Article(id=1206272762407092819, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1206272755658453329, articleNumber=null, orderNo=null, doi=10.16155/j.0254-1793.2024-1361, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1734883200000, receivedDateStr=2024-12-23, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1765527438021, onlineDateStr=2025-12-12, pubDate=null, pubDateStr=null, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1765527438021, onlineIssueDateStr=2025-12-12, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1765527438021, creator=13701087609, updateTime=1765527438021, updator=13701087609, issue=Issue{id=1206272755658453329, tenantId=1146029695717560320, journalId=1205117023404326918, year='2025', volume='45', issue='5', pageStart='739', pageEnd='920', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=0, createTime=1765527436411, creator=13701087609, updateTime=1765531454840, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1206289610234196753, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1206272755658453329, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1206289610234196754, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1206272755658453329, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=796, endPage=801, ext={EN=ArticleExt(id=1206272762671333989, articleId=1206272762407092819, tenantId=1146029695717560320, journalId=1205117023404326918, language=EN, title=Simultaneous determination of eleven constituents in Jinlian Quwen capsules by HPLC, columnId=1206272756333736276, journalTitle=Chinese Journal of Pharmaceutical Analysis, columnName=Ingredient Analysis, runingTitle=null, highlight=null, articleAbstract=

Objective: To establish an HPLC method for the simultaneous determination of chlorogenic acid,puerarin, 3’-methoxy puerarin, puerarin apioside, liquiritin, forsythoside A, 3,5-O-dicaffeoylquinic acid,4,5-dicaffeoylquinic acid, forsythin, honokiol and magnolol in Jinlian Quwen capsules. Methods: The analysis was performed on a Waters AtlantisTM T3 (150 mm×4.6 mm, 3 μm) column, and the mobile phase was comprised of acetonitrile-0.1% phosphoric acid, with the flow rate of 1.0 mL · min-1 in a gradient elution manner. The column temperature was set at 35 ℃. The injection volume was 4 μL and the UV detection wavelengths were set at 225 nm (detecting forsythin), 250 nm (detecting puerarin, 3’-methoxy puerarin and puerarin apioside), 276 nm(detecting liquiritin), 290 nm (detecting honokiol and magnolol) and 325 nm (detecting chlorogenic acid,3,5-O-dicaffeoylquinic acid, 4,5-dicaffeoylquinic acid and forsythoside A). Results: All the 11 constituents showed good linearity within their detection ranges (r≥0.999 5), whose average recoveries (n=6) were 100.1%-108.1%, with the RSDs of 2.8%-4.1%. The content ranges of 11 components in three batches of samples were 7.505-7.606 mg · g-1, 3.485-3.920 mg · g-1, 0.969-1.068 mg · g-1, 0.837-0.955 mg · g-1, 1.009-1.436 mg · g-1,3.037-3.602 mg · g-1, 5.259-5.371 mg · g-1, 0.931-1.012 mg · g-1, 1.428-2.053 mg · g-1, 0.939-1.018 mg · g-1 and 2.744-2.827 mg · g-1, respectively. Conclusion: The method is simple, sensitive and reliable. It can be used as a reference for the establishment of quality standard of Jinlian Quwen capsules.

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目的:建立HPLC法同时测定金连驱瘟胶囊中绿原酸、葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷、甘草苷、连翘酯苷A、异绿原酸A、异绿原酸C、连翘苷、和厚朴酚及厚朴酚11个成分的含量。方法:采用Waters AtlantisTM T3(150 mm×4.6 mm,3 μm)色谱柱,以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,体积流量1.0 mL · min-1,柱温35 ℃,进样量4 μL,检测波长为225 nm(检测连翘苷)、250 nm(检测葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷)、276 nm(检测甘草苷)、290 nm(检测和厚朴酚、厚朴酚)和325 nm(检测绿原酸、异绿原酸A、异绿原酸C、连翘酯苷A)。结果:上述11个成分在各自检测范围内线性关系良好(r均≥0.999 5),平均加样回收率(n=6)在100.1%~108.1%,RSD 在2.8%~4.1%。3批样品中各成分含量范围分别在7.505~7.606、3.485~3.920、0.969~1.068、0.837~0.955、1.009~1.436、3.037~3.602、5.259~5.371、0.931~1.012、1.428~2.053、0.939~1.018和2.744~2.827 mg · g-1结论:该方法简单、灵敏、准确、可靠,可为金连驱瘟胶囊质量标准的建立提供参考。

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1. 绿原酸(chlorogenic acid) 2. 葛根素(puerarin) 3. 3’-甲氧基葛根素(3’-methoxy puerarin) 4. 葛根素芹菜糖苷(puerarin apioside) 5. 甘草苷(liquiritin) 6. 连翘酯苷A(forsythoside A) 7. 异绿原酸A(3,5-O-dicaffeoylquinic acid) 8. 异绿原酸C(4,5-dicaffeoylquinic acid) 9. 连翘苷(forsythin) 10. 和厚朴酚(honokiol) 11. 厚朴酚(magnolol)

, figureFileSmall=289TNpqzKlgne7DXp4aaAw==, figureFileBig=WFNXnofEVbEpVyiuPpAOYw==, tableContent=null), ArticleFig(id=1206300929603732038, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272762407092819, language=EN, label=Tab. 1, caption=

The results of linearity investigation of eleven components

, figureFileSmall=null, figureFileBig=null, tableContent=
成分(component)回归方程(regression equation)r线性范围(linear range)/μg
绿原酸(chlorogenic acid)Y=2.87×106X+7.7×1030.999 60.383~2.298
葛根素(puerarin)Y=4.57×106X-3.71×1040.999 60.307~1.842
3’-甲氧基葛根素(3’-methoxy puerarin)Y=3.45×106X+3.41×1020.999 80.061~0.366
葛根素芹菜糖苷(puerarin apioside)Y=3.17×106X+1.27×1040.999 90.044~0.264
甘草苷(liquiritin)Y=1.74×106X+5.02×1030.999 50.026~0.156
连翘酯苷A(forsythoside A)Y=1.70×106X-1.33×1040.999 70.207~1.242
异绿原酸A(3,5-O-dicaffeoylquinic acid)Y=3.12×106X-7.87×1020.999 50.112~0.672
异绿原酸C(4,5-dicaffeoylquinic acid)Y=3.74×106X+1.47×1040.999 80.019~0.114
连翘苷(forsythin)Y=1.57×106X+4.51×1040.999 70.056~0.336
和厚朴酚(honokiol)Y=1.64×106X+1.28×1040.999 60.061~0.366
厚朴酚(magnolol)Y=1.48×106X-7.580×1030.999 50.171~1.026
), ArticleFig(id=1206300929729561166, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272762407092819, language=CN, label=表1, caption=

11个成分的线性关系考察结果

, figureFileSmall=null, figureFileBig=null, tableContent=
成分(component)回归方程(regression equation)r线性范围(linear range)/μg
绿原酸(chlorogenic acid)Y=2.87×106X+7.7×1030.999 60.383~2.298
葛根素(puerarin)Y=4.57×106X-3.71×1040.999 60.307~1.842
3’-甲氧基葛根素(3’-methoxy puerarin)Y=3.45×106X+3.41×1020.999 80.061~0.366
葛根素芹菜糖苷(puerarin apioside)Y=3.17×106X+1.27×1040.999 90.044~0.264
甘草苷(liquiritin)Y=1.74×106X+5.02×1030.999 50.026~0.156
连翘酯苷A(forsythoside A)Y=1.70×106X-1.33×1040.999 70.207~1.242
异绿原酸A(3,5-O-dicaffeoylquinic acid)Y=3.12×106X-7.87×1020.999 50.112~0.672
异绿原酸C(4,5-dicaffeoylquinic acid)Y=3.74×106X+1.47×1040.999 80.019~0.114
连翘苷(forsythin)Y=1.57×106X+4.51×1040.999 70.056~0.336
和厚朴酚(honokiol)Y=1.64×106X+1.28×1040.999 60.061~0.366
厚朴酚(magnolol)Y=1.48×106X-7.580×1030.999 50.171~1.026
), ArticleFig(id=1206300929817641560, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272762407092819, language=EN, label=Tab. 2, caption=

Determination results of eleven components in Jinlian Quwen capsules

, figureFileSmall=null, figureFileBig=null, tableContent=
批号
(lot No.)
含量(content)/(mg · g-1n=3)
绿原酸
(chlorogenic acid)
葛根素
(puerarin)
3’-甲氧基
葛根素
(3’-methoxy puerarin)
葛根素芹
菜糖苷
(puerarin apioside)
甘草苷
(liquiritin)
连翘酯苷A
(forsythoside A)
异绿原酸A
(3,5-O-dicaffeoylquinic acid)
异绿原酸C
(4,5-dicaffe-oylquinic acid)
连翘苷
(forsythin)
和厚朴酚
(honokiol)
厚朴酚
(magnolol)
2311017.5393.9201.0680.9551.2413.0375.2590.9311.4280.9392.783
2311027.5053.4850.9690.8371.4363.1245.3210.9661.9920.9422.744
2311037.6063.9121.0660.9531.0093.6025.3711.0122.0531.0182.827
), ArticleFig(id=1206300929935082078, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272762407092819, language=CN, label=表2, caption=

金连驱瘟胶囊中11个成分含量测定结果

, figureFileSmall=null, figureFileBig=null, tableContent=
批号
(lot No.)
含量(content)/(mg · g-1n=3)
绿原酸
(chlorogenic acid)
葛根素
(puerarin)
3’-甲氧基
葛根素
(3’-methoxy puerarin)
葛根素芹
菜糖苷
(puerarin apioside)
甘草苷
(liquiritin)
连翘酯苷A
(forsythoside A)
异绿原酸A
(3,5-O-dicaffeoylquinic acid)
异绿原酸C
(4,5-dicaffe-oylquinic acid)
连翘苷
(forsythin)
和厚朴酚
(honokiol)
厚朴酚
(magnolol)
2311017.5393.9201.0680.9551.2413.0375.2590.9311.4280.9392.783
2311027.5053.4850.9690.8371.4363.1245.3210.9661.9920.9422.744
2311037.6063.9121.0660.9531.0093.6025.3711.0122.0531.0182.827
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HPLC法同时测定金连驱瘟胶囊中11个成分的含量*
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刘一菲 , 屠万倩 , 张留记 ** , 李开言 , 张迪文 , 杨丹
药物分析杂志 | 成分分析 2025,45(5): 796-801
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药物分析杂志 | 成分分析 2025, 45(5): 796-801
HPLC法同时测定金连驱瘟胶囊中11个成分的含量*
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刘一菲 , 屠万倩, 张留记** , 李开言, 张迪文, 杨丹
作者信息
  • 河南省中西医结合医院,郑州 450000
  • Tel:15617560688;E-mail:

通讯作者:

** Tel:(0371)66331598;E-mail:
Simultaneous determination of eleven constituents in Jinlian Quwen capsules by HPLC
Yi-fei LIU , Wan-qian TU, Liu-ji ZHANG** , Kai-yan LI, Di-wen ZHANG, Dan YANG
Affiliations
  • Henan Integrative Medicine Hospital, Zhengzhou 450000, China
doi: 10.16155/j.0254-1793.2024-1361
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目的:建立HPLC法同时测定金连驱瘟胶囊中绿原酸、葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷、甘草苷、连翘酯苷A、异绿原酸A、异绿原酸C、连翘苷、和厚朴酚及厚朴酚11个成分的含量。方法:采用Waters AtlantisTM T3(150 mm×4.6 mm,3 μm)色谱柱,以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,体积流量1.0 mL · min-1,柱温35 ℃,进样量4 μL,检测波长为225 nm(检测连翘苷)、250 nm(检测葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷)、276 nm(检测甘草苷)、290 nm(检测和厚朴酚、厚朴酚)和325 nm(检测绿原酸、异绿原酸A、异绿原酸C、连翘酯苷A)。结果:上述11个成分在各自检测范围内线性关系良好(r均≥0.999 5),平均加样回收率(n=6)在100.1%~108.1%,RSD 在2.8%~4.1%。3批样品中各成分含量范围分别在7.505~7.606、3.485~3.920、0.969~1.068、0.837~0.955、1.009~1.436、3.037~3.602、5.259~5.371、0.931~1.012、1.428~2.053、0.939~1.018和2.744~2.827 mg · g-1结论:该方法简单、灵敏、准确、可靠,可为金连驱瘟胶囊质量标准的建立提供参考。

金连驱瘟胶囊  /  高效液相色谱  /  化学成分  /  含量测定

Objective: To establish an HPLC method for the simultaneous determination of chlorogenic acid,puerarin, 3’-methoxy puerarin, puerarin apioside, liquiritin, forsythoside A, 3,5-O-dicaffeoylquinic acid,4,5-dicaffeoylquinic acid, forsythin, honokiol and magnolol in Jinlian Quwen capsules. Methods: The analysis was performed on a Waters AtlantisTM T3 (150 mm×4.6 mm, 3 μm) column, and the mobile phase was comprised of acetonitrile-0.1% phosphoric acid, with the flow rate of 1.0 mL · min-1 in a gradient elution manner. The column temperature was set at 35 ℃. The injection volume was 4 μL and the UV detection wavelengths were set at 225 nm (detecting forsythin), 250 nm (detecting puerarin, 3’-methoxy puerarin and puerarin apioside), 276 nm(detecting liquiritin), 290 nm (detecting honokiol and magnolol) and 325 nm (detecting chlorogenic acid,3,5-O-dicaffeoylquinic acid, 4,5-dicaffeoylquinic acid and forsythoside A). Results: All the 11 constituents showed good linearity within their detection ranges (r≥0.999 5), whose average recoveries (n=6) were 100.1%-108.1%, with the RSDs of 2.8%-4.1%. The content ranges of 11 components in three batches of samples were 7.505-7.606 mg · g-1, 3.485-3.920 mg · g-1, 0.969-1.068 mg · g-1, 0.837-0.955 mg · g-1, 1.009-1.436 mg · g-1,3.037-3.602 mg · g-1, 5.259-5.371 mg · g-1, 0.931-1.012 mg · g-1, 1.428-2.053 mg · g-1, 0.939-1.018 mg · g-1 and 2.744-2.827 mg · g-1, respectively. Conclusion: The method is simple, sensitive and reliable. It can be used as a reference for the establishment of quality standard of Jinlian Quwen capsules.

Jinlian Quwen capsules  /  HPLC  /  chemical constituents  /  content determination
刘一菲, 屠万倩, 张留记, 李开言, 张迪文, 杨丹. HPLC法同时测定金连驱瘟胶囊中11个成分的含量*. 药物分析杂志, 2025 , 45 (5) : 796 -801 . DOI: 10.16155/j.0254-1793.2024-1361
Yi-fei LIU, Wan-qian TU, Liu-ji ZHANG, Kai-yan LI, Di-wen ZHANG, Dan YANG. Simultaneous determination of eleven constituents in Jinlian Quwen capsules by HPLC[J]. Chinese Journal of Pharmaceutical Analysis, 2025 , 45 (5) : 796 -801 . DOI: 10.16155/j.0254-1793.2024-1361
金连驱瘟胶囊为河南省中西医结合医院的医院制剂,由金银花、连翘、板蓝根、炙麻黄、苦杏仁、石膏、薄荷脑、葛根、天花粉、大黄、厚朴、甘草共12味药材组成。方中药味表里兼顾以解表为急,寒热同调以除热为重,具有辛凉疏表、宣肺平喘、生津止渴之功效,用于治疗流行性感冒热毒袭肺证[1-3]。已有文献研究报道,金银花富含的绿原酸、异绿原酸A、异绿原酸C等酚酸类成分[4],连翘中的连翘酯苷A等苯乙醇苷类成分及木脂素类成分连翘苷均具有良好的抗炎解热作用[5-6],葛根中富含的葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷等异黄酮类成分[7-8]与厚朴中厚朴酚、和厚朴酚等木脂素类成分,具有明确的抗氧化、抗菌、抗病毒等药理活性[9-11],均属本品中的功效成分。
金连驱瘟胶囊目前尚无定量标准,本实验结合文献报道[12]与2020年版《中华人民共和国药典》[13]规定,建立了可同时测定金连驱瘟胶囊中绿原酸、异绿原酸A、异绿原酸C、葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷、甘草苷、连翘酯苷A、连翘苷、和厚朴酚、厚朴酚含量的HPLC法,为该制剂有效成分的含量测定和质量控制提供评价依据。
Acquity ArcTM高效液相色谱仪(配有2998二极管阵列检测器、Acquity ArcTM四元泵、Acquity ArcTM自动进样器和Empower 3色谱工作站),Waters公司;AE 240型十万分之一天平,梅特勒公司;ULUP Ⅳ 10T超纯水机,四川优普超纯科技有限公司;SB-5200DT超声波清洗机,宁波新芝生物科技股份有限公司。
对照品绿原酸(批号110753-202119,含量以96.3%计)、葛根素(批号110752-202217,含量以96.8%计)、甘草苷(批号111610-202209,含量以95.2%计)、连翘酯苷A(批号111810-202209,含量以96.4%计)、连翘苷(批号110821-202318,含量以95.8%计)、和厚朴酚(批号110730-201915,含量以99.8%计)、厚朴酚(批号110729-202316,含量以99.2%计),中国食品药品检定研究院;对照品3’-甲氧基葛根素(批号100054-202311,含量以98%计)、葛根素芹菜糖苷(批号070111-202202,含量以98%计)、异绿原酸A(批号150005-202310,含量以98%计)、异绿原酸C(批号250036-202310,含量以98%计),北京德信汇医药科技有限公司。色谱纯甲醇和乙腈,Thermo Fisher Scientific公司;水为实验室自制超纯水;磷酸等试剂为分析纯。金连驱瘟胶囊(批号231101、231102、231103,装量0.34 g · 粒-1),河南省中西医结合医院制剂室。
采用 Waters AtlantisTM T3(150 mm×4.6 mm,3 μm)色谱柱,以乙腈(A)-0.1%磷酸水溶液(B)为流动相,梯度洗脱(0~9 min,8%A→13%A;9~15 min,13%A;15~18 min,13%A→18%A;18~24 min,18%A;24~25 min,18%A→35%A;25~28 min,35%A;28~30 min,35%A→70%A;30~45 min,70%A),体积流量1.0 mL · min-1,柱温35 ℃,检测波长为225 nm(连翘苷)、250 nm(葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷)、276 nm(甘草苷)、290 nm(和厚朴酚、厚朴酚)和325 nm(绿原酸、异绿原酸A、异绿原酸C、连翘酯苷A),进样量4 μL。
取本品内容物0.65~0.70 g(约相当于2粒量,装量按0.34 g · 粒-1计),精密称定,置于100 mL具塞三角瓶中,精密加入甲醇25 mL,密塞后混匀,称量,超声(功率250 W,频率40 kHz)处理40 min,取出冷却,称量并用甲醇补足减失的量,摇匀后滤过,滤液过0.22 μm微孔滤膜,取续滤液,即得。
取各对照品适量,精密称定,用甲醇配成每1 mL分别含绿原酸0.383 mg、葛根素0.307 mg、3’-甲氧基葛根素0.061 mg、葛根素芹菜糖苷0.044 mg、甘草苷 0.026 mg、连翘酯苷A 0.207 mg、异绿原酸A 0.112 mg、异绿原酸C 0.019 mg、连翘苷0.056 mg、和厚朴酚0.061 mg、厚朴酚0.171 mg的混合溶液,即得。
按处方比例,参照金连驱瘟胶囊制法,分别制成缺金银花、缺连翘、缺葛根、缺厚朴和缺甘草的阴性样品,再按“2.2.1”项下方法,分别制成阴性样品溶液。
取“2.2”项下混合对照品溶液、供试品溶液和5种阴性样品溶液各4 μL,按“2.1”项下条件进样测定。结果见图1,供试品色谱中,11个待测成分的分离度良好,5种阴性样品溶液在与待测物相对应的保留时间附近无干扰,表明该方法专属性良好。
精密量取“2.2.2”项下混合对照品溶液2、3、4、5、6 μL,分别按照“2.1”项下条件进样分析,以各成分的进样量(X,μg)为横坐标,以测得的峰面积Y为纵坐标,进行线性回归,计算相关系数(r),结果见表1
精密量取“2.2.2”项下混合对照品溶液4 μL,按“2.1”项下色谱条件连续进样6次测定,记录各待测成分的峰面积,计算RSD。结果绿原酸、葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷、甘草苷、连翘酯苷A、异绿原酸A、异绿原酸C、连翘苷、和厚朴酚、厚朴酚峰面积的RSD分别为0.76%、3.0%、0.65%、0.98%、2.7%、1.0%、0.71%、0.65%、0.81%、1.0%和0.70%,表明仪器精密度良好。
取同一批金连驱瘟胶囊(批号231101)内容物适量,精密称取6份,参照“2.2.1”项下方法制成供试品溶液,按“2.1”项下条件进样测定。结果绿原酸、葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷、甘草苷、连翘酯苷A、异绿原酸A、异绿原酸C、连翘苷、和厚朴酚、厚朴酚的平均含量分别为7.606、3.556、1.066、0.953、0.654、3.225、4.561、0.833、1.021、0.997和2.827 mg · g-1,RSD分别为0.88%、1.4%、0.86%、1.2%、3.8%、1.4%、1.5%、1.3%、1.3%、1.2%和1.0%,表明该方法的重复性良好。
取同一份金连驱瘟胶囊(批号231101)供试品溶液,照“2.1”项下色谱条件,于制备后0、1、2、3、4、5、6、7、8 h进样测定,结果绿原酸、葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷、甘草苷、连翘酯苷A、异绿原酸A、异绿原酸C、连翘苷、和厚朴酚、厚朴酚峰面积的RSD依次为0.63%、2.9%、0.63%、0.93%、2.2%、0.84%、0.67%、0.86%、1.3%、1.3%和0.62%,表明供试品溶液在8 h内稳定性良好。
精密称取已知含量的1粒金连驱瘟胶囊(批号231101)的内容物,置于具塞三角瓶中,分别精密加入用甲醇配制的每1 mL分别含有绿原酸0.103 mg、葛根素0.064 mg、3’-甲氧基葛根素0.014 mg、葛根素芹菜糖苷0.011 mg、甘草苷0.015 mg、连翘酯苷A 0.048 mg、异绿原酸A 0.083 mg、异绿原酸C 0.012 mg、连翘苷0.028 mg、和厚朴酚0.014 mg、厚朴酚0.038 mg的混合对照品溶液25 mL,照“2.2.1”项下方法平行制成6份供试溶液,按“2.1”项下条件进样分析,计算各成分的回收率。结果绿原酸、葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷、甘草苷、连翘酯苷A、异绿原酸A、异绿原酸C、连翘苷、和厚朴酚、厚朴酚的回收率均值分别为103.5%、103.5%、101.1%、107.6%、107.2%、106.7%、105.0%、100.1%、104.0%、103.8%、108.1%,RSD依次为3.5%、3.9%、4.0%、4.1%、3.6%、3.3%、3.4%、3.6%、2.8%、4.0%和3.5%。
取金连驱瘟胶囊样品(批号为231101、231102、231103),按“2.2.1”项下方法制备供试品溶液,在“2.1”项色谱条件下进样分析,记录各待测成分的峰面积并计算在金连驱瘟胶囊样品中的含量。结果见表2
金连驱瘟胶囊组方药味繁多,成分复杂。综合处方量及配伍原则,本研究参照2020年版《中华人民共和国药典》规定和已有文献对相关药材指标成分[12-17]的报道,初步选定以金银花的代表性成分绿原酸、异绿原酸A、异绿原酸C,连翘的代表性成分连翘苷、连翘酯苷A,板蓝根的代表性成分(RS)-告依春,苦杏仁的代表性成分苦杏仁苷,葛根的代表性成分葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷,厚朴的代表性成分和厚朴酚、厚朴酚,甘草的代表性成分甘草苷为指标进行测定。预试验结果显示,(RS)-告依春和苦杏仁苷含量较低,无法准确测定其含量且峰形欠佳,也无法与相邻色谱峰有效分离,故本研究以绿原酸、葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷、甘草苷、连翘酯苷A、异绿原酸A、异绿原酸C、连翘苷、和厚朴酚、厚朴酚等11个成分为金连驱瘟胶囊的定量指标。
结合各待测成分的理化性质及金连驱瘟胶囊的制备工艺,本实验分别对供试品的提取方式、提取时间及提取溶剂进行了考察优选[18-21]。以不同体积分数的甲醇水溶液(50%、70%、100%)为溶剂,对比超声或加热回流方式在不同提取时间(20、30、40 min)制备的供试品溶液,发现100%甲醇超声提取40 min时各成分检测含量高,且操作简便高效。
本实验考察了甲醇、乙腈与不同体积分数的磷酸水溶液等流动相体系,发现由乙腈和0.1%磷酸溶液组成流动相,梯度洗脱时基线较平稳,各待测成分峰形良好,与相邻峰均可有效分离,对应保留时间附近无阴性干扰。对各成分进行190~400 nm全波长扫描,综合各物质出峰时间及最大吸收波长,最终选定在225~325 nm区间内分时间段切换波长扫描,提高测定的灵敏度。另外,试验中先后对Waters AtlantisTM T3(4.6 mm×150 mm,3 μm)、Aglient InfinityLab Poroshell 120 Aq-C18(2.1 mm×100 mm,2.7 μm)和菲罗门Comixsep Polar BiPFP(4.6 mm×100 mm,3 μm)色谱柱进行考察,结果显示本文所建立方法可在多种色谱柱上实现分离,待测物出峰保留时间稳定,峰形良好。
以绿原酸、异绿原酸A、异绿原酸C、葛根素、3’-甲氧基葛根素、葛根素芹菜糖苷、甘草苷、连翘酯苷A、连翘苷、和厚朴酚、厚朴酚等成分为指标,本实验建立了可同时测定金连驱瘟胶囊中上述11个成分含量的HPLC法,方法简便灵敏,稳定可靠,能较全面地评价该制剂的内在质量,保证临床用药的安全有效,同时也为今后将该制剂作开发成创新药物提供实验依据。另外,葛根、金银花、连翘均属解表剂中常见药物,甘草调和诸药,本文所建立的金连驱瘟胶囊中11个成分同时定量的方法,也可为含上述成分的相似制剂的定量控制研究提供技术支持。
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doi: 10.16155/j.0254-1793.2024-1361
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2种不同金属材料的力学参数

Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)

Genus
种数
Number of
species
占总种数比例
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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