Article(id=1240688794056323983, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1240688783964819588, articleNumber=null, orderNo=null, doi=10.16155/j.0254-1793.2023-0543, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=null, receivedDateStr=null, revisedDate=1718121600000, revisedDateStr=2024-06-12, acceptedDate=null, acceptedDateStr=null, onlineDate=1773732859386, onlineDateStr=2026-03-17, pubDate=1727625600000, pubDateStr=2024-09-30, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773732859386, onlineIssueDateStr=2026-03-17, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773732859386, creator=13701087609, updateTime=1773732859386, updator=13701087609, issue=Issue{id=1240688783964819588, tenantId=1146029695717560320, journalId=1205117023404326918, year='2024', volume='44', issue='9', pageStart='1463', pageEnd='1645', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773732856979, creator=13701087609, updateTime=1773733032821, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1240689521587712627, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1240688783964819588, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1240689521587712628, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1240688783964819588, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1586, endPage=1596, ext={EN=ArticleExt(id=1240688794358313892, articleId=1240688794056323983, tenantId=1146029695717560320, journalId=1205117023404326918, language=EN, title=Establishment of HPLC fingerprints and determination of six components for Zilian Shengji gel, columnId=1206272758774821315, journalTitle=Chinese Journal of Pharmaceutical Analysis, columnName=Standard Deliberation, runingTitle=null, highlight=null, articleAbstract=

Objective: To establish the HPLC fingerprints for Zilian Shengji gel and to determine the contents of gallic acid, tableberberine, coptisine, palmatine, berberine and shikonin. Methods: The establishment of fingerprints was performed on a 25 ℃ thermostatic Agilent C18-WR(250 mm×4.6 mm, 5 μm)column with the mobile phase comprising of acetonitrile -0.15% phosphoric acid water at the flowing rate of 0.8mL·min-1 in a gradient elution manner, and the detection wavelength were set at 270 nm, 345 nm and 516 nm. Cluster analysis, principal component analysis(PCA) and orthogonal partial least squares discriminant analysis(OPLS-DA) were adopted in chemical pattern recognition. The six components identified were quantitatively determined. Results: The HPLC fingerprint of Zilian Shengji gel was constructed with twenty-six common chromatographic peaks, eleven batches of samples with the similarities of 0.828-0.997, six chromatographic peaks of gallic acid, tableberberine, coptisine, palmatine, berberine and shikonin were identified by reference substance comparison. Six constituents showed good linear relationships within their own ranges (r≥0.999 5) whose average recoveries were 98.7%-99.3%, with the RSDs of 1.3%-1.8%. The content ranges of the above mentioned six components in eleven batches of samples were 827.74-1 513.50 μg·g-1, 137.52-296.05 μg·g-1, 381.83-884.73 μg·g-1, 2 023.81-4 051.66 μg·g-1, 524.15-986.13 μg·g-1 and 47.65-549.46 μg·g-1. Conclusion: This simple, stable, reliable and reproducible method can be used for the quality control of Zilian Shengji gel.

, correspAuthors=Xi-xiang LI, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=Zhi-pan YAN, Xi-xiang LI, Li-xia GAO), CN=ArticleExt(id=1240688797680201801, articleId=1240688794056323983, tenantId=1146029695717560320, journalId=1205117023404326918, language=CN, title=紫连生肌凝胶剂HPLC指纹图谱建立及6个成分含量测定, columnId=1206272758971953622, journalTitle=药物分析杂志, columnName=标准研讨, runingTitle=null, highlight=null, articleAbstract=

目的:建立紫连生肌凝胶剂指纹图谱,并测定没食子酸、表小檗碱、黄连碱、巴马汀、小檗碱和左旋紫草素的含量。方法:采用Agilent C18-WR(250 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-0.15%磷酸水,梯度洗脱,流速0.8 mL·min-1,柱温25 ℃,检测波长270、345、516 nm,结合聚类分析、主成分分析和正交偏最小二乘法判别分析对紫连生肌凝胶剂的指纹图谱进行化学模式识别,并对指定的6个成分进行定量分析。结果:建立了紫连生肌凝胶剂指纹图谱,共标定26个共有峰,与对照指纹图谱的相似度为0.828~0.997;指认出没食子酸、表小檗碱、黄连碱、小檗碱、巴马汀和左旋紫草素6个色谱峰。6个成分在各自范围内线性关系良好(r≥0.999 5),平均加样回收率在98.7%~99.3%,RSD 在1.3%~1.8%。11批样品中6个成分含量分别为827.74~1 513.50 μg·g-1、137.52~296.05 μg·g-1、381.83~884.73 μg·g-1、2 023.81~4 051.66 μg·g-1、524.15~986.13 μg·g-1和47.65~549.46 μg·g-1结论:该方法简便,稳定可靠,重复性好,可用于紫连生肌凝胶剂的质量控制。

, correspAuthors=李喜香, authorNote=null, correspAuthorsNote=
** Tel: 15002550389; E-mail:
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Tel: 18193140379; E-mail:

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Smith by HPLC, refAbstract=null), Reference(id=1240704467415388992, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, doi=null, pmid=null, pmcid=null, year=2022, volume=42, issue=11, pageStart=1917, pageEnd=null, url=null, language=null, rfNumber=[19], rfOrder=36, authorNames=陈芳园, 张云静, 赵冰, journalName=药物分析杂志, refType=null, unstructuredReference=陈芳园,张云静,赵冰,等. 华佗救心丸GC-MS特征图谱及3个成分的含量测定[J]. 药物分析杂志202242 (11):1917, articleTitle=华佗救心丸GC-MS特征图谱及3个成分的含量测定, refAbstract=null), Reference(id=1240704467495080771, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, doi=null, pmid=null, pmcid=null, year=2022, volume=42, issue=11, pageStart=1917, pageEnd=null, url=null, language=null, rfNumber=[19], rfOrder=37, authorNames=CHEN FY, ZHANG YJ, ZHAO B, journalName=Chin J Pharm Anal, refType=null, unstructuredReference=CHEN FYZHANG YJZHAO B,et al. GC-MS characteristic chromatogram and assay of three components for Huatuo Jiuxin pills[J]. Chin J Pharm Anal202242 (11):1917, articleTitle=GC-MS characteristic chromatogram and assay of three components for Huatuo Jiuxin pills, refAbstract=null)], funds=[Fund(id=1240704462554190528, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, awardId=GZKZ-2020-4, language=CN, fundingSource=甘肃省中医药重点科研项目(GZKZ-2020-4), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1240704453599351212, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, xref=null, ext=[AuthorCompanyExt(id=1240704453607739821, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, companyId=1240704453599351212, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Gansu Provincial Hospital of Traditional Chinese Medicine, Lanzhou 730050, China), AuthorCompanyExt(id=1240704453611934126, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, companyId=1240704453599351212, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=甘肃省中医院,兰州 730050)])], figs=[ArticleFig(id=1240704458481521236, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=EN, label=Fig.1, caption=HPLC fingerprints of 11 batches of Zilian Shengji gel samples (Sz1-Sz11) and reference fingerprint (R), figureFileSmall=8J27JlQ3YBnn4+i6XibH+Q==, figureFileBig=CJS0yVrAwSU8Lzifbat/FQ==, tableContent=null), ArticleFig(id=1240704458561213013, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=CN, label=图1, caption=11批紫连生肌凝胶剂样品的HPLC指纹图谱与对照图谱R, figureFileSmall=8J27JlQ3YBnn4+i6XibH+Q==, figureFileBig=CJS0yVrAwSU8Lzifbat/FQ==, tableContent=null), ArticleFig(id=1240704458687042139, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=EN, label=Fig.2, caption=HPLC chromatograms of test sample(A),mixed reference(B),negative reference without Coptis chinensis Franch(C),negative reference without Galla chinensis Mill. (D),negative reference without Arnebia euchroma(Royle) Johnst.(E),Coptis chinensis Franch sample(F),Galla chinensis Mill. sample(G) and Arnebia euchroma(Royle) Johnst. sample(H), figureFileSmall=3Mw5U1jleeqLROZhhsZLhg==, figureFileBig=gIXssn4t/i3fu1nX4IUdHg==, tableContent=null), ArticleFig(id=1240704458775122525, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=CN, label=图2, caption=供试品溶液(A)、混合对照品溶液(B)、不含黄连阴性样品溶液(C)、不含五倍子阴性样品溶液(D)、不含紫草阴性样品溶液(E)、黄连药材样品溶液(F)、五倍子药材样品溶液(G)和紫草药材样品溶液(H)HPLC色谱图(270、345、516 nm)

2.没食子酸(gallic acid) 16.表小檗碱(tableberberine) 18.黄连碱(coptisine) 19.巴马汀(palmatine) 20.小檗碱(berberine) 21.左旋紫草素(shikonin)

, figureFileSmall=3Mw5U1jleeqLROZhhsZLhg==, figureFileBig=gIXssn4t/i3fu1nX4IUdHg==, tableContent=null), ArticleFig(id=1240704458875785826, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=EN, label=Fig.3, caption=Cluster analysis diagram, figureFileSmall=tfE2pDQ7O4quuCmK8NSv+w==, figureFileBig=UzU30hKRrfC8UM5Tb26g8A==, tableContent=null), ArticleFig(id=1240704459022586470, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=CN, label=图3, caption=聚类分析图, figureFileSmall=tfE2pDQ7O4quuCmK8NSv+w==, figureFileBig=UzU30hKRrfC8UM5Tb26g8A==, tableContent=null), ArticleFig(id=1240704459114861163, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=EN, label=Fig.4, caption=Scree plot for PCA, figureFileSmall=qCA59xH0LmtmNydNhF4CSw==, figureFileBig=cV+7UmKgCZfGAxiYq10JFA==, tableContent=null), ArticleFig(id=1240704459211330157, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=CN, label=图4, caption=主成分分析破碎图, figureFileSmall=qCA59xH0LmtmNydNhF4CSw==, figureFileBig=cV+7UmKgCZfGAxiYq10JFA==, tableContent=null), ArticleFig(id=1240704459299410549, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=EN, label=Fig.5, caption=Score plot for OPLS-DA, figureFileSmall=82+p+Z69zfmhJQbT65ZziQ==, figureFileBig=4vWu3P/uxUki72HUWNYSwQ==, tableContent=null), ArticleFig(id=1240704459433628279, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=CN, label=图5, caption=正交偏最小二乘判别分析得分图, figureFileSmall=82+p+Z69zfmhJQbT65ZziQ==, figureFileBig=4vWu3P/uxUki72HUWNYSwQ==, tableContent=null), ArticleFig(id=1240704459567846013, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=EN, label=Fig.6, caption=VIP value for OPLS-DA, figureFileSmall=u2yVYtgqMuxcEVaA5itEbQ==, figureFileBig=T6UzKA5J6wZfoQDxqHMCpQ==, tableContent=null), ArticleFig(id=1240704459693675138, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=CN, label=图6, caption=正交偏最小二乘判别分析VIP图, figureFileSmall=u2yVYtgqMuxcEVaA5itEbQ==, figureFileBig=T6UzKA5J6wZfoQDxqHMCpQ==, tableContent=null), ArticleFig(id=1240704459777561221, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=EN, label=Tab.1, caption=

Information of 11 batches of Zilian Shengji gel samples

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample No.)
批号(lot No.)
黄连
(Coptidis Rhizoma)
紫草
(Arnebiae Radix)
白及
(Bletillae Rhizoma)
五倍子
(Galla Chinensis)
Sz1210702210602201001210101
Sz2210702202110012006037220101
Sz322060222060221050141222001
Sz4210821JZ21030282006037220101
Sz5JZ210502220070120050441222001
Sz6220101210602200701191102
Sz722030119030121050141222001
Sz82207032018070120210901210101
Sz9191007200601210501200901
Sz10201102202203012006037210101
Sz1122061720170901211101CP059191102
), ArticleFig(id=1240704459865641609, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=CN, label=表1, caption=

11批紫连生肌凝胶剂样品信息

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample No.)
批号(lot No.)
黄连
(Coptidis Rhizoma)
紫草
(Arnebiae Radix)
白及
(Bletillae Rhizoma)
五倍子
(Galla Chinensis)
Sz1210702210602201001210101
Sz2210702202110012006037220101
Sz322060222060221050141222001
Sz4210821JZ21030282006037220101
Sz5JZ210502220070120050441222001
Sz6220101210602200701191102
Sz722030119030121050141222001
Sz82207032018070120210901210101
Sz9191007200601210501200901
Sz10201102202203012006037210101
Sz1122061720170901211101CP059191102
), ArticleFig(id=1240704459983082127, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=EN, label=Tab.2, caption=

Similarities of 11 batches of zilian shengji gel samples

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample No.)
相关系数(correlation coefficient)
Sz1Sz2Sz3Sz4Sz5Sz6Sz7Sz8Sz9Sz10Sz11
Sz110.7770.8950.8250.8940.9100.9690.9190.9170.9160.917
Sz20.77710.9640.9850.9730.9500.6450.9420.9410.9450.945
Sz30.8950.96410.9870.9880.9890.8020.9890.9870.9880.989
Sz40.8250.9850.98710.9750.9750.7130.9710.9710.9720.972
Sz50.8940.9730.9880.97510.9840.7860.9810.9790.9820.983
Sz60.9100.9500.9890.9750.98410.8100.9990.9990.9990.999
Sz70.9690.6450.8020.7130.7860.81010.8270.8230.8200.823
Sz80.9190.9420.9890.9710.9810.9990.82710.9990.9990.999
Sz90.9170.9410.9870.9710.9790.9990.8230.99910.9990.999
Sz100.9160.9450.9880.9720.9820.9990.8200.9990.99910.999
Sz110.9170.9450.9890.9720.9830.9990.8230.9990.9990.9991
R0.9200.9550.9950.9780.9910.9970.8280.9970.9960.9970.997
), ArticleFig(id=1240704460058579602, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=CN, label=表2, caption=

11批紫连生肌凝胶剂样品相似度

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample No.)
相关系数(correlation coefficient)
Sz1Sz2Sz3Sz4Sz5Sz6Sz7Sz8Sz9Sz10Sz11
Sz110.7770.8950.8250.8940.9100.9690.9190.9170.9160.917
Sz20.77710.9640.9850.9730.9500.6450.9420.9410.9450.945
Sz30.8950.96410.9870.9880.9890.8020.9890.9870.9880.989
Sz40.8250.9850.98710.9750.9750.7130.9710.9710.9720.972
Sz50.8940.9730.9880.97510.9840.7860.9810.9790.9820.983
Sz60.9100.9500.9890.9750.98410.8100.9990.9990.9990.999
Sz70.9690.6450.8020.7130.7860.81010.8270.8230.8200.823
Sz80.9190.9420.9890.9710.9810.9990.82710.9990.9990.999
Sz90.9170.9410.9870.9710.9790.9990.8230.99910.9990.999
Sz100.9160.9450.9880.9720.9820.9990.8200.9990.99910.999
Sz110.9170.9450.9890.9720.9830.9990.8230.9990.9990.9991
R0.9200.9550.9950.9780.9910.9970.8280.9970.9960.9970.997
), ArticleFig(id=1240704460129882773, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=EN, label=Tab.3, caption=

Characteristic and cumulative variance contribution rate

, figureFileSmall=null, figureFileBig=null, tableContent=
主成分
(principal component)
特征值
(characteristic value)
方差贡献率
(variance contribution)/%
累积方差贡献率
(cumulative contribution rate)/%
112.33647.44647.446
24.43217.04864.494
33.50513.48277.976
41.8527.12385.100
51.2044.63089.730
61.0984.22193.952
), ArticleFig(id=1240704460209574554, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=CN, label=表3, caption=

特征值和累积方差贡献率

, figureFileSmall=null, figureFileBig=null, tableContent=
主成分
(principal component)
特征值
(characteristic value)
方差贡献率
(variance contribution)/%
累积方差贡献率
(cumulative contribution rate)/%
112.33647.44647.446
24.43217.04864.494
33.50513.48277.976
41.8527.12385.100
51.2044.63089.730
61.0984.22193.952
), ArticleFig(id=1240704460293460639, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=EN, label=Tab.4, caption=

Component matrix

, figureFileSmall=null, figureFileBig=null, tableContent=
共有峰号
(common peak No.)
矩阵(matrix)
PC1PC2PC3PC4PC5PC6
10.6040.062-0.521-0.1720.0790.453
20.2890.6530.525-0.4330.039-0.053
30.815-0.271-0.444-0.0960.170-0.080
40.7940.1740.363-0.2870.0060.094
50.8170.2530.319-0.2160.0430.077
60.651-0.069-0.373-0.297-0.1240.549
70.764-0.0480.3260.458-0.0370.111
80.810-0.189-0.4680.0750.184-0.178
90.881-0.092-0.326-0.0410.110-0.207
100.852-0.166-0.4150.0130.176-0.183
11-0.0420.4310.517-0.4650.5130.087
120.9620.1220.144-0.015-0.0320.164
130.892-0.216-0.360-0.0040.062-0.071
140.921-0.156-0.272-0.138-0.0460.040
150.8730.0250.1640.1840.069-0.031
160.882-0.0830.2170.263-0.0650.053
170.7560.1000.4750.272-0.063-0.225
180.744-0.2120.4850.093-0.2540.211
190.826-0.0770.3600.065-0.011-0.308
200.752-0.3230.494-0.137-0.233-0.061
210.1860.825-0.3270.290-0.220-0.015
220.0990.850-0.3090.165-0.3790.006
23-0.203-0.0160.3010.6140.5830.338
240.1280.828-0.0100.243-0.1170.166
250.1930.808-0.181-0.3260.100-0.247
260.3710.755-0.2430.3040.338-0.071
), ArticleFig(id=1240704460410901157, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=CN, label=表4, caption=

各成分初始因子载荷矩阵

, figureFileSmall=null, figureFileBig=null, tableContent=
共有峰号
(common peak No.)
矩阵(matrix)
PC1PC2PC3PC4PC5PC6
10.6040.062-0.521-0.1720.0790.453
20.2890.6530.525-0.4330.039-0.053
30.815-0.271-0.444-0.0960.170-0.080
40.7940.1740.363-0.2870.0060.094
50.8170.2530.319-0.2160.0430.077
60.651-0.069-0.373-0.297-0.1240.549
70.764-0.0480.3260.458-0.0370.111
80.810-0.189-0.4680.0750.184-0.178
90.881-0.092-0.326-0.0410.110-0.207
100.852-0.166-0.4150.0130.176-0.183
11-0.0420.4310.517-0.4650.5130.087
120.9620.1220.144-0.015-0.0320.164
130.892-0.216-0.360-0.0040.062-0.071
140.921-0.156-0.272-0.138-0.0460.040
150.8730.0250.1640.1840.069-0.031
160.882-0.0830.2170.263-0.0650.053
170.7560.1000.4750.272-0.063-0.225
180.744-0.2120.4850.093-0.2540.211
190.826-0.0770.3600.065-0.011-0.308
200.752-0.3230.494-0.137-0.233-0.061
210.1860.825-0.3270.290-0.220-0.015
220.0990.850-0.3090.165-0.3790.006
23-0.203-0.0160.3010.6140.5830.338
240.1280.828-0.0100.243-0.1170.166
250.1930.808-0.181-0.3260.100-0.247
260.3710.755-0.2430.3040.338-0.071
), ArticleFig(id=1240704460498981546, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=EN, label=Tab.5, caption=

Principal component score and comprehensive score

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample No.)
得分(score)综合得分
(comprehensive score)
PC1PC2PC3PC4PC5PC6
Sz1-0.606-0.877-0.214-0.412-0.262-0.317-0.554
Sz2-1.6211.163-1.0770.372-1.659-0.292-0.829
Sz31.116-0.0061.7720.122-1.594-0.1190.742
Sz40.610-0.225-1.488-0.464-0.0361.6790.092
Sz50.435-0.761-0.152-1.8840.3500.275-0.053
Sz60.595-0.8480.2860.674-0.307-0.7450.190
Sz7-0.029-1.467-0.5861.185-0.080-0.115-0.284
Sz80.9681.9160.193-0.4130.0280.4610.855
Sz9-1.0520.1641.2581.2001.2041.696-0.095
Sz10-1.3720.1250.832-1.2800.874-1.079-0.653
Sz110.9560.816-0.8250.8991.483-1.4430.589
), ArticleFig(id=1240704460603839148, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=CN, label=表5, caption=

主成分得分和综合得分

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample No.)
得分(score)综合得分
(comprehensive score)
PC1PC2PC3PC4PC5PC6
Sz1-0.606-0.877-0.214-0.412-0.262-0.317-0.554
Sz2-1.6211.163-1.0770.372-1.659-0.292-0.829
Sz31.116-0.0061.7720.122-1.594-0.1190.742
Sz40.610-0.225-1.488-0.464-0.0361.6790.092
Sz50.435-0.761-0.152-1.8840.3500.275-0.053
Sz60.595-0.8480.2860.674-0.307-0.7450.190
Sz7-0.029-1.467-0.5861.185-0.080-0.115-0.284
Sz80.9681.9160.193-0.4130.0280.4610.855
Sz9-1.0520.1641.2581.2001.2041.696-0.095
Sz10-1.3720.1250.832-1.2800.874-1.079-0.653
Sz110.9560.816-0.8250.8991.483-1.4430.589
), ArticleFig(id=1240704460708696756, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=EN, label=Tab.6, caption=

Linear relationships of various components

, figureFileSmall=null, figureFileBig=null, tableContent=
成分(component)回归方程(regression equation)r线性范围(linear range)/(μg·mL-1
没食子酸(gallic acid)Y=5.223×104X-3.216×1050.999 50.328 8~1.972 8
表小檗碱(tableberberine)Y=7.234×104X-9.211×1040.999 90.051 2~0.307 2
黄连碱(coptisine)Y=3.354×104X-8.801×1040.999 90.112 8~0.676 8
巴马汀(palmatine)Y=6.099×104X-2.186×1050.999 80.186 4~1.118 4
小檗碱(berberine)Y=6.322×104X-1.000×1060.999 80.627 2~3.763 2
左旋紫草素(shikonin)Y=2.487×104X-1.481×1040.999 90.025 2~0.151 2
), ArticleFig(id=1240704462201868982, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=CN, label=表6, caption=

各成分线性关系

, figureFileSmall=null, figureFileBig=null, tableContent=
成分(component)回归方程(regression equation)r线性范围(linear range)/(μg·mL-1
没食子酸(gallic acid)Y=5.223×104X-3.216×1050.999 50.328 8~1.972 8
表小檗碱(tableberberine)Y=7.234×104X-9.211×1040.999 90.051 2~0.307 2
黄连碱(coptisine)Y=3.354×104X-8.801×1040.999 90.112 8~0.676 8
巴马汀(palmatine)Y=6.099×104X-2.186×1050.999 80.186 4~1.118 4
小檗碱(berberine)Y=6.322×104X-1.000×1060.999 80.627 2~3.763 2
左旋紫草素(shikonin)Y=2.487×104X-1.481×1040.999 90.025 2~0.151 2
), ArticleFig(id=1240704462285755066, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=EN, label=Tab.7, caption=

Results of content determination of six quantitative components of 11 batches of Zilian Shengji gel samples

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample No.)
含量(content)/(μg·g-1
没食子酸
(gallic acid)
表小檗碱
(tableberberine)
黄连碱
(coptisine)
小檗碱
(berberine)
巴马汀
(palmatine)
左旋紫草素
(shikonin)
Sz11 112.87178.05476.962 854.52754.6587.29
Sz21 113.23137.52381.832 023.81524.15549.46
Sz31 452.17296.05884.734 051.66986.13288.70
Sz41 080.27244.89572.982 796.09736.04316.83
Sz51 281.95190.72679.483 393.53712.4461.36
Sz61 065.64237.40725.433 563.18842.29154.35
Sz7827.74230.01646.822 978.81746.9564.08
Sz81 513.50232.16682.773 135.61817.98465.03
Sz91 196.11192.09594.962 565.54636.00190.84
Sz101 328.21165.86404.592 599.77713.3847.65
Sz111 261.31248.15512.052 754.77883.02498.38
), ArticleFig(id=1240704462373835452, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688794056323983, language=CN, label=表7, caption=

11批紫连生肌凝胶剂样品中6个定量成分的含量测定结果

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample No.)
含量(content)/(μg·g-1
没食子酸
(gallic acid)
表小檗碱
(tableberberine)
黄连碱
(coptisine)
小檗碱
(berberine)
巴马汀
(palmatine)
左旋紫草素
(shikonin)
Sz11 112.87178.05476.962 854.52754.6587.29
Sz21 113.23137.52381.832 023.81524.15549.46
Sz31 452.17296.05884.734 051.66986.13288.70
Sz41 080.27244.89572.982 796.09736.04316.83
Sz51 281.95190.72679.483 393.53712.4461.36
Sz61 065.64237.40725.433 563.18842.29154.35
Sz7827.74230.01646.822 978.81746.9564.08
Sz81 513.50232.16682.773 135.61817.98465.03
Sz91 196.11192.09594.962 565.54636.00190.84
Sz101 328.21165.86404.592 599.77713.3847.65
Sz111 261.31248.15512.052 754.77883.02498.38
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紫连生肌凝胶剂HPLC指纹图谱建立及6个成分含量测定
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闫治攀 , 李喜香 ** , 高丽霞
药物分析杂志 | 标准研讨 2024,44(9): 1586-1596
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药物分析杂志 | 标准研讨 2024, 44(9): 1586-1596
紫连生肌凝胶剂HPLC指纹图谱建立及6个成分含量测定
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闫治攀 , 李喜香** , 高丽霞
作者信息
  • 甘肃省中医院,兰州 730050
  • Tel: 18193140379; E-mail:

通讯作者:

** Tel: 15002550389; E-mail:
Establishment of HPLC fingerprints and determination of six components for Zilian Shengji gel
Zhi-pan YAN , Xi-xiang LI** , Li-xia GAO
Affiliations
  • Gansu Provincial Hospital of Traditional Chinese Medicine, Lanzhou 730050, China
出版时间: 2024-09-30 doi: 10.16155/j.0254-1793.2023-0543
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目的:建立紫连生肌凝胶剂指纹图谱,并测定没食子酸、表小檗碱、黄连碱、巴马汀、小檗碱和左旋紫草素的含量。方法:采用Agilent C18-WR(250 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-0.15%磷酸水,梯度洗脱,流速0.8 mL·min-1,柱温25 ℃,检测波长270、345、516 nm,结合聚类分析、主成分分析和正交偏最小二乘法判别分析对紫连生肌凝胶剂的指纹图谱进行化学模式识别,并对指定的6个成分进行定量分析。结果:建立了紫连生肌凝胶剂指纹图谱,共标定26个共有峰,与对照指纹图谱的相似度为0.828~0.997;指认出没食子酸、表小檗碱、黄连碱、小檗碱、巴马汀和左旋紫草素6个色谱峰。6个成分在各自范围内线性关系良好(r≥0.999 5),平均加样回收率在98.7%~99.3%,RSD 在1.3%~1.8%。11批样品中6个成分含量分别为827.74~1 513.50 μg·g-1、137.52~296.05 μg·g-1、381.83~884.73 μg·g-1、2 023.81~4 051.66 μg·g-1、524.15~986.13 μg·g-1和47.65~549.46 μg·g-1结论:该方法简便,稳定可靠,重复性好,可用于紫连生肌凝胶剂的质量控制。

紫连生肌凝胶剂  /  没食子酸  /  表小檗碱  /  黄连碱  /  巴马汀  /  小檗碱  /  左旋紫草素  /  含量测定  /  质量评价  /  高效液相色谱指纹图谱

Objective: To establish the HPLC fingerprints for Zilian Shengji gel and to determine the contents of gallic acid, tableberberine, coptisine, palmatine, berberine and shikonin. Methods: The establishment of fingerprints was performed on a 25 ℃ thermostatic Agilent C18-WR(250 mm×4.6 mm, 5 μm)column with the mobile phase comprising of acetonitrile -0.15% phosphoric acid water at the flowing rate of 0.8mL·min-1 in a gradient elution manner, and the detection wavelength were set at 270 nm, 345 nm and 516 nm. Cluster analysis, principal component analysis(PCA) and orthogonal partial least squares discriminant analysis(OPLS-DA) were adopted in chemical pattern recognition. The six components identified were quantitatively determined. Results: The HPLC fingerprint of Zilian Shengji gel was constructed with twenty-six common chromatographic peaks, eleven batches of samples with the similarities of 0.828-0.997, six chromatographic peaks of gallic acid, tableberberine, coptisine, palmatine, berberine and shikonin were identified by reference substance comparison. Six constituents showed good linear relationships within their own ranges (r≥0.999 5) whose average recoveries were 98.7%-99.3%, with the RSDs of 1.3%-1.8%. The content ranges of the above mentioned six components in eleven batches of samples were 827.74-1 513.50 μg·g-1, 137.52-296.05 μg·g-1, 381.83-884.73 μg·g-1, 2 023.81-4 051.66 μg·g-1, 524.15-986.13 μg·g-1 and 47.65-549.46 μg·g-1. Conclusion: This simple, stable, reliable and reproducible method can be used for the quality control of Zilian Shengji gel.

Zilian Shengji gel  /  gallic acid  /  tableberberine  /  coptisine  /  palmatine  /  berberine  /  shikonin  /  contents determination  /  quality evaluation  /  HPLC fingerprints
闫治攀, 李喜香, 高丽霞. 紫连生肌凝胶剂HPLC指纹图谱建立及6个成分含量测定. 药物分析杂志, 2024 , 44 (9) : 1586 -1596 . DOI: 10.16155/j.0254-1793.2023-0543
Zhi-pan YAN, Xi-xiang LI, Li-xia GAO. Establishment of HPLC fingerprints and determination of six components for Zilian Shengji gel[J]. Chinese Journal of Pharmaceutical Analysis, 2024 , 44 (9) : 1586 -1596 . DOI: 10.16155/j.0254-1793.2023-0543
紫连生肌凝胶剂为甘肃省中医院院内制剂玉红油纱条(甘药制字Z04000845)二次开发产品,处方由黄连、白及、五倍子和紫草组成,广泛用于临床外科急慢性创面,疗效显著。前期,课题组对其制备工艺进行了系统研究,并制定了稳定可行的制备工艺规程[1],但基于医院院内制剂检验成本和质量检验方法简单易行,造成了其质量标准简单落后,只对处方中的黄连进行了薄层鉴别,不能满足现代中药复方制剂的质量检验需求,本实验建立紫连生肌凝胶剂HPLC指纹图谱,并同时测定没食子酸、表小檗碱、黄连碱、巴马汀和左旋紫草素的含量,再采用聚类分析和主成分分析对指纹图谱数据信息进行挖掘[2],快速筛选质量差异成分,以期为该制剂批次间稳定性和质量评价研究提供参考。
2478高效液相色谱仪(Waters公司);SQP型十万分之一电子天平(赛多利斯科学仪器公司);FA1004十万分之一电子天平(上海良平仪器仪表有限公司);溶剂过滤器(津腾服务有限公司);HH-7型恒温水浴锅(常州国华电器有限公司);KQ-300DB型超声波清洗器(昆山市超声仪器有限公司);Labonce-9240A型电热恒温鼓风干燥箱(北京兰贝恒温技术股份有限公司);PDV旋转粘度计(上海尼润智能科技有限公司);PHS-3CpH计(杭州奥立龙仪器有限公司);RE-3000旋转蒸发仪(上海亚荣生化仪器厂)。
对照品没食子酸(批号110831-201906,纯度99.76%)、黄连碱(批号112026-201802,纯度98.9%)、小檗碱(批号110713-201814,纯度99%)、巴马汀(批号110732-201913,纯度99%)、左旋紫草素(批号110713-201814,纯度99%)均购自中国食品药品检定研究院;表小檗碱(批号D20108,纯度98%)购自源叶生物技术有限公司;泊洛沙姆407、泊洛沙姆188、聚乙二醇6000均购自湖北兴银河化工有限公司;卡波姆购自山东萍聚生物科技有限公司;乙腈、甲醇、磷酸均为色谱纯,均购自天津大茂化学试剂有限公司;盐酸分析纯,购自国药集团化学试剂有限公司;水为超纯水。黄连 (批号191007、201102、210702、210821、220101、220301、220602、220617、220703、JZ2105022、210702,产地四川)、紫草(批号190301、200601、200701、20170901、20180701、20211001、20220301、210602、JZ2103028、220602,产地新疆)、白及(批号 200504、2006037、210501、200701、201001、20210901、211101CP059,产地云南)和五倍子(批号191102、210101、220101、41222001、200901,产地四川),均由甘肃省中医院提供,饮片经甘肃省药品检定研究院宋平顺主任药师鉴定,均符合2020年版《中华人民共和国药典》有关规定。
每味中药饮片按照处方配比(黄连、紫草、白及、五倍子)称取11份全方(从现有的4味药材批次中随机组合成11份,组合详见表1),处方以90%乙醇温浸提取2次,溶媒用量分别为11倍和9倍,2次均提取45 min,提取温度设为60 ℃,合并2次提取液,回收乙醇至无醇味,浓缩至浓度为0.5 g·mL-1[3]。按制剂处方比例称取泊洛沙姆407、泊洛沙姆188、聚乙二醇6000和去离子水,将泊洛沙姆407、泊洛沙姆188和聚乙二醇6000置于烧杯中,加入去离子水,-4 ℃溶胀24 h[4],取处方量的浓缩药液加入到溶胀好的空白凝胶中,摇匀,脱气制成紫连生肌凝胶剂(序号Sz1~Sz11)。
称取紫连生肌凝胶剂5 g,加入20%氯化钠溶液20 mL,精密称定,超声(功率300 W,频率40 kHz)提取30 min,拭干锥形瓶表面水分,放冷后用20%氯化钠溶液补足减失的量,滤过,取续滤液10 mL,水浴蒸干,残渣用90%甲醇-盐酸(100∶2)溶解并定容至25 mL,0.22 μm微孔滤膜滤过,即得。
分别取五倍子、紫草和黄连药材各1.0 g,按“2.1.2”项下方法制备各药材供试品溶液。
精密称定对照品没食子酸、表小檗碱、黄连碱、巴马汀、小檗碱和左旋紫草素适量,分别置于5 mL量瓶中,加甲醇溶解并定容至刻度,制成质量浓度分别为1.644、0.256、0.564、0.932、3.136和0.126 mg·mL-1的对照品溶液,分别精密取上述对照品溶液各0.5mL,置于10mL量瓶中,加甲醇定容至刻度,制成浓度为82.20、12.80、28.20、46.60、156.80和6.30 mg·mL-1的混合对照品溶液。
依据处方量称饮片,按“2.1.1”项下方法制备不含黄连、不含紫草、不含五倍子、不含白及的阴性样品制剂,按“2.1.2”项下方法制备各阴性样品溶液。
采用Agilent C18-WR色谱柱(250 mm×4.6 mm,5 μm)色谱柱,以乙腈为流动相A,以0.15%磷酸水为流动相B,梯度洗脱(0~10 min,5% A→12% A;10~48 min,12% A→20% A;48~60 min,20% A→21% A;60~70 min,21% A→34% A;70~85 min,34% A→80% A;85~100 min,80% A→95% A)[5],流速0.8 mL·min-1,进样体积10μL,柱温25 ℃,检测波长270 nm(0~48 min)、345 nm(48~85 min)、516 nm(85~100 min),采集时长100 min。
按“2.1.2”项下方法制备供试品溶液(Sz1),在“2.2.1”项色谱条件下连续测定6次,以19号峰为参照峰,计算各共有色谱峰相对保留时间和相对峰面积的RSD,均不大于0.87%和4.7%,表明仪器精密度良好。
按“2.1.2”项下制备供试品溶液(Sz1)6份,按照“2.2.1”项下色谱条件依次进样,以19号峰为参照峰,计算各共有色谱峰相对保留时间和相对峰面积的RSD,均不大于0.89%和4.6%,表明方法重复性良好。
按“2.1.2”项下制备供试品溶液(Sz1),按照“2.2.1”项下色谱条件分别在0、2、4、8、12、24、48、72 h进样,以19号峰为参照峰,计算各共有色谱峰相对保留时间和相对峰面积的RSD,均不大于0.64%和4.8%,说明样品在72 h内稳定。
将得到的11批紫连生肌凝胶剂色谱图导入“中药色谱指纹图谱相似度评价系统(2012 版)”,对紫连生肌凝胶剂样品色谱图基线分析,以时间宽度为0.1,采用中位数法、多点校正、Mark峰匹配生成11批样品图谱(Sz1~Sz11)和对照指纹图谱(R),共标定26个共有峰[7-8],结果见图1,11批样品与对照指纹图谱的相似度见表2
取“2.1.3”项下各药材供试品溶液、“2.1.4”项下对照品溶液和“2.1.5”项下阴性样品溶液适量,在“2.2.1”项色谱条件下进样测定,其中15、16、17、18、19和20号峰归属于黄连,1、2、3、4、5、8、9、10、11、12、13和14号峰归属于五倍子,21、22、23、24、25和26号峰归属于紫草;共指认出6个化合物,分别为没食子酸(2号峰)、表小檗碱(16号峰)、黄连碱(18号峰)、巴马汀(19号峰)、小檗碱(20号峰)和左旋紫草素(21号峰),结果见图2
将11批样品共有峰峰面积导入SPSS 20.0软件,对11批紫连生肌凝胶剂指纹图谱进行聚类,如图3所示,当分类距离为5时,11批样品可以分为4大类,Sz1、Sz3、Sz6、Sz7为一类,Sz4、Sz5、Sz8、Sz11为一类,Sz9、Sz10为一类,Sz2为一类;当分类距离大于10时,11批样品可以分为两大类,Sz2、Sz9、Sz10,其余样品归为一大类,说明紫连生肌凝胶剂各批次间质量存在差异,这主要是由于饮片批次间质量差异造成的。
利用 SPSS 20.0软件,对11批紫连生肌凝胶剂的26个共有峰进行主成分分析,破碎图见图4。以主成分特征值>1为标准,提取出6个主成分,第一主成分的特征值为12.336,方差累积贡献率为47.446%;第二主成分的特征值为4.432,方差累积贡献率为64.494%;第三主成分的特征值为3.505,方差累积贡献率为77.976%;第四主成分的特征值为1.852,方差累积贡献率为85.100%;第五主成分的特征值为1.204,方差累积贡献率为89.730%;第六主成分的特征值为1.098,方差累积贡献率为93.952%。较全面地表征紫连生肌凝胶剂样品化学成分特征,故选择对该6个主成分进行分析,特征值和方差贡献率见表3
根据主成分载荷矩阵结果可知,影响紫连生肌凝胶剂样品批次间质量差异的是多成分联合作用的结果,见表4。共有峰1、3、4、5、6、7、8、9、10、12、13、14、15、16、17、18、19、20在第一主成分上有较高载荷;共有峰2、21、22、24、25、26在第二主成分上有较高载荷;共有峰2、11、17、18、20在第三主成分上有较高载荷;共有峰7、16、17、21、22、23、24、26在第四主成分上有较高载荷;共有峰11、23、26在第五主成分上有较高载荷;共有峰1、6、23在第六主成分上有较高载荷;其中第一主成分、第三主成分主要反映处方中五倍子和黄连的化学成分信息,第二、五、六主成分主要反映处方中紫草和五倍子的化学成分信息,第四主成分主要反映处方中紫草和黄连的化学成分信息。
根据主成分得分计算综合得分,综合得分越高紫连生肌凝胶剂的质量越好,综合得分以主成分的贡献率对主成分得分进行加权平均,即主成分总和得分=(主成分1得分×47.446+主成分2得分×17.048+主成分3得分×13.482+主成分4得分×7.123+主成分5得分×4.630+主成分6得分×4.221)/93.952。结果见表5。结果表明,11批紫连生肌凝胶剂样品质量存在差异,其中Sz8、Sz3、Sz11、Sz6和Sz4样品质量较好。
为了进一步找出影响批次间质量差异的成分,采用SIMCA14.1软件进行有监督模式的OPLS-DA分析,散点得分图见图5,由图可知11批样品可分为4类,与聚类分析结果基本一致。再采用变量重要性投影值(VIP值)筛选差异成分,以VIP值>1为条件共筛选出6个成分,见图6,按数值大小排序依次为11号峰(未知)、22号峰(未知)、21号峰(左旋紫草素)、25号峰(未知)、20号峰(小檗碱)、18号峰(黄连碱),均为引起样品批次间质量差异的主要成分。
同“2.1”项下方法。
同“2.2.1”项下方法。
精密吸取对照品溶液、供试品溶液、阴性样品溶液和药材样品溶液各10μL,按“2.2.1”条件进样测定,结果供试品色谱图中有与对照品色谱图同样对应的色谱峰,而阴性样品溶液相应位置无该峰,说明本品中其他成分对含量测定的几个成分无干扰,本方法专属性强,详见图2
分别精密吸取40、80、120、160、180、200、240 μL混合对照品溶液,置于10 mL量瓶中,加甲醇定容至刻度,配制成不同浓度梯度的混合对照品溶液,按“2.2.1”项下色谱条件进样测定,记录每个成分不同进样量的峰面积,以混合对照品溶液的质量浓度X为横坐标,以峰面积Y为纵坐标,进行线性回归,回归方程见表6
取上述混合对照品溶液按“2.3.2”项下色谱条件连续进样6次,记录每个成分的峰面积,得出没食子酸、表小檗碱、黄连碱、小檗碱、巴马汀和左旋紫草素峰面积的RSD分别为1.7%、1.5%、1.8%、1.5%、1.3%、1.5%,表明仪器精密度良好。
取同一样品,按“2.1.2”项下方法平行制备6份供试品溶液,按“2.3.2”项下色谱条件测定,记录每个成分的峰面积,得出没食子酸、表小檗碱、黄连碱、小檗碱、巴马汀和左旋紫草素的平均含量分别为1 253.82、248.27、511.87、2 766.08、888.48、496.48 μg·g-1,RSD分别为1.7%、1.8%、1.6%、1.4%、1.2%、1.5%,表明该方法重复性良好。
取供试品溶液,分别于0、4、8、12、24、48、72 h按“2.2.1”项下色谱条件下测定,记录每个成分的峰面积,得出没食子酸、表小檗碱、黄连碱、小檗碱、巴马汀和左旋紫草素的峰面积的RSD分别为1.7%、1.9%、1.6%、1.4%、1.7%、1.4%,表明供试品溶液在72 h内稳定。
取已知含量的样品,称取9份,加入20%氯化钠溶液20 mL,超声提取30 min,滤过,滤液水浴蒸干,即得供试品残渣;另取没食子酸、表小檗碱、黄连碱、小檗碱、巴马汀和左旋紫草素对照品适量,加甲醇制得质量浓度分别为0.502、0.472、0.509、0.494、0.473、0.513 mg·mL-1的对照品溶液,分别按照含量50%、100%和150%的比例用移液枪吸取1.2、2.4、3.6 mL没食子酸对照品溶液,230、460、690 μL表小檗碱对照品溶液,0.6、1.2、1.8 mL黄连碱对照品溶液,3.0、6.0和9.0 mL小檗碱对照品溶液,0.8、1.6、2.4 mL巴马汀对照品溶液,240、480、720 μL左旋紫草素对照品溶液,分别加入到供试品残渣中溶解,并用90%甲醇-盐酸(100∶2)定容至25 mL,最后用0.22 μm微孔滤膜滤过,即得加样回收试验供试品溶液。按“2.2.1”项下色谱条件下测定,计算得没食子酸、表小檗碱、黄连碱、、巴马汀、小檗碱和左旋紫草素的平均加样回收率分别为98.7%、99.3%、99.2%、98.7%、98.7%、98.7%,RSD分别为1.3%、1.8%、1.3%、1.3%、1.8%、1.7%。
取11批样品,按“2.1.2”项下方法制备供试品溶液,按“2.3.2”项下色谱条件下测定,计算样品中6个成分的含量,结果见表7
紫连生肌凝胶剂处方由黄连、五倍子、紫草和白及组成,为复方制剂,且各位药材化学成分理化性质差异较大,在对比其他色谱柱,发现使用Agilent C18-WR色谱柱(250 mm×4.6 mm,5 μm)分离效果、峰型、基线平稳的均较好;流动相分别考察比较了甲醇-水系统、甲醇-0.1%甲酸水系统、甲醇-0.15%磷酸水系统、乙腈-水系统、乙腈-0.1%甲酸水系统和乙腈-0.15%磷酸水系统,发现乙腈-0.15%磷酸水系统的色谱峰信号丰富,同时各峰之间的分离度较好,故选择乙腈-0.15%磷酸水系统进行梯度洗脱;在190~400 nm范围内通过全波长扫描发现在270、345、516 nm 3个波长同时检测的条件下能够全面的检测出处方的色谱峰,同时基线的噪音低和各峰之间的分离度较好,因此选择270、345、516 nm进行多波长检测。
紫连生肌凝胶剂经处方化学成分分析,主要含有有机酸、生物碱和萘醌衍生物等成分,极性及溶解度差异较大,前期为提高处方中生物碱等有效成分的溶解性,先用20%氯化钠溶液进行超声提取,再分别考察甲醇、甲醇-水系统、甲醇-甲酸系统和甲醇-盐酸系统对其成分的提取效果,结果发现90%甲醇-盐酸(100∶2)系统对处方中成分的提取范围广,能够较为全面地反映出处方的化学成分,因此选用90%甲醇-盐酸(100∶2)作为供试品溶液制备的溶媒。
19号峰巴马汀为处方中黄连的指标性成分,出峰时间为70.22 min。各批次样品色谱图显示,19号峰的出峰时间比较稳定,峰面积适中,与相邻峰之间的分离度较好,峰型好,故选择19号峰作为参照峰。
按照中药处方组成原则,对君臣药黄连、紫草和五倍子的共有峰进行了确认,结果显示共有峰个数(24个)占总共有峰的92.31%,足以定性表征紫连生肌凝胶剂质量。其中关于峰6、峰7的归属,有可能是白及(佐药)的成分,也有可能是处方产生的新成分,有待在后续研究中进一步确认。
医院中药制剂多为复方制剂,其化学成分复杂,质量控制较为单一,难以符合现代中药制剂的质量控制需求,成为制约其发展的主要因素之一[17-19]。因此本实验从定性结合定量的模式采用HPLC指纹图谱对紫连生肌凝胶剂进行定性表征和对没食子酸等多指标定量测定对其质量进行全面的控制。
实验结果表明,11批样品HPLC指纹图谱的相似度在0.828~0.997,虽在一定程度上表征产品质量的一致性,但也说明产品批次间存在差异,经过全过程分析,初步判断为不同批次原料药材质量差异所致;通过聚类分析和主成分分析2种化学模式识别技术进行综合分析:11批样品可以分为三大类,并筛选出了6个主要成分;通过化学对照品对比鉴定出6个成分,分别为没食子酸、表小檗碱、黄连碱、巴马汀、小檗碱和左旋紫草素,并对其进行了含量的测定。
本实验采用同一的色谱条件实现了紫连生肌凝胶剂指纹图谱定性和6个成分定量分析,再采用化学模式分析筛选出不同批次样品之间的差异成分,经方法学考察,所建立的方法专属性强,重复性好,准确可靠,可用于该制剂的质量评价。
  • 甘肃省中医药重点科研项目(GZKZ-2020-4)
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2024年第44卷第9期
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doi: 10.16155/j.0254-1793.2023-0543
  • 首发时间:2026-03-17
  • 出版时间:2024-09-30
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  • 修回日期:2024-06-12
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甘肃省中医药重点科研项目(GZKZ-2020-4)
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    甘肃省中医院,兰州 730050

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2种不同金属材料的力学参数

Family
属数
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genus
种数
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species
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Percentage of
total species (%)

Genus
种数
Number of
species
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Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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