燈盞花素分散片燈盞花素分散片 燈盞花素滴丸 質(zhì)量標(biāo)準(zhǔn) 野

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燈盞花素分散片燈盞花素滴丸質(zhì)量標(biāo)準(zhǔn)野黃芩苷BreviscapinedispersibletabletsBreviscapineDroppingPillQualitystandardsWildyellowbaicalin

燈盞花素分散片論文：燈盞花素系列品種質(zhì)量標(biāo)準(zhǔn)研究

對(duì)燈盞花素滴丸、燈盞花素分散片2個(gè)系列品種進(jìn)行質(zhì)量標(biāo)準(zhǔn)研究并統(tǒng)一其質(zhì)量標(biāo)準(zhǔn),為燈盞花素系列品種提供質(zhì)控依據(jù)。方法：通過薄層色譜法研究并統(tǒng)一兩品種專屬性的鑒別條件；采用高效液相色譜法對(duì)其可能存在的有毒成分焦袂康酸建立了檢查方法,色譜柱為AgilentC18(TC)(250×4.6mm,5μm),滾動(dòng)相為甲醇-0.1%磷酸水溶液,梯度洗脫；流速為0.8mL·min-1,檢測(cè)波長(zhǎng)為270nm,柱溫為35℃；根據(jù)《中國(guó)藥典2023年版》二部附錄XC其次法,對(duì)兩品種的溶出度項(xiàng)目進(jìn)行檢查,并確立了統(tǒng)一的測(cè)定方法；采用高效液相色譜法建立統(tǒng)一兩品種的野黃芩苷含量測(cè)定方法,色譜柱為AgilentC18(TC)(250×4.6mm,5μm),滾動(dòng)相為甲醇-四氫呋喃-0.1%磷酸溶液(14：14：72),檢測(cè)波長(zhǎng)為335nm,流速為0.8mL·min-1,柱溫為35℃；建立燈盞花素滴丸、分散片及燈盞花素原料的HPLC指紋圖譜分析方法。采用高效液相色譜法,色譜柱為AgilentC18(TC)(250×4.6mm,5μm);滾動(dòng)相為乙腈-0.1mol·L-1醋酸銨(磷酸調(diào)pH至3.0),梯度洗脫；檢測(cè)波長(zhǎng)為335nm；流速為0.8mL·min-1;柱溫為35℃。

結(jié)果：野黃芩苷的薄層鑒別特征斑點(diǎn)明了、陰性無(wú)干擾,其有毒成分焦袂康酸規(guī)定不得檢出；在統(tǒng)一的溶出條件下,燈盞花素滴丸和燈盞花素分散片分別在30min、20min溶出限度為含量的70%、80%；通過高效液相色譜法測(cè)定燈盞花素滴丸和燈盞花素分散片中野黃芩苷含量,測(cè)定方法專屬性強(qiáng)、確鑿性和重復(fù)性好；應(yīng)用“中藥色譜指紋圖譜相像度評(píng)價(jià)系統(tǒng)〞對(duì)燈盞花素滴丸、燈盞花素分散片及燈盞花素原料各批次進(jìn)行了質(zhì)量評(píng)價(jià),相像度均≥0.99,方法縝密度、穩(wěn)定性和重復(fù)性良好。結(jié)論：以燈盞花素系列品種為示范性研究品種研究其質(zhì)量標(biāo)準(zhǔn),為中藥質(zhì)量標(biāo)準(zhǔn)研究和信息化體系建設(shè)平臺(tái)子課題中成藥質(zhì)量標(biāo)準(zhǔn)研究平臺(tái)建設(shè)提供依據(jù)。

:TostudythequalitystandardstwoseriesofvarietiesofBreviscapineDroppingPillandbreviscapinedispersibletablets,andtoharmonizeitsqualitystandards,astoprovidequalitycontrolbasistoBreviscapineseriesofvarieties.Method:Throughthinlayerchromatographytoreunificatetheexclusiveidentificationconditionsofthetwovarieties;usinghighperformanceliquidchromatographymethodtoestablishtheexaminationmethodexamingtoxicingredientspyromeconicacidexistprobably,columnwasAgilentC18(TC)(250mm×4.6mm×5μm),mobilephasewas

methanol-0.1%phosphoricacid,withgradientelution;flowrate

was0.8mL·min-1,thedetectionwavelengthwas270nm,columntemperaturewas35℃;referencetothesecondmethodofChinesePharmacopoeia2023editiontwoAppendixXC,twovarietiesofdissolutionitemtobechecked,andestablishedaunifieddetermination;usinghighperformanceliquidchromatographytoestablishaunifiedmethoddeterminingthescutellarinoftwovarieties,thecolumnwasAgilentC18(TC)(250mmx4.6mm×5μm),mobilephasewasmethanol-tetrahydrofuran-0.1%phosphoricacid(14:14:72),detectionwavelengthwas335nm,flowratewsa0.8mL·min-1,thecolumntemperaturewas35℃;toestablishHPLCfingerprintanalysismethodofBreviscapineDroppingPill,dispersibletabletsandBreviscapinerawmaterials.Usinghighperformanceliquidchromatography,columnwasAgilentC18(TC)(250mm×4.6mm×5μm);mobilephasewas

acetonitrile-0.1mol-L-1ammoniumphosphate(usingaceticacidadjusttopH3.0),gradientelution;thedetectionwavelengthwas335nm;aflowratewas0.8mL·min-1;columntemperaturewas35℃.Results:ThecharacteristicsspotsofthescutellarininTLCwereclear,withoutthenegativeinterference,toxicingredientspyromeconicacidshalln’tbedetected;undertheuniformdissolutionconditions,thecontentofdissolution

limitsforBreviscapineDroppingPillandbreviscapinedispersibletabletswere70%,80%at30minutesand20minutes,respectively;determiningthecontentofthescutellarinofBreviscapineDroppingPillandbreviscapinedispersibletabletsbyHighPerformanceLiquidChromatographyMethodwithgoodspccificity,accuracyandrepeatability;applingtheTraditionalChinesemedicinechromatographicfingerprintsimilarityofevaluationsystemtoassessthequalityofthebatchesofBreviscapineDroppingPill,breviscapinedispersibletabletsandBreviscapinerawmaterials,thesimilarity>0.99,theprecision,stabilityandreproducibilityofthemethodwasgood.Conclusion:UsingseriesofvarietiesofBreviscapineasthedemonstrationvarietiestostudythequalitystandards,andfortraditionalChinesemedicinequalitystandardsandsub-projectofinformationsystemconstructionplatformofproprietaryChinesemedicinesprovidethebasis.

燈盞花素系列品種質(zhì)量標(biāo)準(zhǔn)研究6-8

Abstract8-10

引言11-13

中文摘要第一部分質(zhì)量2鑒別項(xiàng)研究

標(biāo)準(zhǔn)研究13-5313-1714-16

1樣品收集狀況13

2.1儀器與試藥142.2鑒別試驗(yàn)

3檢查項(xiàng)研

2.3擬定方法的溫濕度考察16-17

究17-3525-3535-3636-37備38-404142-43

3.1焦袂康酸17-254含量測(cè)定項(xiàng)研究35-474.2對(duì)照品溶液的制備

36

3.2溶出度4.1儀器與試藥4.3測(cè)定波長(zhǎng)的選擇4.5供試品溶液的制4.7線性關(guān)系考察4.9穩(wěn)定性試驗(yàn)

4.12重

4.4滾動(dòng)相的選擇37-384.6專屬性考察40-41

4.8進(jìn)樣縝密度試驗(yàn)41-424.10檢測(cè)限43

4.11定量限43

44-4546-47

復(fù)性試驗(yàn)43-44量測(cè)定45-4647-52

4.13回收率試驗(yàn)4.15耐用性考察

4.14樣品含5質(zhì)量標(biāo)準(zhǔn)草案

6小結(jié)與探討52-53其次部分燈盞花素系列品

1.1參照物的選擇

3

種指紋圖譜研究53-7553

1參照物53

1.2參照物的制備532儀器與試藥53-54

試驗(yàn)過程54-59的選擇54-5656-57定58-59確立63峰的確定63證63-7465-6768-69

3.1供試品溶液的制備543.3色譜柱的選擇56

3.2滾動(dòng)相

3.4柱溫的選擇3.6色譜條件的確5指紋圖譜標(biāo)準(zhǔn)的

5.2共有

3.5測(cè)定