the contents of seven active components simultaneously. METHODS Using coptisine hydrochloride as reference ，the Similarity Evaluation System for Chromatographic Fingerprint of TCM （2012 edition）was utilized to establish the HPLC fingerprints of 13 batches of QTXT and analyze their similarity. The common peaks were confirmed by comparing with the chromatogram of the mixed control ；the attribution of the common peak was determined by comparing the chromatograms of the sample solutions of single decoction pieces and negative sample solutions ；using SPSS 22.0 and SIMCA 14.1 software，cluster analysis （CA），principal component analysis （PCA）and orthogonal partial least squares-discriminant analysis （OPLS-DA）were carried out ，and the markers affecting the quality of QTXT were screened ，using the variable importance in projection（VIP）value greater than 1 as the standard. Using coptisine hydrochloride as internal reference ，the contents of naringin ， hesperidin，neohesperidin，berberine hydrochloride ，palmatine hydrochloride and lovastatin were determined by quantitative analysis of multicomponents by single marker （QAMS），and then compared wi th the result s（except for coptisine hydrochloride ） of external standard method. RESULTS There were 17 Δ 基金项目：江苏省“双创团队”项目[No.（2018）2024号] ＊硕士研究生。研究方向：中药新药药学。E-mail：2769544062@ common peaks in 13 batches of QTXT ，and the similarity was qq.com 0.987-0.999. Seven chromatographic peaks were identified ， # 通信作者：副研究员，硕士生导师，博士。研究方向：中药药剂 namely naringin （peak 4）， hesperidin （peak 5）， 学。E-mail：tsliur411@sina.com neohesperidin（peak 6），coptisine hydrochloride （peak 8）， ·1204· China Pharmacy 2022Vol. 33 No. 10 中国药房 2022年第33卷第10期 palmatine hydrochloride （peak 9），berberine hydrochlo ride（peak 10），lovastatin（peak 14）. Peaks 7-10 were the exclusive peaks of Coptis chinensis ；peaks 3-6 and 11-13 were the exclusive peaks of bran-fried Fructus aurantii ；peak 14 was the exclusive peak of Monascus purpureus ；peak 1 was the common peak of C. chinensis and M. purpureus . Peak 2 and 15 were the common peak of bran-fried F. aurantii and M. purpureus ；peaks 16 and 17 were the common peaks of 6 traditional Chinese medicines. The results of CA showed that 13 batches of QTXT could be divided into three categories ，S2 was clustered into one category ，S1，S9，S10 were clustered into one category ，S3-S8 and S 11-S13 were clustered into one category. The results of PCA showed that accumulative variance contribution of the first three principal components was 85.120％. Compared with CA ，S1 was further distinguished from S9 and S 10 by PCA. OPLS-DA showed that 7 common peaks with VIP value greater than 1（from large to small ）were peak 10 （berberine hydrochloride ），peak 9（palmatine hydrochloride ），peak 5（hesperidin），peak 11 and peak 8（coptisine hydrochloride ）， peak 12 and peak 6（neohesperidin）. The contents of naringin ，hesperidin，neohesperidin，berberine hydrochloride ，palmatine hydrochloride and lovastatin measured by QAMS were 40.198-77.552，6.138-13.413，71.823-125.868，11.274-49.951，3.303- 5.367，1.821-3.185 mg/g，respectively. The contents of naringin ，hesperidin，neohesperidin，berberine hydrochloride ，coptisine hydrochloride，palmatine hydrochloride and lovastatin measured by external reference method were 41.454-79.976，6.404-13.993， 74.068-129.081，11.627-51.512，5.922-12.020，3.158-5.131 and 1.901-3.325 mg/g，respectively. The deviations of the two methods （except for coptisine hydrochloride ）were all less than 3.00％. CONCLUSIONS The established HPLC fingerprint and the method of QAMS are simple ，accurate and reproducible. Combined with chemical pattern recognition analysis ，it can be used for the quality evaluation of QTXT. Berberine hydrochloride ，palmatine hydrochloride and other components may be the markers affecting the quality of the drug. |
| 期刊： | 2022年第33卷第10期 |
| 作者： | 李思毅，李宏，刘陶世 |
| AUTHORS： | LI Siyi，LI Hong，LIU Taoshi |
| 关键字： | 轻身调脂消渴片；高效液相色谱法；指纹图谱；化学模式识别；一测多评法；含量测定 |
| KEYWORDS： | Qingshen tiaozhi xiaoke tablets ；HPLC；fingerprint；chemical pattern recognition ；QAMS；content determination |
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