RP—HPLC测定复方当归妇康胶囊中丹参酮ⅡA的含量(英)
RP—HPLC测定复方当归妇康胶囊中丹参
酮?A的含量(英) 2005年4月
第27卷第4期
中成药
ChineseTraditionalPatentMedicine April2005
V0J.27No.4
参考文献
[1]宋立人,洪恂,丁绪亮,等主编.现代中药学大辞典(
)
[M].北京:人民卫生出版社.1231.
[2]
[3]
封锡兰,徐绥绪.苦碟子中新黄酮苷(II)[J].中国药物化学
杂志,2000,IO(2):143.
封锡志,徐绥绪,岳大彪,等.苦碟子中新黄酮苷[J].中国药
物化学杂志,2000,9(3):134—136.
RP—HPLC测定复方当归妇康胶囊中丹参酮?A的含量(英) 王新春,于志庚,陈卫军,胡志林
(新疆石河子大学医学院第一附属医院,新疆石河子832008) 关键词:HPLC;当归妇康胶囊;丹参酮?A
摘要:目的:建立HPLC法测定复方当归妇康胶囊中丹参酮IIA含量的方法.方法:采用ODS柱,以甲醇.水(80:10)为
流动相,检测波长为270nln,流速为1.0mL?min,.结果:丹参酮IIA在0.01,0.16Ixg,范围内呈良好线性关系,丹参
酮?A平均回收率99.73%,RSD为2.91%(=5).结论:该方法简便,分离完全,结果可靠,适用于该制剂的质量控制.
中图分类号:R927文献标识码:A文章编号:1001—1528(2005)04-0424-03 DeterminationoftanshinonelIAinCompoundDangguifukangCapsulebyRIP-
H]f.LC
WANGXin-chun,YUZhi—geng,CHENWei-jun,HUZhi-lin
(TheFirstHospitalaffai~atoMedicalCollege,ShiheziUniversity,Shlhezl832008,China)
KEYWORDS:tanshinoneIIA;DangguifukangCapsule;HPLC ABSTRACT:A:ToestablishaHPLCmetIlodf0rthedeterminationoftanshinone1IAinCom
poundDanguifu—
kangCapsule.METHODS:Analyticcolumn:ReliasilC18(5m,250mm×
4.6mln),protectivecolumn:(5
m,12.50mm×4.6mm);mobilephase:methnaol—
ultrapurewater(80:20);detectivewavelengthwasat270 nm;temperaturewasat30.C;theflowratewasabout1.0mL?min,.REsULTS:,I'}lestandardcurveshowed
agoodlinearitywithintherangeof1×10,
-0.16Ixg./-=0.9995.Theaveragerecoverywas99.73%and脚
was2.91%.CoNCLUSIoN:Themethodisfeasible.andsimpletooperateandsuitablefortheq
ualitycontrolof
CompoundDangguifukangCapsule.
CompoundDangguifukangCapsuleispreparedby ourhospital,whichiscomposedofseveraltraditional ChinesemedicinessuchasRadixAngelicasinensis, RadixSalviaeMiltiorrhiaze,andRadixAstragali,and soon.Thispreparationhasbeenusedintheclinicfor thetreatmentandpreventionofmenoxenia,painful menstruation,menoschesisandothergynecologicaldis—
eases
(
,
whichwasprescribedonthebaseofthetheo—
ryofTCMandresearchedbyapplyingtheadvanced modelTlpharmaceuticstechnology.Theresultsfrom morethantenyearsclinicalexperimenthavebeensat—
istiedwitIlitssmallsideeffectandcurativeeffective—
ness.TanshinonelIAisonemaioringredientofRadix SalviaeMihiorrhiaze,Ithasstrongerbiologicalac—
tiont【
,
so,inthispaperthemethodfordetermination oftanshinonelIAinCompoundDangguifukangCap—
sulebyHPLCisreported.
1ApparatusHP1100HPLC,HPRev.A.05.01
I~ttareceived:2004-01-02
Support:TheresearchwassupportedbyShiheziUniversityofNaturalScienceFundCommitt
ee,itemnumber:2001-822574
Biography:WANGXin-ehun(1969
一),female,masterdegree,associatedirectorpharmacist.E-mail:wxc69@sohu.corn.
424
2005年4月
第27卷第4期
中成药
ChineseTraditionalPatentMedicine
April2005
Vo1.27No.4
[273]chemicalworkstation.1314A—uvvariable
wavelengthdetector,electronicscales,inprecisionof oneoftenthousand,modelAE-200(Swiss),ultra—
soniccleaningwashmachine,modelKS-5000(Ning—
bo,China).
ReagentsCompoundDangguifukangCapsule(from TheFirstHospitalAffiliatedtoMedicalCollege,Shihe—
ziUniversity),tanshinonelIA(boughtfromNational InstituteforControlofPharmaceuticalandBiological Product,batchnumber0765-200011andforuseofde—
termination),otherreagentsandsolventswereA.R. grade.
2Experiment
ChromatographicconditionsAnalyticColumn:Re—
liasilC18(5Ixm,250mm×4.6Inln),protectivecol—
umn:(5Ixm,12.50mm×4.6mm);mobilephase:
methanol—water(80:20);detectivewavelengthwasat 270nm;temperaturewasat30.C;theflowratewas 1.0mL?min,:therelativeretentiontimewas17
min;theinjectvolumewas10L.
2.1AssaypreparationGrindthecontentsofnot lessthanCompoundDangguifukangCapsulestoafine powdertopassthrougha40一meshscreen.Transferan
accuratelyweighedportionofthepowder,equivalentto about2.0g.toSoxhletextractor,add50mLofe—
thertoflaskandextractcontinuouslyfor3hinawater bathmaintainedatthetemperatureof50.C.Evapo—
rateethersolutiononawaterbath,controlledatthe temperaturethatwillnotcausetheethersolutiontoboil over,withtheaidofastreamofnitrogen,completethe evaporationremovingthelasttracesofetherwithoutthe applicationofheat,immediatelyswirltodissolvethe residueinsmallportionsmethano1.Transfertoa50
mLvolumetricflask.dilutewithmethanoltovolume, mix.Filterthesolutionthrougha0.45Ixmmicropore filtermembrane,discardingthefirst5mLofthefil—
trate.Pipe1mLofthesubsequentfiltratetoacentri—
fugetube,centrifugeatabout8000rpmfor4min. IIsetheclearsolutionsoobtaiBedasthetestsolution. 2.2BlanksamplepreparationUsethesamees—
tablishedmethodforassaysampletotreatthecapsule withoutRadixSalviaeMihiorrhiage.
2.3Standardcurveoftanshinone1IADissolve anaccuratelyweighedquantityoftanshinonelIA,e—
quivalenttoabout12.5mg,ina25mLbrownvolu—
metricflask.addmethanolandmixtoobtainastock solutionhavingaknownconcetrationofabout0.50mg oftanshinonelIApermL.Separatelyinjectaliquotof 2O,4O,100,150,200,250,300,320IxL,respec—
tively,ofstocksolutionpreparationintoseparate10 mLbrownvolumetricflask,dilutewithmethanolto volume,andmix.Injectequalvolumesoftheprepared solutionintothechromatograph,recordthechromato? grams,andmeasuretheresponsesforthemajorpeaks. Accordingtotherecordedchromatogram.thepeakare—
as(Y)withstatisticaltreatmentasafoundationofthe amount(X)gavethegoodlinearityforweighttanshi—
none11A.intherangof0.01-0.16Ixg.X=O.078Y 一
0.5793.r=0.9995.
2.4PrecisionInjection,continuouslyoneofthe standardsampleandassaysample10IxL,respective?
ly,for5timesandmeasuringthepeakareasofTanshi—
none11A.theRSDofstandardsampleandassays枷一
piewere0.84%and2.12%:
2.5Repeatabilityweighup5portionsofsample (batchnumber.-030315),preparingthetestsolution asdirectedundertheprocedure2.2,theinjectvolume ofsamplein10IxLaccordingtothechromatogramre—
corded.theRSDwas3.O3%.
2.6SolutionstabilityOneofthestandardsamples thatwasplaced,atroomtemperaturefor1,2,3,4,5 h.respectively,wasinjected.rI1hepeakareaswereba? sicallyunchangeableandRSDwas1.62%.indicating thatthesolutionwasstableatleastfor5h. 2.7RecoveryUntreatedcapsulesampleswere mimedtopassthrough40meshscreenandweighted accuratelyup5portionofsample,everyportionwase—
quivalenttoabout1.Og.Separatelyeveryportionof samplehomogenizedwith1.5mLstocksolutionprepa—
ration,thenprocessedaccordingtothe2.2procedure. rI1heresultswereobtainedwithaveragerecovery 99.73%.andRSDwas2.91%(n=5).
2.8FeasibilityofmethodInjectionblanksample. oneofthestandardsamplesandassaysample10IxL, resrectively,asshowninFigure1,nointerferences werefound.
425
2005年4月
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中成药
ChineseI'raditionalPatentMedicine
April2005
V01.27No.4
A
B
Fig.1ItPLCchromatogramsoftanshinonelIA(A)Com- poundI)angeifukangCapsule(B)blanksample(C) 2.9Determinationofsample
Weighup3batchesofsamples,preparingthetest solutionasdirectedundertheprocedure2.2,Sepa- ratelyinjectequalvolumesintothechromatograph,re—
cordthechromatograms,andmeasuretheresponses 426
forthemajorpeaks.Calculatethequantity,inmg,of tanshinoneIIAineachofthecapsule.Themeasured contentswerelistedinrIle1.
Table1Tanshinone?AinCompoundDangulf-nkan~
Capsule(,l=3J
3Discussion
3.1TheselectionofthewavelengthOptimizethe absorbanceofassaypreparationatabout223m,254 nm,270am,determine270nnlasthewavelengthof test,almostwithoutinterferingofothercomponents. 3.2TheelectionofextractingmethodOptimize severaldifferentextractingmethodssuchasultrasonic bath,waterbathataconstanttemperature,and Soxhletextracting,accompanyingwithdifferentextrac—
tingsolventsincludingmethanol,ethanol,amixtureof
methanolandwater,andether,determinetheextrac—
tingmethodaccordingtotherecordedchromatogram, asshowninassaypreparation.
3.3Thereportedmethodissimple,reliabletodeter- minetanshinoneIIAinCompoundDangguifukang
CapsuleandsuitableforthequalitycontrolofCorn—
poundDanguifukangCapsule.
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