[生物医药论文精品a]玄参水提液陶瓷膜精制工艺初步研究

1玄参水提液陶瓷膜精制工艺初步研究罗友华，杨辉，黄亦琦，曾伟成（厦门市医药研究所厦门361003）摘要目的应用陶瓷膜分离技术对玄参水提液精制工艺进行初步研究。方法按单因素试验法，分别制备4种孔径陶瓷膜微滤精制液，以药液含固量、哈巴俄苷含量为优选指标，筛选出最佳的陶瓷膜孔径，并测定精制前后玄参水提液的浊度、粘度。结果膜孔径按含固量减少率由高到低顺序为10NM50NM200NM100NM，按哈巴俄苷转移率由高到低顺序为10NM100NM50NM200NM，4种孔径精制液浊度均比原液显著降低，而其粘度均无明显变化。结论初步确定10NM孔径的陶瓷膜对玄参水提液的精制效果最好。关键词陶瓷膜；微滤；玄参；哈巴俄苷；HG51G47G38PRIMARYSTUDYONREFININGOFRADIXSCROPHULARIAWATEREXTRACTBYCERAMICMEMBRANETECHNIQUELUOYOUHUA,YANGHUI,HUANGYIQI,ZENGWEICHENG（XIAMENMEDICALINSTITUTE,XIAMEN361003,CHINA）ABSTRACTOBJECTIVEUSETHECERAMICMEMBRANESEPERATIONTECHNIQUETOINVERSTIGATETHEREFINEMENTOFTHERADIXSCROPHULARIAWATEREXTRACTMETHODSACCORDINGTOTHESINGLEFACTOREXPERIMENTATION,4KINDSOFREFINEDLIQUIDWEREPREPAREDBYDIFFERENTCERAMICMEMBRANEAPERTURESTHEBESTMEMBRANEAPERTUREWASOPTIMIZEDBYVALUINGTHECONTENTOFTHESOLIDSANDHARPAGOSIDETHETURBIDITYANDVISCOSITYWEREDETERMINEDRESULTSTHEDECREASINGRATEOFTHESOLIDSCONTENTWAS10NM50NM100NM200NMANDTHEHARPAGOSIDECONTENTWAS10NM50NM100NM200NMTHETURBIDITYOF4KINDSOFREFINEDLIQUIDWEREDECREASEDSIGNIFICANTLY,BUTTHEREWERENOSIGNIFICANTDIFFERENCEINVISCOSITYCONCLUSIONTHE10NMCERAMICMEMBRANEISTHEBESTAPERTUREKEYWORDSCERAMICMEMBRANEMICROFILTRATIONRADIXSCROPHULARIAHARPAGOSIDEHPLCG1025药精制G11458前G3822以成分G19400G7509G5627G5058G5334G17837G980G3534G7424原G10714G7481分离G7446G17148。G19555G11540G1025药G10714G16782G2656制G2070技术G2469G4649，G1268G13491精制G7053法G3926水提G18267G8797法G5061G7304G19718出G980G1135G13582G9869A2A0A1。膜分离技术A3A4A5A6A7A8A9A10A11A12A13A14A15A16A173502Z20084038A18A19A20A21A22A23A24A25A26A27A28A27A29A30A31A11A32A33A34A35A36A37A38A39A40A27A41A42A43A44A45A46A31A47A48A45A49A50A51A52A31A31A53A33A54A19A48A55A56A57A43A17A58A59A60A61A18A61A58A59A58A61A62A61A63A64A65A66A67A68A57A43A69A70A71A72A71A67A57A71A70A73A74A70A72A71A75A76A70A662G7171以化G4410成分G19400分G4388量G5058G5334为分离原G10714，因其G14033G13803低、无G1120G8437G8757G7591、分离效率高G12573G10317G9869，G5062G5203G8879应用G1122G20147G2709、医药、化工、水G3800G10714G12573G20058G3507。G18331用膜分离技术对G1025药提G2474液进行分离提G13443，G2499G19512G2447G3835分G4388G7446G17148G2462其G4439G993G9354G5627微G12902，G7094降低G14033G13803G2460提高药G2709G13443度A77A78A79。其G1025，陶瓷膜G1867G7389G13796G18252G11909、G13796高G9213、G13796G7389G7438G9354G2070、G1363用G4563G2641G19283G12573优G9869，G4600其G17878用G1122G1025药提G2474液的精制A77A80A79。玄参为玄参G12197G7905G10301玄参G54G70G85G82G83G75G88G79G68G85G76G68NG76NG74G83G82G72NG86G76G86HG72MG86G79G17的G5190G10169G7693，G1867G7389G1949G15892G9375G19464、G8911G9791G16311G8614G12573G2163效，用G1122G9921G11161G1272G19464、G8953G1272G1427G12204、G11458G17208、G2705G11183G12573，含G10627G9923G18286G14832类、苯丙素苷类、G7389G7438G18252、挥G2469油G12573成分，其G1025哈巴俄苷（G75G68G85G83G68G74G82G86G76DG72）G7171G11458前玄参药材G2656制G2070的主要G17148量控制指标成分A77A81A82A83A79，现代药G10714活G5627研究表明玄参G1867G7389保肝、抗炎、抗G15892小板聚集、抗G13582G15892、抗氧化G12573作用。G7424文以玄参水提液为模型，以膜滤前后药液的含固量、哈巴俄苷含量转移率为优选指标，确定陶瓷膜的最优孔径，同时测定药液粘度、浊度G12573G10714化指标，对陶瓷膜技术精制玄参水提液工艺进行初步研究。1仪器与材料11仪器陶瓷膜小试设备（江苏久吾高G12197技股份G7389限公司）膜孔径为10NM、50NM、100NM、200NM，膜材G17148为A1A780A80，膜面积为0G171MA78，膜的形式为管式膜，管G192830G175M；高效液相色谱仪（美国WATERG54公司）1525泵，2487双波G19283紫外检测器；NDJ8G54型数显粘度计（上海精密G12197G4410仪器G7389限公司）；G54TZA24型浊度仪（南京艾赛G10317G12197技G2469G4649G7389限公司）；电G9921恒G9213水浴锅（上海沪南G12197G4410仪器联营厂）；YF40型微压循G10627煎药G7438（东华原医疗仪器厂）；G54HZG79G79G79型循G10627水真空泵（上海亚荣生化仪器厂）；BG51211D电G4388天平（德国G54G68G85TG82G85G76G88G86公司）。12材料玄参（厦门鹭燕制药G7389限公司，经鉴定符合G1025国药典（2005版）I部规定，批号20080401）；哈巴俄苷（G1025国药G2709生G10301制G2709检定所，供含量测定用，批号111730200604）；乙腈（色谱G13443，TEDIA公司，批号711916）；甲G18267（色谱G13443，TEDIA公司，批号710915）；冰醋G18252（AR，汕G3848市G16211G19483化工厂G7389限公司，批号0703072）；G8694氧化G19060（AR，江苏G18341G3375G2451试G2070厂）。2方法与结果21玄参水提液制备G12228G2474玄参G20290G102676G78G74，用循G10627煎药G7438分G1016G8437提G2474，提G2474G9213度95G263G794100G263，G8611G8437G216410G1505量水提G24742G8437，G8611G84371G175小时，G17819滤，合并滤液，G12228G18337，G2474G7691后均分为4份，G8611份28G46G74，密G4565G1931G15267备用。22玄参水提液的膜过滤2G172G171膜初G3999水G17902量测定分别G457010NM、50NM、100NM、200NM的陶瓷膜G6930G1849膜分离小试设备，G2164G1849G13443水10G47，G6521G17902电G9316，G16855G14422G19412门，G1363进G2487压G2159G994出G2487压G2159G1055G5058为1G170G78G74G18G70MA84，G8504时的膜G17902量G2375为G16825孔径膜的初G3999水G17902量。G13479果G16277表1。由表1G2499G11705膜初G3999水G17902量G3534G7424G19555孔径的G3698G3835而G3698G2164。3A85A86A87A88A89A90A91A92A93A94A95A96A86A97A98A99A100A99A101A94A102A103A94A104A105A98A106A105A98A107A105A94A104A99A101A100A108A102A109A110A111A108A104A112A105A107A105A107A95A98A94A101A105APERTUREA113NMA114IMPORTPRESSUREA113KG/CM2A114OUTPORTPRESSUREA113KG/CM2A114A115A116A117A118A117A119A120A121A122A120A123A124A116A125A124A116A126A124A120A123A117A119A118A127A121A128A129A113L/M2A130A131A130KGA114102010380502010720100201072020020108802G172G172玄参水提液的膜G17819滤测G4448初G3999水G17902量后，G2533陶瓷膜小试设备G7754G1881G2164G184928G78G74玄参水提液，G5332G2563G1931G1969水，G11464G6521微滤。同时G861110分G19059G16772G5417G980G8437膜G17902量，G5415滤液G1781020G78G74时，G12447G2375G1584G8502微滤。按G8504法分别制备10NM、50NM、100NM、200NMG3247种孔径的膜滤液，G5483到4份精制液G7691G2709。4种孔径膜的G17902量变化G13479果G16277G32821、G32822。由G32821、G32822G2499G11705G19555G11540微滤的进行，4种孔径的膜G17902量均G1262G17817G17907G991降，按膜G17902量G15940减率G1186高到低的顺序为50NM200NM100NM10NM。A132A132A133A134A135A135A133A134A136A136A133A134A132A136A132A137A132A138A132A139A140A141A142A143A141A140A144A145A146A147A148A149A150A151A146A152A146A149A147A146A150A153A154A151A155A156A157A158A159A160A161A152A147A162A163A164A165A166A163A164A165A162A163A163A164A165A167A163A163A164A165A168A86A87A91A92A169A170A168A171A99A100A96A86A172A112A94A101A100A105A111A108A104A112A105A107A105A107A95A98A94A101A105A106A105A98A107A105A94A104A99A101A100A108A102A109A110A173A174A173A175A173A176A173A177A173A178A173A179A173A180A173A181A173A182A173A173A174A173A175A173A176A173A177A173A178A173A179A173A183A184A185A186A187A185A184A188A189A190A191A192A190A193A194A191A195A196A197A197A198A195A199A190A200A190A200A201A194A191A193A190A202A190A194A200A190A191A195A196A193A203A198A204A205A206A207A208A174A173A188A185A178A173A188A185A174A173A173A188A185A175A173A173A188A185A168A209A87A91A92A210A211A212A169A170A168A171A99A100A96A209A213A105A94A214A105A101A98A94A104A99A111A111A108A104A112A105A107A105A107A95A98A94A101A105A106A105A98A107A105A94A104A99A101A100A108A102A109A1104223膜清洗G6922集滤液后G1820G2462时用G14270G7481水G1926G8939，G11464G14279微滤液G9560G9177，用G13443水测定水G8939后的膜G17902量。G4570G9177G8939液G6930G4448后，G13505用1G8NG68G50HG9354液10G78G74，循G10627G9177G893930MG76N，G9994后用G14270G7481水G8939G14279G1025G5627，G1889用G13443水测定G11909G8939后的膜G17902量。G13479果G16277表2。A215A216A217A218A219A220A221A222A223A218A219A221A222A224A225A226A227A216A226A227A228A228A229A230A226A231A225A232A229A229A106A105A98A107A105A94A104A99A101A100A233A234A235A236A225A233A237A229A231A238A234A229A225A232A239A232A240A229A231APERTUREA113NMA114THEMEMBRANEPERMEATINGFLUXAFTERWATERWASHINGA113L/M2A130HA130KGA114THERECOVERYRATEOFMEMBRANEPERMEATINGFLUXAFTERWATERWASHINGA113A114THEMEMBRANEFLUXAFTERALKALIWASHINGA113L/M2A130A131A130KGA114THERECOVERYRATEOFMEMBRANEPERMEATINGFLUXAFTERALKALIWASHINGA113A1141022057938010050280389680944100320444680944200200227840955由表2G2499G162774种膜经水G8939后的膜G17902量G5686G3809率G1177G1781022G177G79457G179G705，其G1025200NM膜的水G8939后膜G17902量G5686G3809率最低，10NM膜的水G8939后膜G17902量G5686G3809率最高，G2499G14033G7171因为G7424G1319G13007G1363200NM膜G1147生G1114G1881部G8757G7591，而对10NM膜主要G1147生表面G8757G7591。4种膜经1G8NG680H水G9354液G9177G8939后的膜G17902量G5686G3809率均G1781094G8以上，G6937膜G9177G8939合G7696，G2499供G991G8437G18337G3809G1363用。23浊度测定用浊度计测定浊度。G13479果G16277表3。24粘度测定用数显粘度计测定粘度，G18331用3号转G4388，转G1790730G85G18MG76N。G13479果G16277表3。A215A241A242A243A244A245A246A247A248A249A247A243A244A246A247A248A249A224A225A226A227A241A224A250A229A237A235A231A226A239A251A239A237A252A225A232A251A253A239A254A238A255A254A239A237A252A255A233A254A226A227A239A237A254A238A255A239A237A225A230A12A234A229A254A83A120A126A125A121A124A70A51A128A116A0A117A1A117A123A2A86A3A51A4A5A90A117A70A6A7A70A117A123A2A86A8A120A9A70A5A92A120A123A124A116A124A129A123A116A120A6A123A117A7A119A121A117A78A128A117A1A57A57A9A10A94A9A11A13A14A94A14A119A126A127A117A121A123A116A120A123A124A14A94A9A11A57A94A10A14A119A126A127A117A121A123A116A120A123A124A14A94A9A11A57A95A94A14A14A119A126A127A117A121A123A116A120A123A124A14A94A9A11A94A15A57A14A14A119A126A127A117A121A123A116A120A123A124A14A94A9A11A94A15由表3G2499G16277玄参水提液分别经4种孔径陶瓷膜微滤后，G2520G7691G2709液的浊度均显著降低，液G1319外G16278G5627G10378由G9163浊变G9560G9177，而粘度无明显变化。25含固量测定G4570制G5483的5份G7691G2709液G2520G247410MG47，G6930G1849G5062G9900G51903小时的表面G11411G1025，水浴G2164G9921，G11464G14279成G12276G14179G10378，移G1849G9900G12677103G263G9900G51903小时，G2474出G13634G5190G10169器G6930G193130MG76N，G12228G18337。G13479果G16277表4。5A215A44A242A243A244A245A29A16A223A224A225A226A227A44A224A250A229A254A255A234A239A251A47A238A255A232A237A225A239A232A239A232A240A238A255A232A237A229A232A237A255A233A254A225A230A12A234A229A254A83A120A126A125A121A124A70A51A131A124A70A7A121A117A1A61A6A7A119A123A120A117A119A117A119A118A6A7A119A123A124A119A123A113A118A75A94A14A126A17A114A51A131A124A1A124A6A116A124A120A70A124A116A120A123A124A7A127A70A7A121A117A1A61A6A7A119A123A120A117A119A117A119A118A6A7A119A123A124A119A123A113A100A114A92A120A123A124A116A124A129A123A116A120A6A123A117A7A119A121A117A78A128A117A1A14A9A13A57A57A57A75A94A14A119A126A127A117A121A123A116A120A123A124A14A9A13A14A57A54A13A57A9A15A10A14A119A126A127A117A121A123A116A120A123A124A14A9A13A14A13A10A13A57A9A95A94A14A14A119A126A127A117A121A123A116A120A123A124A14A9A13A94A94A54A13A14A9A15A57A14A14A119A126A127A117A121A123A116A120A123A124A14A9A13A14A11A15A13A57A9A11A101A18A51A131A124A1A124A6A116A124A120A70A124A116A120A123A124A7A127A70A7A121A117A1A61A6A7A119A123A120A117A119A117A119A118A6A7A119A123A124A119A123A102A94A61A113A51A131A124A70A7A121A117A1A61A6A7A119A123A120A117A119A117A119A118A6A7A119A123A124A119A123A7A127A127A117A121A123A116A120A123A124A75A51A131A124A70A7A121A117A1A61A6A7A119A123A120A117A119A117A119A118A6A7A119A123A124A119A123A7A127A122A120A123A124A116A124A129A123A116A120A6A123A114A103A113A57A14A75A57A19A114A103A94A14A14A100A2026哈巴俄苷含量测定G18331用HG51G47G38法测定A21A22A23。2G176G171色谱G7477G1226以G2325G1855G9931G3534G11801G9931G19202合G11801G14026为G3647G1817G2070，以乙腈为G8981G2172相A，以1G8醋G18252G9354液为G8981G2172相B，按表5的比G1375进行G7811度G8939G14085，检测波G19283为278NM。G10714G16782G3624板数按哈巴俄苷G4804计G993低G11225000。A215A48A49A24A25A26A27A49A24A26A27A224A225A226A227A48A224A250A229A231A225A237A229A255A233A230A255A226A239A234A229A12A250A225A254A229A230A255TIMEMINTHEMOBILEPHASEATHEMOBILEPHASEB02020A1055080A105502G176G172对G10043G2709G9354液制备精密G12228G2474哈巴俄苷对G10043G2709，用30G8甲G18267G18209成11G173G22037G74G18MG47G9354液，G2375G5483。2G176G173供试G2709G9354液制备G2462测定G7691G2709液用0G1745G22037M微孔膜G17819滤，密G4565备用。测G5483G2520G7691G2709HG51G47G38G3282，按G4804面积计G12651G2520G7691G2709哈巴俄苷转移率。G13479果G16277表6G2656G32823G794G32828。A215A28A242A243A244A245A30A31A32A33A34A35A36A243A244A30A31A32A33A224A225A226A227A28A224A250A229A226A227A237A231A225A232A254A233A229A231A231A225A237A229A229A231A255A233A250A250A225A231A12A225A240A255A254A239A251A229A225A231A255A233A254A225A230A12A234A229A254A83A120A126A125A121A124A106A124A123A124A119A123A117A7A119A123A117A126A124A113A70A114A8A124A120A91A120A116A124A120A51A116A120A119A70A127A124A116A116A120A123A124A113A100A114A37A38A39A40A38A41A42A43A45A46A50A72A52A53A55A56A52A58A59A59A60A62A63A63A96A96A64A62A62A64A98A65A66A55A67A56A67A68A55A56A66A72A55A69A52A53A58A69A71A73A69A74A59A59A60A64A62A76A59A76A77A79A62A80A76A98A59A63A53A81A82A69A58A55A56A66A55A67A59A59A60A64A77A96A59A76A76A79A76A84A96A84A64A60A80A59A80A63A53A81A82A69A58A55A56A66A55A67A59A59A60A64A62A59A59A59A84A64A76A63A84A84A79A60A96A84A59A63A63A53A81A82A69A58A55A56A66A55A67A59A59A60A64A77A96A59A59A64A77A79A64A79A84A80A60A63A79A76A63A63A53A81A82A69A58A55A56A66A55A67A59A59A60A64A80A64A59A59A59A62A80A96A77A84A59A60A84A62A85A87A88A89A67A55A56A66A53A93A82A67A56A56A66A55A67A52A82A89A66A56A97A66A99A52A93A69A74A67A52A82A93A66A81A97A58A67A93A104A107A108A67A66A109A66A56A67A66A52A82A82A69A58A55A56A66A55A67A98A108A67A66A109A66A56A67A66A52A82A110A66A55A67A56A67A68A55A56A66A72A55A111A112A107A76A63A98A76A62A111A112A59A63A63A113A1146A115A116A117A118A119A120A121A122A123A124A125A126A127A115A128A115A129A130A131A132A133A124A125A126A127A115A128A134A135A136A137A116A124A125A126A127A138A139A140A139A141A142A135A143A144A140A135A145A143A145A146A147A145A143A140A141A145A148A134A135A136A137A129A124A125A126A127A138A139A140A139A141A142A135A143A144A140A135A145A143A145A146A149A144A140A139A141A139A150A140A141A144A147A140A115510NMA151A152HPLCA153650NMA151A152HPLCA153A154A155A156A157A158A159A160A161A162A163A164A165A166A165A167A168A156A169A170A166A156A171A169A171A172A173A174A169A168A172A156A175A166A167A170A166A165A155A156A157A158A176A160A161A162A163A164A165A166A165A167A168A156A169A170A166A156A171A169A171A172A159A174A169A168A172A156A175A166A167A170A166A165A1537100NMA151A152HPLCA153A154A1538200NMA151A152HPLCA153A154A155A156A157A158A177A160A161A162A163A164A165A166A165A167A168A156A169A170A166A156A171A169A171A172A173A174A174A169A168A172A156A175A166A167A170A166A165A155A156A157A158A178A160A161A162A163A164A165A166A165A167A168A156A169A170A166A156A171A169A171A172A179A174A174A169A168A172A156A175A166A167A170A166A165由表6G2656G32823G794G32828G2499G11705G2520G7691G2709均G332411G17757G86G79411G17800G86G19400G7389哈巴俄苷吸G6922G4804，且HG51G47G38G3282谱的G4804形相近，说明玄参水提液经陶瓷膜微滤后的主要化G4410成分未G2469生明显变化。膜孔径按哈巴俄苷转移率G1186高到低排列的顺序为10NM100NM50NM200NM。3讨论G1025药化G4410成分的G3809G7446G5627导致G1025药生G1147G17819程G1025提G2474G2656分离工艺繁G7446、分离效率低、成G7424高、G10627境G8757G7591严G18337以G2462劳G2172强度G3835。膜分离技术应用G1122G1025药生G1147，G1867G7389许G3822G1268G13491G7053法无法比拟的优G9869分离G17819程简G1427，G17878用G1122G9921敏G5627G10301G17148的分离，分离效率高，G993消G13803G7389G7438G9354G2070，G2499以缩短生G1147周期，降低成G7424，分离选择G5627高，满足7G1025药现代化生G1147的要求A180A181A182。G1186表4G2499G11705，G33244种膜孔径G1025，10NM膜滤液含固量最小，其含固量减少率为32G179G8。由表6G2499G1627710NM膜滤液的哈巴俄苷转移率最高。由G32821、G32822G2499G11705