消增颗粒淫羊藿苷的测定

消增颗粒淫羊藿苷的测定 Ci—R r- — RbCr 注:ci为样品溶液的浓度;Cr为对照品溶液的浓度;Ri为样 品溶液的荧光强度;Rr为对照品溶液的荧光强度;Rb为空白 溶剂的荧光强度. 按拟定的含量测定,测定了3批盐酸特拉唑嗪胶囊 的含量,结果见表2. 表2样品测定结果(标示量%) Tab2Determinationresultsofsamples(thelabeleda— mount%) 4讨论 DeterminationoficariininXiaozenggranules 4.1比较了不同浓度的盐酸液,甲醇和甲醇.水.盐酸不同比 例的混合液作为溶剂,结果用甲醇一水一盐酸(300:700:0.9)作 为溶剂既能使样品易于溶解,又能使样品在此溶液中保持稳 定. 4.2根据盐酸特拉唑嗪的内源荧光测定其荧光强度,该方 法与高效液相色谱法测量结果相比较,基本一致.本法用甲 醇一水-盐酸(300:700:0.9)作为溶剂,测定盐酸特拉唑嗪胶囊 的含量,具有用量少,荧光强度稳定,操作方便,重现性好,灵 敏度高等优点,也可作为含量测定的一种常规方法. 参考文献 [1]刘玉真.盐酸特拉唑嗪的含量测定及含量均匀度检查.药物 分析杂志.1993,13(6):197. [2]国药局药品标准.WSr(X-088)-2003Z 收稿日期:2004-05.11 WANGJing—xia,XUJia— luan(ZhejiangHospitalofTraditionalChineseMedicine,Hangzhou310006,China) ABSTRACT:OBJECTIVEToestablishanHPLCmethodforanalysisoficariininXIAOZENGgranules.METHODSTheHPLC systemconsistedofG1314Avariablewavelengthuv— visibledetector,HypersilODS(4.6ram×250ram,5m),HPchemstation, Hp1100seriesquaternarypumpandvacuumdegasser(G1322A).ThemobilephaseWasacet onitrile:water(30:70,v/v).Theflow— ratewas1.0mLmin,,theinjectionvolumeWas20ul,andthedetectorwavelengthWas270nm.RESULTSThemethodWaslinearo- vertheicariinrangeof0.169,gto4.Op.g.therecoveryofmethodWas98.6%(n=5),theaverage RSDWas1.7%forprecisionof within-day,theaverageRSDwas2.1%forprecisionofbetween— day.CONCLUSIONThemethodissimple,accurateandselective, Canbeusedfordeterminationoficariin. KEYWORDS:Xiaozenggranules;icariin;HP【, 消增颗粒淫羊藿苷的测定 王京霞,许家鸾(浙江省中医院,浙江杭州310006) 摘要:目的建立高效液相色谱法测定消增颗粒中淫羊藿苷的含量方法.方法采用 HP1100高效液相色谱仪(包括G1314A 可变波长紫外检测器,HP化学工作站,G1322A真空脱气机,HP1100四元 泵),HypemilODS柱(4.6mm×250mm,5岬).流动 相:乙腈一水(30:70),流速:1.0mL?min一,检测波长:270am,进样量:20txl.结果淫羊藿 苷在0.16—4,0txg范围内呈现良好 的线性关系,回收率为98.6%(n=5),日内平均RSD为1.7%,日间平均RSD为2,l%. 结论该法简便,准确,具有专属性, 可用于测定消增颗粒淫羊藿苷的含量. 关键词:消增颗粒;淫羊藿苷;高效液相色谱法 中图分类号:R284,1文献标识码:B文章编号:1007—7693(2005)06-0489-03 Xiaozenggranulesisapreparationofourhospita1.Itconsis— tedoftwelveherbs,includingpericarpiumcitrireticulatae,her- baEpimedii,RadixGlycyrrhizaeect.itcancoursetheliverand rectifyqi,transformstasisdissipatebind,usinginbreastgland withliverdepressionandqistagnation.Inordertoestablishthe 中国现代应用药学杂志2005年l2月第22卷第6期 standardforqualityofXiaozenggranules,weselectHerbaEpi— medii,usingHPLCtodetermineicariininXiaozenggranules. 1ApparatusandReagents 1.1Apparatus Agilent1100chromatographicsystem(AgilentTechnolo— ChinJMAP,2005December.Vol,22No.6489 gies,USA)includingHpl100SeriesQuaternaryPump,avaria— blewavelengthuv—visibledetector(G1314A),avacuumdegas— ser(G1322A)andaHPchemstation.HypersilODS(4.6mm× 250ram,5tun)wasslurrypackedwithamonolayerofoctadecyl silane(Dupontcompany,USA).AnultrasonicdegasserKQ 3200(KUNSHANdetectioninstrumentfactory,Shanghai,Chi— an),athermostatwaterbath(Thefifthmedicalinstrumentcorpo- ration,Shanghai,China). 1.2Reagents HPLCgradeacetonitrile,methanol(SiYouchemicalrea- gentfactory,Tianjin,China).Distilledwatermadebyourselves. Analyticalpurityethanolandethylacetate(SuZhouchemicalre— agentfactory,ANHUI,China).Icariin(batch:0737-200111) supplierwaftNationalinstituteforthecontrolofpharmaceutical andBiologicalproducts.Thepolyamide(80一lOOmu,TaizhouLu. Qiaoehemicobiologyplasticfactory,ZHEJIANG,China).HPLC gradeaeetonitrile,methanolandwaterwerefilteredthrougha 2p,mfilteranddegassedundervacuumpriortouse.Xiaozeng granulesmadebyourselves. 2.Experimentalmethods 2.1Chromatographicconditions Thenumberoftheoreticalplatesofieariinwasmorethan 1500,aRPLCcolumnHypersilODS(4.6mm×250mm,5), themobilephasewasaeetonitrile:water(30:70,v/v).111e flowratewas1.0mL?min_.,theinjedionvolumewas20L, andthedetectorwavelengthwas270nm. 2.2EstablishedthestandardCurve Thestandardsolutionwerepreparedbyaccuratelyweighing (ieariinneeddry)anddissolvingintheappropriateamountsof methano1.Preparedaseriessolutionsoficariinstandardsample at0.2,0.1,0.04,0.02,0.008mg?mL,,theninjected 201~Ltomeasurethepeakareaundertheabove?-mentionedcon?- ditions.Analyzedlinearregressionwithareaintegrationasab- scissa(X)andinjectionamount(I.Lg)asordinate(Y).Ob- tainedtheregressionequation:Y=0.1056+0.0004448X,the linearrangeoficariinwas0.16g一4.0andthecorrelation ceefficient:r=0.9999(n=5). 2.3Theprecisiontestofmethod Preparesolutionsoficariinstandardsamplesthatconoentra- tionwere0.2mg?mL一,0.1mg?mL一,0.04mg?mL一,ac— cording2.1chromatographicconditions,measureeachsample peakareafivetimeseachday,forfoUowing5days,accordingto theregressionequation,calculatedthewithin—dayprecisionand between-dayprecision,resultswereshownintable1. 2.4Thereproductiontest Thesamplewerepreparedaccurately(batch:20021019), accordingto2.7sampleextractmethod,measureseve[1timesin sameway.Accordingtotheregressionequation,calculatedthe 490'ChinJMAP,2005December,Vo1.22No.6 contentoficariin.TheRSD=1.5%(n=7) Tab1Theresultsofprecisiontest 表1精密度试验结果 ConcentrationMethodrecoveryPrecision mg?mL一?SD/%Within-dayRSDBetween-dayRSD Note:theaverageRSDwas1.7%forprecisionolwithin—day,theaverage RSDwas2.1%forprecisionofbetween-day. 2.5Therecoverytest Prepareknownconcentrationsample(batch:20021019,con- tentwere0.468mg/10g)10g,mixedrespectivelywithstandard sample(concentrationwere0.04mg?mL)lOmL,accordingto 2.7sampleextractmethod,theninjected20ultomeasurethe peakareaundertheabove-mentionedconditions.Accordingto theregressionequation,resultsofrecoverywereshownintable 2. Tab2Theresultsofrecoverytest 表2回收率试验结果 2.6HPLCchromatographicfigure Accordingtoprescriptionratioproducethenegativerefer- encesamplewithoutHerbaEpimedii.MeasurethestandardSBHI- pie,thesampleandthenegativereferencesampleunderthea- bove—mentionedconditions,seeingfigure1. l…1Il?1if:i'…1' ,j Fig1TheHPLCchromatogramsofthenegativereferencesaln- ple(A),thesample(B),thestandardsample(c),(1): icariin 图1阴性样品(A),样品(B)及对照HPLC包谱图 2.7Determinationofsample 中国现代应用药学杂志2005年12月第22卷第6期 PreparedXiaozenggranules10g(passedthrough40mu) dissolvingin30mLethylacetate,refluxing0.5hour,coldingand filter.Thefilterextracttwotimeswith1mol?L,HC1,each time20mL,theethylacetateextractionevaporatetodrynessand theresiduewasredissolvedin2mLethano1.Theethanolsample waspassedthroughthepolyamidecolumn(80-100mu,5g,dp 10mm).Thepolyamidecolumnwaselutedwith100mLwater andthewatereluatewerethrownaway.Thenthecolumnwase— lutedwith80mLethanolandtheethanoleluatewasdriedusinga waterstreamandtheresiduewasredissolvedinlOmLethanol, theninjected20LLLtomeasurethepeakareaundertheabove- mentionedconditions,measuringfivebatchXiaozenggranules, eachsamplewiththreetimes.Theresultswereshownintable3. Tab3TheresultsofIcariininXiaozenggranules(n=3) 表3含量测定结果 3Discussion 3.1TherearemanycomplexcomponentsinXiaozenggranules. Icariinbelongtoflavonoid.Thepolyamidecolumnwasexclusive forflavonoid,itcanremainflavonoidandgetridofothercompo- nent,soweselectedthepolyamidecolumntopurifyicariin. 3.2Thepolyamidecolumnwaselutedwith100mLwater,one samplewascollectedeverylOmL,tensampleswerecollectedto— tally,theninjected20Ltomeasurethepeakareaofeverysam— pieseparatelyundertheabove—mentionedconditions,theresults suggestthattherewerenoicariininwatersample.Thencolumn waselutedwith80mLethanolandcollectingonesampleevery lOmL,Eigthsampleswerecollectedtotally,theninjected20ulto measurethepeakareaofeightsampleseparatelyunderthea— bore—mentionedconditions,theresultssuggestthattherewereal- mostnoicariinineishthsample,icariinin70mLethanoleluate, soweselectedthepolyamidecolumnwaselutedwithlOOmLwa- terandthewatereluatewerethrownaway.Thencolumnwaselu- tedwith80mLethanoland80mLofeluatewerecollected. Themethodissimple,accurateandexclusive. RFERENCES [1] [2] [3] Chinesepharmacopoeia[M]2000,vo1.1:267. ChaiYF,LiXL.Re—HPLCdeterminationoflcariininEpimedium brericomumanditspreparation[J],ChinJPharmAnal,1991,11 (3):207. NingJS,YangJO.DeterminationofleariininJinfukangoralLiq— uid[J].ChinJPharmAnal,2002,22(4):328. 收稿13期:2003-08-04 反相高效液相色谱法测定八珍颗粒中芍药苷含量研究 胡双丰(宁波市药品检验所,浙江宁波315040) 摘要:目的建立八珍颗粒的含量测定项目.方法采取RP—HPLC方法,HypemilC.8 色谱柱,流动相甲醇-水(38:62),流速 0.7mL?min一,检测波长230nm.结果芍药苷线性范围在0.125—5.0,相关系数 r=0.9998;样品平均回收率为100.8%, RSD=2.8%(n=5).结论该方法操作简便,结果准确,具有较好的重现性与稳定性,可 用于八珍颗粒的质量控制. 关键词:芍药苷;八珍颗粒;高效液相色谱 中图分类号:R917.792.1文献标识码:B文章编号:1007-7693(2005)06-0491-03 DeterminationofpaeoniflorininBazhengranulebyRP-HPLC HUShuang-feng(NingboInstituteforDrugControl,Ningbo315040,China) ABSTRACT:OBJECTIVETodeteminepaeoniflorincontentingranuleByRP— HPLC.METHODSThecontentofpaeoniflorinin thepreparationwasmeasuredbyRP—HPLC.RP— HPLCanalysiswascarriedoutonC,scolumn,themobilephase:methanol—water(38 :62),Theflowratewas0.7mL?min, andthedetectionwavelengthwas230nmRESULTSFromtherangeof0.125,5.0g, therewasanexcellentlinearshapebetweentheconcentrationandthearea(r=09998).Themea nrecoveryrateofpaeoniflorinwas 作者简介:胡双丰,女,主任巾药师,主从事中药检验.电活0574—87848343 中国现代应用药学杂志2005年12月第22卷第6期 ChinJMAP,20051)ecember,Vo1.22No.6491'