[生物醫(yī)藥論文精品]丹參分散片中丹參總酚酸和丹酚酸b的含量測(cè)定方法研究

丹參分散片中丹參總酚酸和丹酚酸B的含量測(cè)定方法研究摘要目的建立丹參分散片中丹參總酚酸及丹酚酸B的測(cè)定方法。方法以丹酚酸B作對(duì)照品，采用UV法測(cè)定丹參分散片中丹參總酚酸的含量；采用HPLC法測(cè)定丹參分散片中丹酚酸B的含量。結(jié)果本品中丹參總酚酸在020MG120MG范圍內(nèi)呈良好的線性關(guān)系（R09998，N6），平均回收率為9969，RSD097；丹酚酸B在044G220G范圍內(nèi)呈良好的線性關(guān)系R09999，N5，平均回收率為9563，RSD122。結(jié)論本方法簡(jiǎn)便可行，重復(fù)性好，可有效控制丹參分散片的質(zhì)量。關(guān)鍵詞丹參分散片；UV；HPLC；丹參總酚酸；丹酚酸B所屬專(zhuān)業(yè)藥劑（藥劑質(zhì)量標(biāo)準(zhǔn)研究）丹參為唇形科鼠尾草屬植物丹參SALVIAMILTIORRHIZABGE的干燥根及根莖，是中醫(yī)臨床治療心腦血管疾病的常用藥材，祛瘀止痛，活血通經(jīng)，對(duì)心血管系統(tǒng)，能擴(kuò)張血管，加快血流，改善微循環(huán)，改變血液黏滯性1,2。現(xiàn)代藥理學(xué)研究表明水溶性酚酸類(lèi)是丹參的主要有效成分，其中丹酚酸B含量G7380G20652，活性G7380G53903,4。為G17839G980G8505G6564G20652藥物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。為G1114控制丹參分散片的質(zhì)量，G1457G16789療效，本G7003采用G56G57法對(duì)丹參總酚酸G17839行含量測(cè)定，采用G43G51G47G38法對(duì)丹酚酸BG17839行含量測(cè)定，方法簡(jiǎn)便G451G1946G11842G451可控。G31G1214G3132G994G16809藥11G1214G3132LC10ATVPG20652效液G11468G14406G16901G1214（G4719G8953G1856G2508）；UV2401PCG3423G13055G3818分G1821G1821G5242G1214（G4719G8953G1856G2508）；CQG3423G17241G3780G8886G9177G8939G3132（G990G9035G8830G17241G3780G8886G1214G3132有G19492G1856G2508）；AG285G3423G11017G4388G3837平（METTLERG1856G2508）G312G16809藥G6164用G16809G2070中G19512G11014G18267為G14406G16901G13443，其G1325G16809G2070均為分G7524G13443。丹酚酸B對(duì)照品（中G3281藥品G10995物制品G7828定G6164，G6221G2507111562200605）；丹參分散片（G14270制）。2總丹參酚酸的含量測(cè)定21溶液的制G3803211對(duì)照品溶液的制G3803G12946G4506G12228G2474丹酚酸B對(duì)照品，加60G11014G18267制成040MG/ML溶液，作為對(duì)照品G1660G3803液。212G1391G16809品溶液的制G3803G2474丹參分散片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含丹參G6564G2474物的分散片，G6365212G20045G991G1391G16809品溶液制G3803方法G3800理，作為G19464性G7691品溶液。22G8886G19283的G17885G6333G12946G4506量G2474211G20045G991對(duì)照品G1660G3803液2ML，G1427925MLG4493量G10954，加60G11014G18267定G4493，G6683G2260，作為對(duì)照品溶液，G2528G990G17860G24902G12193溶液G1122G13055G3818分G1821G1821G5242G1214中在190NMG794500NM范圍內(nèi)G17839行G6207G6563，G16772G5417G13055G3818G2572收G1821G16901，G13479G7536G16277G3282G20，G6164測(cè)G5483G7691品G994對(duì)照G3品G7380G3835G2572收G8886G19283為286NM，G1000空白G7691品無(wú)干擾。G3G32821G8886G19283G6207G6563G32821丹酚酸B對(duì)照品；2G1391G16809品；3G19464性G7691品23線性關(guān)系考察G12946G4506量G2474211G20045G991對(duì)照品G1660G3803液05，1，15，2，25，3ML分別G1427925MLG4493量G10954中，以75G11014G18267定G4493，G6683G2260。以75G11014G18267為空白，在286NMG8886G19283G3800測(cè)定G2572收G5242。以G2572收G5242為縱坐標(biāo)G451丹參總酚酸濃G5242為橫坐標(biāo)繪制標(biāo)G1946曲線，G5483回歸方程Y21286X00082，R09998，N6。表明丹參總酚酸在020MG120MG范圍內(nèi)呈良好的線性關(guān)系。24重復(fù)性G16809驗(yàn)G2474G2528G980G6221G2507的丹參分散片，G6365212G20045G991G1391G16809品溶液制G3803方法，重復(fù)G17839行6次平行G16809驗(yàn)，測(cè)定G2572收G5242，G13479G7536RSD121，G13479G7536表明本方法重復(fù)性良好。25加G7691回收率G16809驗(yàn)G12228G2474已知含量的丹參分散片（G6221G250720071208）5份，每份G1343401G，G12946G4506G12228定，G1427950MLG4493量G10954中，分別G12946G4506加G1849211G20045G991對(duì)照品G1660G3803液5ML，G6365212G20045G991方法G3800理，測(cè)定G2572收G5242。根G6466標(biāo)G1946曲線計(jì)算G7691品中丹參總酚酸的含量。G13479G7536G16277表1。表1UV加G7691回收率G16809驗(yàn)G13479G7536G13479G7536丹參總酚酸以丹酚酸B計(jì)平均回收率為9969，RSD為097，表明此方法的加G7691回收率良好。26G7691品測(cè)定G24743G6221丹參分散片，G6365212G20045G991方法制G3803G1391G16809品溶液，測(cè)定G2572收G5242。根G6466標(biāo)G1946曲線，G5483G1998G7691品中總丹參酮的含量。G13479G7536G16277表2。表2丹參總酚酸含量測(cè)定G13479G7536A1A0A3A2A4A5A6A7A8A10A9A112007121062920071212658200712146423丹酚酸B的含量測(cè)定31G14406G16901條件G14406G16901柱ZORBAXODS46150MM,5M；流動(dòng)G11468G11014G182671乙酸4555；柱溫25；流G1790710ML/MIN；G7828測(cè)G8886G19283286NM。G17839G7691量為10L。理論塔板數(shù)G6365丹酚酸B峰計(jì)算應(yīng)G993低G11221000。此條件G991分離情況良好，G19464性無(wú)干擾。G16277G32822G451G32823G451G32824。G32822G19464性G7691品G14406G16901G3282A13A12A8GA7A8MGA15A14A8MGA17A16A18MGA19A20A21A22A23A19A20A21RSD009816172008191012499690970099662620082498880102364320084299210108968520088510002009836182008169910G32823丹酚酸B對(duì)照品G14406G16901G32821丹酚酸BG32824G1391G16809品G14406G16901G32821丹酚酸B32溶液的制G3803321對(duì)照品溶液的制G3803G12946G4506G12228G2474丹酚酸B對(duì)照品，加水制成022MG/ML的溶液，作為對(duì)照品溶液。322G1391G16809品溶液的制G3803G2474丹參分散片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含丹參G6564G2474物的分散片，G6365322G20045G991G1391G16809品溶液制G3803方法G3800理，作為G19464性G7691品溶液。33線性關(guān)系考察G12946G4506G2572G2474321G20045G991丹酚酸B對(duì)照品溶液2G4514G4516G4518G45110L，G6365G990G17860G14406G16901條件測(cè)定，以峰G19766積積分值為縱坐標(biāo)，丹酚酸B量為橫坐標(biāo)繪制標(biāo)G1946曲線，計(jì)算G5483回歸方程Y1259252X14333R09999，N5，表明丹酚酸B量在044G220G范圍內(nèi)具有良好的線性關(guān)系。34G12946G4506G5242G16809驗(yàn)G12946G4506G2572G2474321G20045G991丹酚酸B對(duì)照品溶液10L，重復(fù)G17839G76915次，測(cè)定峰G19766積，G13479G7536RSD為078，表明此方法G12946G4506G5242良好。35穩(wěn)定性G16809驗(yàn)G12946G4506G2572G2474322G20045G991G1391G16809品溶液，分別在0，1，2，4，5，6HG17839G769110L，測(cè)定峰G19766積積分值，G13479G7536RSD為109N6，表明G1391G16809品溶液分別在6H內(nèi)穩(wěn)定。G336重復(fù)性G16809驗(yàn)G2474G2528G980G6221G7691品G12946G4506G12228G2474G13434015G，G6365G1391G16809品溶液制G3803法G3800理，G17839行6次平行G16809驗(yàn)，測(cè)定丹酚酸B含量，G13479G7536其RSD為091，表明此方法重復(fù)性良好。37加G7691回收率G16809驗(yàn)G12228G2474已知含量的丹參分散片（G6221G250720071208，含量為198）5份，每份G1343401G，G12946G4506G12228定，G1427950MLG4493量G10954中，分別G12946G4506加G1849211G20045G991對(duì)照品G1660G3803液4ML，G6365322G20045G991方法G3800理，測(cè)定丹酚酸B的含量，計(jì)算回收率。G13479G7536G16277表3。3HPLC加G7691回收率G16809驗(yàn)G13479G7536A24A25A18GA26A18MGA27A28A18MGA17A16A18MGA19A20A21A22A23A19A20A21RSD010362051603569438956312201021201160355962501023202160353943811010842151603709687011042181603729625G13479G7536丹酚酸B平均回收率為9563，RSD為122，表明此方法的加G7691回收率良好。38G7691品測(cè)定G24743G6221G993G2528G6221G2507丹參分散片，G6365322G20045G991方法制G3803G1391G16809品溶液，G6365G990G17860G14406G16901條件G17839行測(cè)定，以G3818標(biāo)法計(jì)算G7691品中丹酚酸B的含量。G13479G7536G16277表4。表4丹酚酸B含量測(cè)定G13479G7536A29A30A31A32A33BA26A18A34A35A362007121020120071212199200712142024討論41溶G2070的G17885G6333在G1391G16809品溶液的制G3803G17819程中，由G1122輔料等G3252素可能會(huì)對(duì)目標(biāo)成分的溶G1998G5242產(chǎn)G10995影響，能否G7380G3835程G5242的G6564G2474G1998藥品中的目標(biāo)成分，G4570影響到含量測(cè)定的G1946G11842性。G6365322G20045G991方法，本G7003采用G993G2528溶G2070G17241G3780G6564G2474，G17839行含量測(cè)定，G13479G7536G16277表5，表明60G11014G18267為G7380佳的G6564G2474溶G2070。表5G993G2528溶G2070G17241G3780后丹酚酸B含量的G8616較A37A38A39A40A31A32A33BA26A18A34A35A36A4114660A42A43198A42A4315842G17241G3780G3800理時(shí)間G17885G6333丹酚酸B具有熱G993穩(wěn)定性5，加熱時(shí)間越G19283降G16311越多。G3252此，采用G17241G3780對(duì)G7691品G17839行G3800理，方法簡(jiǎn)單，G2528時(shí)避免G1114丹酚酸BG3252熱G993穩(wěn)定性G13792降G16311。在G17241G3780的時(shí)間G11842定G990，本G7003對(duì)G8616G1114G17241G378015MING45130MING45145MIN后G6164測(cè)G5483的丹酚酸B含量，G16277表6。G13479G7536表明G17241G378030MIN的效率G7380G20652。G3表6G993G2528G17241G3780時(shí)間丹酚酸B含量G8616較A44A45A46A47A34MINA36A31A32A33BA26A18A34A35A3615178301964519543丹參水溶性成分具有抗心肌缺血G994缺氧的作用，其主要是由酚酸類(lèi)物質(zhì)組成的，G13792丹酚酸B又是酚酸類(lèi)中含量G7380多，藥理活性G7380G5390的成分。G3252此，G2528時(shí)G4570丹參總酚酸及丹酚酸B作為指標(biāo)成分，能夠很好的控制丹參分散片的質(zhì)量。G3A48A49A50A511A52A53A54A55A56A57A58A59A60A52A54A552005A61A62A63A64SA59A65A66A67A68A69A70A71A72A62A73A742005A595253A592A75A76A59A77A48A78A54A79A80A81A82A83A84A85A81JA59A60A86A87A88A89A90A91A741990A74104A67242243A593A92A93A94A59A95A96A97A59A77A48A98A99A100A101A102A103A104A105A105A77A106A107A108A109A110A111JA59A112A113A87A69A114A83A84A742000A74205A6710A594A115A116A117A59A118A52A119A59A120A121A122A59A77A48A98A99A100A106A107A123A68A89A124A54A79A82A125A124A89A103A126A127A108A109A110A111JA59A60A128A54A742004A74353A67341A595A129A130A131A59HPLCA132A133A134A135A136A137A138A139A60A77A106A107BA78A140A141JA59A142A143A54A69A742007A7