在0.2mol·L-1NaOH底液中,酚磺乙胺的氧化产物能够在示波图阴极支-0.3V处产生一个灵敏的切口,在一定的浓度范围内其二次微分简易示波伏安峰峰高随酚磺乙胺浓度的增大而线性增加,可用于酚磺乙胺片和注射液酚磺乙胺含量的测定.线性范围1.5×10-5～3.4×10-4mol·L-1,回归方程:h(V)=135.6+3.29×106C(mol·L-1),r=0.9921,检出限:6.0×10-6mol·L-1.对3.0×10-5mol·L-1酚磺乙胺5次测定的RSD为2.1%.与高效液相色谱及其他方法相比,本方法具有仪器简单、简便快速、无需通氮除氧等特点.
In 0.2 mol L~(-1) NaOH solution, ethamsylate can yield a sensitive incision on cathodic branch of dE/dt-E osillogram at 0.3V (vs. SCE). Based on the oscillographic characteristic, a second order differential simple oscillographic voltammetry for determination of ethamsylate in tablet and injection is presented in this paper. The peak height on second order differential simple oscillographic voltammogram is linearly proportional to concentration of the ethamsylate in the range of 1.5×10~(-5)～3.4×10~(-4) mol·L~(-1 )with a 0.9921 correlation coefficient and a detection limit of 6.0×10~(-6 )mol·L~(-1 ) for ethamsylate. The relative standard deviation is 2.1% for the determination of 3.0 10~(-5) mol L~(-1) ethamsylate (n=5). Compared with HPLC and other methods, the second order differential simple oscillographic voltammetry is a convenient method due to its cheap equipment and rapid measurement.
[1]Editorialcommitteeofpharmacopeiaoftheministryof healthofChina(中华人民共和国卫生部药典委员会).PharmacopeiaofChina:PartⅡ[M].Beijing:ChemicalIndustryPress,1995.788.
[2]XuZC(许自超),LiXH(李晓晔),ShiJ(施炯),et al.Thespectrometricdeterminationofethamsylateinstomachtissueofrabbit[J].ChineseJournalofAna lyticalChemistry,1994,22(4):420.
[3]MaJW(马剑文),LIUYB(刘玉波).HPLCanalysis ofethamsylate[J].ChinesejournalofPharm.Anal.,1984,4(4):209～212.
[4]YangGJ(杨功俊),JinLT(金通利),LengZZ(冷宗周).Determinationofmicroscaleethamsylateoncar bonpasteelectrodewithadsorptivevoltammetry[J].ChinesejournalofPharm.Anal.,1998,18(5):311～313.
[5]WangZH(汪振辉),ZhangD(张岱),ZhangY(张岩),etal.Voltammetricbehaviorofdicynonumatpoly(4aminopyridine)filmmodifiedelectrodeanditsdeter minationbyadsorptivestrippingvoltammetry[J].Chi neseJournalofAnalyticalChemistry,2001,29(1):83～86.
[6]HunX(混旭),YangWP(杨维平),ZhangZJ(章竹君).Anovelaerodynamicforcecapillarymicrodrop in jectiondeterminationofethamsylatewithchemilumines cence[J].ChemicalJournalofChineseUniversities,2004,25(2):264～266.
[7]LiYH(李银环),DuJX(杜建修),LvJR(吕九如).Chemiluminescencereactionofluminal[potassi umferricyanide potassiumferrocyanide]ethamsylate system[J].ChineseJournalofAnalyticalChemistry,2002,30(6):742～744.
[8]YangFZ,ZhangC,WillyRGB,etal.Determination ofethamsylateinpharmaceuticalpreparationsbasedon anauto oxidationchemiluminescencereaction[J].J.PharmaceuticalandBiomedicalAnalysis,2002,30:473～478.
[9]ZhengJB,ZhangXQ,GaoM,etal.Astudyona Multi orderSemidifferentialOscillographicChronopoten tiometricInstrument[J].InstrumentationScience&Technology,2000,28(5):403～412.
[10]ZhengJB(郑建斌),GaoH(高鸿).Theadjustingof oscillograminoscillographicdetermination[J].Jour nalofNorthwestUniversity(NaturalScienceEdition),1995,25(4):309～314.
[11]ZhengJB(郑建斌),FuYW(高鸿),LiY(李媛),etal.Investigationof3.5thorderdifferentialcyclicos cillochronopotentiometry[J].ChemicalJournalof ChineseUniversities,1998,19(3):368～371.
[12]GaoH(高鸿).OscillographicMedicalAnalysis[M].Chengdu:SichuanEducationPress.1992,263.
