[生物医药论文精品]丹参分散片中丹参总酚酸和丹酚酸b的含量测定方法研究

丹参分散片中丹参总酚酸和丹酚酸B的含量测定方法研究摘要目的建立丹参分散片中丹参总酚酸及丹酚酸B的测定方法。方法以丹酚酸B作对照品，采用UV法测定丹参分散片中丹参总酚酸的含量；采用HPLC法测定丹参分散片中丹酚酸B的含量。结果本品中丹参总酚酸在020MG120MG范围内呈良好的线性关系（R09998，N6），平均回收率为9969，RSD097；丹酚酸B在044G220G范围内呈良好的线性关系R09999，N5，平均回收率为9563，RSD122。结论本方法简便可行，重复性好，可有效控制丹参分散片的质量。关键词丹参分散片；UV；HPLC；丹参总酚酸；丹酚酸B所属专业药剂（药剂质量标准研究）丹参为唇形科鼠尾草属植物丹参SALVIAMILTIORRHIZABGE的干燥根及根茎，是中医临床治疗心脑血管疾病的常用药材，祛瘀止痛，活血通经，对心血管系统，能扩张血管，加快血流，改善微循环，改变血液黏滞性1,2。现代药理学研究表明水溶性酚酸类是丹参的主要有效成分，其中丹酚酸B含量G7380G20652，活性G7380G53903,4。为G17839G980G8505G6564G20652药物G10995物G2045用G5242，G3252G13792G4570其制成分散片，G994G7234通片G2070G11468G8616，在G4861G16311及溶G1998G17907率方G19766G18129G3835G3835G3698加。为G1114控制丹参分散片的质量，G1457G16789疗效，本G7003采用G56G57法对丹参总酚酸G17839行含量测定，采用G43G51G47G38法对丹酚酸BG17839行含量测定，方法简便G451G1946G11842G451可控。G31G1214G3132G994G16809药11G1214G3132LC10ATVPG20652效液G11468G14406G16901G1214（G4719G8953G1856G2508）；UV2401PCG3423G13055G3818分G1821G1821G5242G1214（G4719G8953G1856G2508）；CQG3423G17241G3780G8886G9177G8939G3132（G990G9035G8830G17241G3780G8886G1214G3132有G19492G1856G2508）；AG285G3423G11017G4388G3837平（METTLERG1856G2508）G312G16809药G6164用G16809G2070中G19512G11014G18267为G14406G16901G13443，其G1325G16809G2070均为分G7524G13443。丹酚酸B对照品（中G3281药品G10995物制品G7828定G6164，G6221G2507111562200605）；丹参分散片（G14270制）。2总丹参酚酸的含量测定21溶液的制G3803211对照品溶液的制G3803G12946G4506G12228G2474丹酚酸B对照品，加60G11014G18267制成040MG/ML溶液，作为对照品G1660G3803液。212G1391G16809品溶液的制G3803G2474丹参分散片10片，研G13466，G2474G13434015G，G12946G4506G12228定，G1427950MLG4493量G10954中，加G184940ML60G11014G18267，G17241G378030MIN，G6930G1931，以60G11014G18267定G4493，G6683G2260。G17819G9400。G12946G4506量G2474G13505G9400液1MLG1427910MLG4493量G10954，以60G11014G18267定G4493，G6683G2260，G2375G5483。213G19464性G7691品溶液的制G3803根G6466G3800方制成G993含丹参G6564G2474物的分散片，G6365212G20045G991G1391G16809品溶液制G3803方法G3800理，作为G19464性G7691品溶液。22G8886G19283的G17885G6333G12946G4506量G2474211G20045G991对照品G1660G3803液2ML，G1427925MLG4493量G10954，加60G11014G18267定G4493，G6683G2260，作为对照品溶液，G2528G990G17860G24902G12193溶液G1122G13055G3818分G1821G1821G5242G1214中在190NMG794500NM范围内G17839行G6207G6563，G16772G5417G13055G3818G2572收G1821G16901，G13479G7536G16277G3282G20，G6164测G5483G7691品G994对照G3品G7380G3835G2572收G8886G19283为286NM，G1000空白G7691品无干扰。G3G32821G8886G19283G6207G6563G32821丹酚酸B对照品；2G1391G16809品；3G19464性G7691品23线性关系考察G12946G4506量G2474211G20045G991对照品G1660G3803液05，1，15，2，25，3ML分别G1427925MLG4493量G10954中，以75G11014G18267定G4493，G6683G2260。以75G11014G18267为空白，在286NMG8886G19283G3800测定G2572收G5242。以G2572收G5242为纵坐标G451丹参总酚酸浓G5242为横坐标绘制标G1946曲线，G5483回归方程Y21286X00082，R09998，N6。表明丹参总酚酸在020MG120MG范围内呈良好的线性关系。24重复性G16809验G2474G2528G980G6221G2507的丹参分散片，G6365212G20045G991G1391G16809品溶液制G3803方法，重复G17839行6次平行G16809验，测定G2572收G5242，G13479G7536RSD121，G13479G7536表明本方法重复性良好。25加G7691回收率G16809验G12228G2474已知含量的丹参分散片（G6221G250720071208）5份，每份G1343401G，G12946G4506G12228定，G1427950MLG4493量G10954中，分别G12946G4506加G1849211G20045G991对照品G1660G3803液5ML，G6365212G20045G991方法G3800理，测定G2572收G5242。根G6466标G1946曲线计算G7691品中丹参总酚酸的含量。G13479G7536G16277表1。表1UV加G7691回收率G16809验G13479G7536G13479G7536丹参总酚酸以丹酚酸B计平均回收率为9969，RSD为097，表明此方法的加G7691回收率良好。26G7691品测定G24743G6221丹参分散片，G6365212G20045G991方法制G3803G1391G16809品溶液，测定G2572收G5242。根G6466标G1946曲线，G5483G1998G7691品中总丹参酮的含量。G13479G7536G16277表2。表2丹参总酚酸含量测定G13479G7536A1A0A3A2A4A5A6A7A8A10A9A112007121062920071212658200712146423丹酚酸B的含量测定31G14406G16901条件G14406G16901柱ZORBAXODS46150MM,5M；流动G11468G11014G182671乙酸4555；柱温25；流G1790710ML/MIN；G7828测G8886G19283286NM。G17839G7691量为10L。理论塔板数G6365丹酚酸B峰计算应G993低G11221000。此条件G991分离情况良好，G19464性无干扰。G16277G32822G451G32823G451G32824。G32822G19464性G7691品G14406G16901G3282A13A12A8GA7A8MGA15A14A8MGA17A16A18MGA19A20A21A22A23A19A20A21RSD009816172008191012499690970099662620082498880102364320084299210108968520088510002009836182008169910G32823丹酚酸B对照品G14406G16901G32821丹酚酸BG32824G1391G16809品G14406G16901G32821丹酚酸B32溶液的制G3803321对照品溶液的制G3803G12946G4506G12228G2474丹酚酸B对照品，加水制成022MG/ML的溶液，作为对照品溶液。322G1391G16809品溶液的制G3803G2474丹参分散片10片，研G13466，G2474G1343402G，G12946G4506G12228定，G1427950MLG4493量G10954，加G184960G11014G1826740MLG11014G18267，G17241G378030MIN，G6930G1931，加60G11014G18267定G4493G14279刻G5242，G6683G2260。用045M微孔G9400膜G9400G17819，G2474G13505G9400液，G2375G5483。323空白G7691品溶液的制G3803根G6466G3800方制成G993含丹参G6564G2474物的分散片，G6365322G20045G991G1391G16809品溶液制G3803方法G3800理，作为G19464性G7691品溶液。33线性关系考察G12946G4506G2572G2474321G20045G991丹酚酸B对照品溶液2G4514G4516G4518G45110L，G6365G990G17860G14406G16901条件测定，以峰G19766积积分值为纵坐标，丹酚酸B量为横坐标绘制标G1946曲线，计算G5483回归方程Y1259252X14333R09999，N5，表明丹酚酸B量在044G220G范围内具有良好的线性关系。34G12946G4506G5242G16809验G12946G4506G2572G2474321G20045G991丹酚酸B对照品溶液10L，重复G17839G76915次，测定峰G19766积，G13479G7536RSD为078，表明此方法G12946G4506G5242良好。35稳定性G16809验G12946G4506G2572G2474322G20045G991G1391G16809品溶液，分别在0，1，2，4，5，6HG17839G769110L，测定峰G19766积积分值，G13479G7536RSD为109N6，表明G1391G16809品溶液分别在6H内稳定。G336重复性G16809验G2474G2528G980G6221G7691品G12946G4506G12228G2474G13434015G，G6365G1391G16809品溶液制G3803法G3800理，G17839行6次平行G16809验，测定丹酚酸B含量，G13479G7536其RSD为091，表明此方法重复性良好。37加G7691回收率G16809验G12228G2474已知含量的丹参分散片（G6221G250720071208，含量为198）5份，每份G1343401G，G12946G4506G12228定，G1427950MLG4493量G10954中，分别G12946G4506加G1849211G20045G991对照品G1660G3803液4ML，G6365322G20045G991方法G3800理，测定丹酚酸B的含量，计算回收率。G13479G7536G16277表3。3HPLC加G7691回收率G16809验G13479G7536A24A25A18GA26A18MGA27A28A18MGA17A16A18MGA19A20A21A22A23A19A20A21RSD010362051603569438956312201021201160355962501023202160353943811010842151603709687011042181603729625G13479G7536丹酚酸B平均回收率为9563，RSD为122，表明此方法的加G7691回收率良好。38G7691品测定G24743G6221G993G2528G6221G2507丹参分散片，G6365322G20045G991方法制G3803G1391G16809品溶液，G6365G990G17860G14406G16901条件G17839行测定，以G3818标法计算G7691品中丹酚酸B的含量。G13479G7536G16277表4。表4丹酚酸B含量测定G13479G7536A29A30A31A32A33BA26A18A34A35A362007121020120071212199200712142024讨论41溶G2070的G17885G6333在G1391G16809品溶液的制G3803G17819程中，由G1122辅料等G3252素可能会对目标成分的溶G1998G5242产G10995影响，能否G7380G3835程G5242的G6564G2474G1998药品中的目标成分，G4570影响到含量测定的G1946G11842性。G6365322G20045G991方法，本G7003采用G993G2528溶G2070G17241G3780G6564G2474，G17839行含量测定，G13479G7536G16277表5，表明60G11014G18267为G7380佳的G6564G2474溶G2070。表5G993G2528溶G2070G17241G3780后丹酚酸B含量的G8616较A37A38A39A40A31A32A33BA26A18A34A35A36A4114660A42A43198A42A4315842G17241G3780G3800理时间G17885G6333丹酚酸B具有热G993稳定性5，加热时间越G19283降G16311越多。G3252此，采用G17241G3780对G7691品G17839行G3800理，方法简单，G2528时避免G1114丹酚酸BG3252热G993稳定性G13792降G16311。在G17241G3780的时间G11842定G990，本G7003对G8616G1114G17241G378015MING45130MING45145MIN后G6164测G5483的丹酚酸B含量，G16277表6。G13479G7536表明G17241G378030MIN的效率G7380G20652。G3表6G993G2528G17241G3780时间丹酚酸B含量G8616较A44A45A46A47A34MINA36A31A32A33BA26A18A34A35A3615178301964519543丹参水溶性成分具有抗心肌缺血G994缺氧的作用，其主要是由酚酸类物质组成的，G13792丹酚酸B又是酚酸类中含量G7380多，药理活性G7380G5390的成分。G3252此，G2528时G4570丹参总酚酸及丹酚酸B作为指标成分，能够很好的控制丹参分散片的质量。G3A48A49A50A511A52A53A54A55A56A57A58A59A60A52A54A552005A61A62A63A64SA59A65A66A67A68A69A70A71A72A62A73A742005A595253A592A75A76A59A77A48A78A54A79A80A81A82A83A84A85A81JA59A60A86A87A88A89A90A91A741990A74104A67242243A593A92A93A94A59A95A96A97A59A77A48A98A99A100A101A102A103A104A105A105A77A106A107A108A109A110A111JA59A112A113A87A69A114A83A84A742000A74205A6710A594A115A116A117A59A118A52A119A59A120A121A122A59A77A48A98A99A100A106A107A123A68A89A124A54A79A82A125A124A89A103A126A127A108A109A110A111JA59A60A128A54A742004A74353A67341A595A129A130A131A59HPLCA132A133A134A135A136A137A138A139A60A77A106A107BA78A140A141JA59A142A143A54A69A742007A7