[生物医药论文精品]高效液相色谱法测定蒙药“色布如棍钦德吉德”含量

高效液相色谱法测定蒙药“色布如棍钦德吉德”含量A1A0A1A0A2A3A4A5A6A7A8A9A10A11A12A13A14A13A15A16A17A18A19A20A21A22A23A20A8A24A25A26A27A28ODSC18A29A30A31A32A20A33A34A35A36A37A38A39A40A41A42A40A43A30A31A44A33A45A46A40A47A48A49A47A50A51A30A52A53A54A55A33A42A56A42A51A47A26A57A58A59A60A33A40A46A45A40A45A61A62A63A64A65A45A46A40A45A61A62A63A64A66A67A68A40A46A69A69A69A70A66A71A72A73A74A75A33A45A40A76A46A76A77A30A78A79A80A33A40A46A39A77A26A81A82A83A84A85A86A87A88A89A90A91A92A93A94A95A96A97A85A98A99A93A94A85A98蒙药“色布如棍钦德吉德”属散寒、温胃、下气药，临床主治胃寒、脘腹冷痛、呕吐等，主要成分为荜茇、白胡椒等二十一味中药。运用高效液相色谱法对本品中的荜茇、白胡椒建立含量测定方法。通过实验摸索，确定了比较理想的色谱条件，并经过方法学考察及阴性对照实验，表明该方法操作简单，重现性好，专属性强，方中其它组分对胡椒碱的测定无干扰，1仪器与试药岛津LC10ATVP泵，SPD10AVP型检测器,SHIMADZUCLASSVP色谱工作站，TU2450型可见紫外分光光度计。胡椒碱对照品（批G2507G7260775200203G709G726中G3281药品G10995G10301G2058品检定G6164G727蒙药“色布如棍钦德吉德”（批G2507G7262006051、2006069、2006089G709G726G1881蒙G2488G19475G6301G2904G11443蒙G2319G2319G19510G727阴性对照G7691G14270G18209G727G11014G18267为色谱G13443，G8712为G17241G13443G8712，其它试G2070G3355为分G7524G13443。2方法与G13479G7536G321色谱条件色谱G7621G726DIAMONSILRG19087G11719C18色谱G7621（250MMG104G23G17G25G80G80G15G24G80G709G727G8981G2172相G11014G18267G16G8712（G26G19G726G22G19G709G727G8981G17907为G20G17G19G80G79G18G80G76G81，检测G8886G19283为G22G23G22G3G81G80。22G9354液G18209G2058对照品G9354液G3G3G12946G4506G12228G2474胡椒碱对照品G17878量，G2164无G8712G1069G18267G2058成G8611G20G80G79含胡椒碱G20G80G74的G9354液作为对照品G9354液。G3G1391试品G9354液G3G3G2474本品G13434G20G17G25G20G74，G12946G4506G12228定，G13634G20G19G19G80G79G4493量G10954中，G2164无G8712G1069G18267G13434G27G19G80G79，G17241G3780G3800理（G2163G10587G21G24G19G58G15G21G19G46G43G93G709G22G19分G19059，G6930冷，G2164无G8712G1069G18267G14279G2063度，G6683G2260，G12175G5527，G12946G4506G2572G2474G990G9177液G20G19G80G79G15G3G13634G21G24G80G79G4493量G10954中，G2164无G8712G1069G18267G14279G2063度，G6683G2260，G9354液经G19G17G23G24G80G9400G14192G9400过G15G2375G5483。G3阴性对照G9354液G6365照G3800方G2474G19512白胡椒、荜茇G1209外的其它药G7460G17878量，G12946G4506G12228定，G1209下G6365G1391试品G9354液G18209G13634方法G2528法G18209G2058。23专属性G3G2474G1391试品G9354液、对照品G9354液G2656阴性对照G9354液G17839G7691，测G5483G13479G7536为G726阴性对照色谱G3282中G3324与胡椒碱对照品G1209及G1391试品色谱G3282相对G5224的G1457G11053G7114G19400G3800无色谱G4804G1998现，表明其它组分对胡椒碱的测定无干扰（见G3282G20G709。G3MINUTES00255075100125150175200225250275300VOLTS0000002500500075VOLTS0000002500500075G3G3G3G3MINUTES00255075100125150175200225250275300VOLTS0000002500500075VOLTS000000250050007516199MINUTES00255075100125150175200225250275300VOLTS0000002500500075VOLTS000000250050007516029A100A101A102A103A104A105A106A101A107A108A109A104A105A110A111A101A112A113A114A115A116A117A118A117A119A120A121A122A123A124A125A126A127A1192G17G23G3G13459性试验G3G2474胡椒碱对照品G13434G21G24G80G74，G12946G4506G12228定，G13634G21G24G80G79量G10954中，G2164无G8712G1069G18267G1363G9354G16311，并G12244G18334G14279G2063度，G6683G2260，G12946G4506G2572G2474G19G17G21G24、G19G17G24、G20G17G19、G20G17G24、G21G17G19、G21G17G24G80G79G9354液分G2047G13634G21G24G80G79量G10954中，G2164无G8712G1069G18267G14279G2063度，G6683G2260，G9354液经G19G17G23G24G22037G80G9400G14192G9400过，G17839G7691，G6365G990G17860色谱条件测定，G1209G4804G19766G12227对G17839G7691量G17839G15904G3250G5414分G7524，G13479G7536胡椒碱G3324G19G17G20G19G20G24G25G22037G74G794G20G17G19G20G24G25G22037G74G14551G3272G1881呈良好的G13459性关系。G3250G5414方程为G3YG25G259G19G22G22G20XG16G22G23G20G199G3G3G3G3RG19G17999G27G325稳定性G2656G12946G4506度G2474G2528一份G1391试品G9354液（2006051G709，分G2047于0H、2H、4H、8H、16HG17839G7691，测G5483含量的RSD为01，表明G1391试品G9354液G332416小G7114G1881稳定。G2474G2528一份G1391试品G9354液（2006069G709连续G17839G76916次，测G5483含量的RSD为04。G2474G2528一批G2507（批G25072006089G709G1391试品5份，G6365“22”项下G2058成G1391试品G9354液，G17839G7691，测G5483含量的RSD为06。27G3250收G10587G24743个不G2528量的G1391试品（批G25072006051G709各3份，各G13434066G、081G、098G，G12946G4506G12228定，G63651G7261的比例，各G12946G4506G2164入胡椒碱对照品G9354液G17878量，分G2047G6365“22”项下方法G2058成G1391试品G9354液，G17839G7691，测G5483平G3355G3250收G10587为1022，RSD为07。3G7691品测定分G2047G2474对照品G9354液G2656G1391试品G9354液G17839G7691测定，G6365外标法G1209G4804G19766G12227计算G5483胡椒碱含量，G13479G7536见表1G3。G3G3G3表1样品中胡椒碱含量测定结果批G2507含量（MG/GG7092006051542006069542006089544讨论G8981G2172相的选择G726参照文献A128A129A130，用G11014G18267G16G8712为G8981G2172相G17839G15904G8981G2172相条件摸索，通过不G2528比例的比较，当G8981G2172相的比例为（G26G19G726G22G19G709G7114，G7691品中的胡椒碱与其它成分达到较好的分G12175度，并具有较合G17878的G1457G11053G7114G19400。G3检测G8886G19283的选择G726G2474胡椒碱对照品G9354液，于紫外G16可见分光光度仪G990，G14270G21G19G19G81G80G794G26G19G19G81G80做光谱扫描，G13479G7536胡椒碱G3324G8886G19283G22G23G19G81G80G3800有最大G2572收，G13479合文献A131A132A133选用G22G23G22G81G80作为检测G8886G19283。G3提G2474G9354G2070的选择G726胡椒碱易G9354于无G8712G1069G18267，故选择无G8712G1069G18267作为提G2474G9354G2070。G3提G2474效G10587的考察G726G1209无G8712G1069G18267作为提G2474G9354G2070G17839G15904G17241G3780提G2474，实验中考察了G17241G3780G20G19分G19059、G21G19分G19059、G22G19分G19059、G23G19分G19059、G24G19分G19059等不G2528提