simultaneous determination of lafutidine and domperidone in ... - IJPI
simultaneous determination of lafutidine and domperidone in ... - IJPI
simultaneous determination of lafutidine and domperidone in ... - IJPI
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INTERNATIONAL JOURNAL OFRESEARCH ARTICLEPHARMACEUTICAL INNOVATIONS ISSN 2249-1031SIMULTANEOUS DETERMINATION OF LAFUTIDINE ANDDOMPERIDONE IN TABLET DOSAGE FORM BY HPLCRay Chaudhury Dipanjan*, Chakraborty Mithun, Chakraborty Susanto, Saha N<strong>and</strong>itaCentral Drugs Laboratory, Govt. <strong>of</strong> India, 3 Kyd Street, Kolkata-700016Abstract:A simple, precise <strong>and</strong> rapid isocratic reverse phase high performance liquid chromatographicmethod was developed for the <strong>simultaneous</strong> <strong>determ<strong>in</strong>ation</strong> <strong>of</strong> Lafutid<strong>in</strong>e <strong>and</strong> Domperidone <strong>in</strong>tablet dosage form. The chromatographic separation was performed on µ-Bondapack C18column (250 mm × 4.6 mm I.D. 5 µm particle size). Mobile phase consisted <strong>of</strong> a mixture <strong>of</strong>phosphate buffer <strong>of</strong> pH 7.0 <strong>and</strong> acetonitrile <strong>in</strong> the ratio <strong>of</strong> 60: 40 at a flow rate <strong>of</strong> 1.5 mL/m<strong>in</strong><strong>and</strong> with the detection wavelength <strong>of</strong> 220 nm. The proposed method was validated for l<strong>in</strong>earity,accuracy, precision, robustness LOD <strong>and</strong> LOQ. The calibration curve was l<strong>in</strong>ear over the range<strong>of</strong> 20-80 µg/mL for Lafutid<strong>in</strong>e <strong>and</strong> 60-240 µg/mL for Domperidone. The retention times werefound as 4.8 m<strong>in</strong> for Domperidone <strong>and</strong> 6.1 m<strong>in</strong> for Lafutid<strong>in</strong>e. The method can be easilyadopted for rout<strong>in</strong>e analysis <strong>of</strong> the same type <strong>of</strong> comb<strong>in</strong>ation products.Keywords: Lafutid<strong>in</strong>e, Domperidone, RP-HPLC, ValidationIntroductionLafutid<strong>in</strong>e (LAF) is 2-(furan-2-ylmethylsulf<strong>in</strong>yl)-N [4-[4-(piperid<strong>in</strong>-1-ylmethyl) pyrid<strong>in</strong>-2-yl] oxybut-amide [1](structure <strong>in</strong> Fig 1a). It belongs to the class<strong>of</strong> H 2 receptor antagonists. Used <strong>in</strong> thetreatment <strong>of</strong> peptic ulcer <strong>and</strong> gastrooesophagealreflux disease (GERD) [1]. Itis freely soluble <strong>in</strong> methanol, whereas it ispractically <strong>in</strong>soluble <strong>in</strong> water. It is asecond generation histam<strong>in</strong>e H 2 -receptorantagonist used as an antiulcerative agent[2]. Structures are shown <strong>in</strong> fig 1a. This isan antisecretory drug. Antisecretory drugsare used <strong>in</strong> the treatment <strong>and</strong> prophylaxis<strong>of</strong> peptic ulcer disease some are alsoemployed <strong>in</strong> other disorders associatedwith gastric hyperacidity such as gastro-oesophageal reflux disease <strong>and</strong> dyspepsia.They may be divided <strong>in</strong>to Histam<strong>in</strong>e H2-receptor antagonist (H2-antagonists),which act by block<strong>in</strong>g histam<strong>in</strong>e H2-receptors on gastric parietal cells, therebyantagoniz<strong>in</strong>g the normal stimulatory effect<strong>of</strong> endogenous histam<strong>in</strong>e on gastric acidproduction. Literature survey reveals thatmany methods are reported for itsestimation alone <strong>in</strong> biological fluids byt<strong>and</strong>em mass spectrometry [3-5] <strong>and</strong> chiralseparations by HPLC <strong>and</strong> LC-MS [6].Domperidone (DOM) chemicallyCorrespond<strong>in</strong>g Author*Ray Chaudhury DipanjanVolume 2, Issue 6, Nov. − Dec. 20121 | P a g ehttp://www.ijpi.org
INTERNATIONAL JOURNAL OFRESEARCH ARTICLEPHARMACEUTICAL INNOVATIONS ISSN 2249-1031(5-chloro-1-{1-[3(2,3-dihydro-2-oxo-1Hbenzimidazol-1-yl)propyl] -4-piperid<strong>in</strong>yl} benzimidazol<strong>in</strong>-2-one)(Structure <strong>in</strong> Figure 1b) used as anantiemetic drug [7,8]. It stimulates gastro<strong>in</strong>test<strong>in</strong>almotility an disused as anantiemetic forth short term treat men t <strong>of</strong>nausea <strong>and</strong> vomit<strong>in</strong>g.A comb<strong>in</strong>ation <strong>of</strong> these drugs, DOM <strong>and</strong>LAF is available as tablets for cl<strong>in</strong>icalpractice. This unique comb<strong>in</strong>ation hascomprehensive acid control <strong>and</strong> prok<strong>in</strong>eticaction which ensures better control <strong>and</strong>relief from reflux, gastric ulcers, <strong>and</strong>associated gastro<strong>in</strong>test<strong>in</strong>al (GIT) disorders.Many methods like HPLC [9],[10],HPTLC [11], <strong>and</strong> LCMS [12] have beendescribed <strong>in</strong> the literature for the<strong>determ<strong>in</strong>ation</strong> <strong>of</strong> DOM <strong>and</strong> LAF<strong>in</strong>dividually or <strong>in</strong> comb<strong>in</strong>ation with others.aim <strong>of</strong> present work is to develop <strong>and</strong>validate the rapid <strong>and</strong> sensitive highperformance liquid chromatography(HPLC) method for <strong>simultaneous</strong><strong>determ<strong>in</strong>ation</strong> <strong>of</strong> Lafutid<strong>in</strong>e <strong>and</strong>Domperidone <strong>in</strong> tablets.Experimental:Instrumentation:HPLC (Agilent 1200 series) equipped withQuaternary pump, Auto sampler, UltravioletDetector <strong>and</strong> EZ-Chrome EliteS<strong>of</strong>tware. Waters Spherisorb ODS2 (4.0 x250 mm, 5 µm) column was used.Chemicals <strong>and</strong> ReagentsThe solvents used were <strong>of</strong> Mili-Q water(18.2 MΩ-cm conductivity) forpreparation <strong>of</strong> buffer <strong>of</strong> mobile phase,HPLC grade Acetonitrile <strong>and</strong> Orthophosphoricacid (AR-Grade). ReagentPotassium-di-hydrogen phosphate (ARgrade)was used for preparation <strong>of</strong> buffer.Lafutid<strong>in</strong>e (Potency: 99.85% as such) <strong>and</strong>Domperidone (Potency: 99.1% as such)reference st<strong>and</strong>ard <strong>of</strong> a renowned companywere used <strong>and</strong> samples was obta<strong>in</strong>edfrom market.Fig 1a: Structure <strong>of</strong> Lafutid<strong>in</strong>eFig 1b: Structure <strong>of</strong> DomperidoneAccord<strong>in</strong>g to literature study, so manyanalytical methods are reported viz. UVspectrophotometry[13-16], HPLC [17-18]<strong>and</strong> drugs <strong>in</strong> human plasma [19- 21]. TheVolume 2, Issue 6, Nov. − Dec. 2012Chromatographic ConditionsWhile several mobile phases were tried,the mobile phase conta<strong>in</strong><strong>in</strong>g buffer (0.01M KH 2 PO 4 , pH adjusted to 7.0 us<strong>in</strong>g diluteorthophosphoric acid) <strong>and</strong> acetonitrile <strong>in</strong>the ratio <strong>of</strong> 60: 40 was used. The mobilephase was filtered through 0.45µmmembrane filter <strong>and</strong> sonicated for 10m<strong>in</strong>utes. After several trials flow rate wasfixed at 1.5 ml/m<strong>in</strong>, column temperature at30 degree-C <strong>and</strong> <strong>in</strong>jection volume 20 µl.The proposed method was validated forl<strong>in</strong>earity, accuracy, precision, LOD <strong>and</strong>2 | P a g ehttp://www.ijpi.org
INTERNATIONAL JOURNAL OFRESEARCH ARTICLEPHARMACEUTICAL INNOVATIONS ISSN 2249-1031LOQ. The calibration was l<strong>in</strong>ear over therange <strong>of</strong> 20-80 µg/mL for Lafutid<strong>in</strong>e <strong>and</strong>60-240 µg/mL for Domperidone. Theretention times were found as 4.8 m<strong>in</strong> forDomperidone <strong>and</strong> 6.1 m<strong>in</strong> for Lafutid<strong>in</strong>e.The method can be easily adopted forregular rout<strong>in</strong>e analysis.Preparations <strong>of</strong> St<strong>and</strong>ard Solutions:Weigh accurately about 10.1 mg <strong>of</strong> LAF<strong>and</strong> 30.4 mg <strong>of</strong> DOM work<strong>in</strong>g st<strong>and</strong>ards<strong>in</strong>to 100 ml volumetric flask. Dissolve <strong>in</strong>methanol, sonicate for 15 m<strong>in</strong>utes <strong>and</strong>make up the volume <strong>in</strong> methanol. Dilute 5ml <strong>of</strong> this stock solution <strong>in</strong> to 10 mlvolumetric flask with Methanol. Theconcentration <strong>of</strong> LAF is about 50.3 µg/ ml<strong>and</strong> DOM is about 150 µg/ ml.Preparations <strong>of</strong> Sample SolutionsTake the weight <strong>of</strong> 20 tablets; take about500 mg powdered, equivalent to about 10mg LAF <strong>and</strong> 30 mg DOM <strong>in</strong> a 100 mlvolumetric flask. Add about 60 ml <strong>of</strong>Methanol, sonicate for 30 m<strong>in</strong>utes <strong>and</strong>dilute up to the mark with Methanol.Filter <strong>and</strong> discard first few ml <strong>and</strong> use thisfiltered as sample solution. Dilute 5 ml <strong>of</strong>this stock solution <strong>in</strong> to 10 ml volumetricflask with Methanol. The concentration <strong>of</strong>LAF is about 50 µg/ ml <strong>and</strong> DOM is about300 µg/ ml.Method ValidationThe method was validated for l<strong>in</strong>earity,precision <strong>and</strong> repeatability, accuracy <strong>and</strong>robustness.Result <strong>and</strong> discussionL<strong>in</strong>earity <strong>of</strong> Lafutid<strong>in</strong>e <strong>and</strong>DomperidoneTo prepare the calibration curve forLafutid<strong>in</strong>e a stock solution <strong>of</strong> Lafutid<strong>in</strong>e <strong>of</strong>conc. about 1mg/ml was prepared. From itVolume 2, Issue 6, Nov. − Dec. 20121.0, 1.5, 2.0, 2.5, 3.0, 3.5 <strong>and</strong> 4 ml <strong>of</strong>st<strong>and</strong>ard stock solution <strong>of</strong> LAF wastransferred to a series <strong>of</strong> seven <strong>in</strong>dividual10 ml volumetric flasks. The volume <strong>of</strong>each flask was adjusted to 10 ml withMethanol. (Table-1). Similarly a stocksolution <strong>of</strong> concentration <strong>of</strong> 1 mg/mlDomperidone was prepared <strong>in</strong> methanol.Form it takes, 0.6, 0.9, 1.2, 1.5, 1.8, 2.1<strong>and</strong> 2.4 ml solution was transferred to each10 ml volumetric flasks. The volume <strong>of</strong>each flask was adjusted to 10 ml withMethanol. (Table-2). Detection responsefor each LAF <strong>and</strong> DOM were found to bel<strong>in</strong>ear <strong>in</strong> concentration range <strong>of</strong> 20.0 – 80.0mcg/ml <strong>and</strong> 60 – 140 mcg/ml ( fig-1 ,fig-2).The slope, regression equation <strong>and</strong>coefficient <strong>of</strong> correlation for DOM <strong>and</strong>LAF were found to be y = 67859 x +28173, R 2 = 0.999 <strong>and</strong> y = 76331x +12902, R 2 = 0.999.PRECISIONa) System precision for LAF <strong>and</strong> DOM:The system precision was evaluated bymeasur<strong>in</strong>g the peak response <strong>of</strong> LAF <strong>and</strong>DOM for six replicate <strong>in</strong>jections <strong>of</strong>st<strong>and</strong>ard solutions, prepared as theproposed method. The result shown <strong>in</strong> theTable- 3 <strong>in</strong>dicates that the precision <strong>of</strong> thesystem is with<strong>in</strong> acceptance criteria( i.e.RSD not more than 2%).b) Method precision LAF <strong>and</strong> DOM:The method precision was determ<strong>in</strong>ed byprepar<strong>in</strong>g a sample solution <strong>of</strong> a s<strong>in</strong>glebatch LAF <strong>and</strong> DOM tablets six times <strong>and</strong>analyz<strong>in</strong>g as per the proposed method. Theresult shown <strong>in</strong> Table- 4 <strong>in</strong>dicates that theproposed method is precise. (Acceptancecriteria: % RSD not more than 2%).3 | P a g ehttp://www.ijpi.org
INTERNATIONAL JOURNAL OFRESEARCH ARTICLEPHARMACEUTICAL INNOVATIONS ISSN 2249-1031A representative chromatogram <strong>of</strong> mixedst<strong>and</strong>ard solution <strong>of</strong> LAF (mcg/ml) <strong>and</strong>DOM (mcg/ml) are shown <strong>in</strong> figure-3.ACCURACY (recovery study) for LAF<strong>and</strong> DOM:Known amount <strong>of</strong> LAF <strong>and</strong> DOM werespiked to placebo at 80%, 100% <strong>and</strong> 120%<strong>of</strong> specification <strong>in</strong> triplicate <strong>and</strong> analyzedas per the proposed method to determ<strong>in</strong>ethe accuracy <strong>of</strong> the method. Percentage <strong>of</strong>recovery was calculated from the amountfound <strong>and</strong> amount added. The results areshown <strong>in</strong> Table- 5 & 6. The percentagerecovery is with<strong>in</strong> the acceptance criteria,which <strong>in</strong>dicates the accuracy <strong>of</strong> themethod.(Acceptancecriteria: % recovery between 98 to 102).Limit <strong>of</strong> detection (LOD):The limit <strong>of</strong> detection (LOD) is thesmallest concentration that can be detectedbut not necessarily quantified as an exactvalue. LOD can be calculated as:LOD = 3.3 σ / SWhere,σ = St<strong>and</strong>ard deviation <strong>of</strong> the response[22]S= Slope <strong>of</strong> the calibration curveLimit <strong>of</strong> quantitation (LOQ):The limit <strong>of</strong> quantitation (LOQ) is thelowest amount <strong>of</strong> analyze <strong>in</strong> the samplethat can be quantitatively determ<strong>in</strong>ed withsuitable precision <strong>and</strong> accuracy. LOQ canbe calculated as:LOQ = 10 σ / SWhere,Volume 2, Issue 6, Nov. − Dec. 2012σ = St<strong>and</strong>ard deviation <strong>of</strong> the responseS= Slope <strong>of</strong> the calibration curveThe limit <strong>of</strong> detection (LOD) was found tobe 16.46 mcg/ml for LAF <strong>and</strong> 15.09mcg/ml for DOM whereas the limit <strong>of</strong>quantitation (LOQ) was found to be 49.89mcg/ml for LAF <strong>and</strong> 45.73 mcg/ml forDOM respectively.RobustnessThe robustness <strong>of</strong> a method is its ability torema<strong>in</strong> unaffected by small deliberatechange <strong>in</strong> parameter. To evaluate therobustness, the developed method wassubjected to small deliberate variation <strong>in</strong>the optimized method parameters likevariation <strong>of</strong> flow rate 1.5 ± 0.2 ml/m<strong>in</strong>,detection wavelength i.e. 220 ± 2.0 nm<strong>and</strong> pH 7.0 ± 0.2 <strong>in</strong> the buffer <strong>of</strong> mobilephase.The mixed st<strong>and</strong>ard solution conta<strong>in</strong><strong>in</strong>g150 mcg/ml <strong>of</strong> DOM <strong>and</strong> 50.3 mcg/ml <strong>of</strong>LAF was <strong>in</strong>jected <strong>in</strong> replicate at variedchromatographic condition <strong>and</strong> thest<strong>and</strong>ard deviation <strong>of</strong> the retention time <strong>of</strong>each analyte were calculated. The methodwas found to be robust as the slightdeliberate variations <strong>in</strong> detectionwavelength <strong>and</strong> flow rate did not lead tochanges <strong>in</strong> retention time <strong>of</strong> the peaks <strong>of</strong><strong>in</strong>terest. While evaluat<strong>in</strong>g the robustnessdata it was observed that system suitabilityparameters (e.g. tail<strong>in</strong>g factor, plate count,resolution etc.) were found to be with<strong>in</strong> thespecified limit under those deliberatelyvaried conditions, which ensures that thevalidity <strong>of</strong> the analytical procedure wasma<strong>in</strong>ta<strong>in</strong>ed whenever used. The result <strong>of</strong>robustness studies is summarized <strong>in</strong> table7.System Suitability4 | P a g ehttp://www.ijpi.org
INTERNATIONAL JOURNAL OFRESEARCH ARTICLEPHARMACEUTICAL INNOVATIONS ISSN 2249-1031System suitability test<strong>in</strong>g is used to verifythat the resolution <strong>and</strong> reproducibility <strong>of</strong>the system are adequate for the analysis tobe performed. System suitability wasassessed by <strong>in</strong>ject<strong>in</strong>g DOM <strong>and</strong> LAFmixed st<strong>and</strong>ard preparation <strong>in</strong> replicate.Parameter such as theoretical plate, tail<strong>in</strong>gfactor, resolution were determ<strong>in</strong>ed. Thesystem suitability parameters for themethod are listed <strong>in</strong> table-8.Conclusions:The developed method is better thanprevious methods <strong>and</strong> valid for capsule<strong>and</strong> tablet dosage also. The mobile phase issimple to prepare. The developed methodfulfilled all the requirements <strong>in</strong>clud<strong>in</strong>gaccuracy, l<strong>in</strong>earity, recovery <strong>and</strong> precisiondata. Therefore the RP-HPLC methodfound to be simple, accurate, economical,<strong>and</strong> rapid <strong>and</strong> can be used as a rout<strong>in</strong>esample analysis.Acknowledgement:The authors express their gratitude to theDirector, Central Drugs Laboratory,Kolkata <strong>and</strong> all the staff member <strong>of</strong>Central Instrument Room <strong>of</strong> Central DrugsLaboratory, Kolkata for provid<strong>in</strong>gnecessary facilities <strong>in</strong> the department.References:1. The Merck Index - Anencyclopedia <strong>of</strong> chemicals,drugs <strong>and</strong> biologicals,published by Merck ResearchLaboratories, 14th edition,Lafutid<strong>in</strong>e, (5347), 9262. Y.Akiba<strong>and</strong>J.D.Kaunitz,“Lafutid<strong>in</strong>e, aprotective H2 receptorantagonist, enhances mucosaldefense <strong>in</strong> ratesophagus,”DigestiveDiseasesaVolume 2, Issue 6, Nov. − Dec. 2012ndSciences,vol.55, no. 11, pp.3063–3069, 2010.3. Dong Chen, W., Y. Liang, H.Li, Y. Xiong, X. Dong Liu, G.Ji Wang <strong>and</strong> L. Xie, 2006.Simple, sensitive <strong>and</strong> rapid LC-ESI-MS method for thequantitation <strong>of</strong> <strong>lafutid<strong>in</strong>e</strong> <strong>in</strong>human plasma-Application topharmacok<strong>in</strong>etic studies. J.Pharmaceutical <strong>and</strong> BiomedicalAnalysis, 41(1): 256-260.4. Wu, L., Z. Zhang, Y. Tian, W.Li, F. Xu, Y. Chen <strong>and</strong> H. Wei,2005. Determ<strong>in</strong>ation <strong>of</strong><strong>lafutid<strong>in</strong>e</strong> <strong>in</strong> human plasma byhigh-performance liquidchromatographyelectrosprayionization mass spectrometry:application to a bioequivalencestudy. J. Mass Spectrometry,40(12): 1637-1643.5. Sun, X., Y. Tian, Z. Zhang <strong>and</strong>Y. Chen, 2009. A s<strong>in</strong>gle LCt<strong>and</strong>emmass spectrometrymethod for the <strong>simultaneous</strong><strong>determ<strong>in</strong>ation</strong> <strong>of</strong> four H2antagonists <strong>in</strong> human plasma. J.Chromatography B,877(31):3953-3959.6. Xiu Pan, C., X. Zhu Xu, H. MeiHe, X. Jun Cai <strong>and</strong> X. JunZhang, 2005. Separation <strong>and</strong>identification <strong>of</strong> cis <strong>and</strong> transisomers <strong>of</strong> 2-butene-1,4-diol<strong>and</strong> <strong>lafutid<strong>in</strong>e</strong> by HPLC <strong>and</strong>LC-MS. J. Zhejiang UniversityScience B., 6(1): 74-78.7. L. Swann, E. N. Thompson,<strong>and</strong> K. Qureshi, “Domperidoneor metoclopramide <strong>in</strong>5 | P a g ehttp://www.ijpi.org
INTERNATIONAL JOURNAL OFRESEARCH ARTICLEPHARMACEUTICAL INNOVATIONS ISSN 2249-1031prevent<strong>in</strong>gchemotherapeutically <strong>in</strong>ducednausea <strong>and</strong> vomit<strong>in</strong>g,” BMJ,vol. 2, no. 6199, article 118,1979.8. Karthik, G. Subramanian, A.Ranjith Kumar, <strong>and</strong> N.Udupa,“Simultaneousestimation <strong>of</strong> paracetamol <strong>and</strong><strong>domperidone</strong> <strong>in</strong> tablets byreverse phase HPLC method,”Indian Journal <strong>of</strong>PharmaceuticalSciences, vol.69, no. 1, pp. 142–144, 2007.9. Karthik, G. Subramanian, A.Ranjith Kumar, <strong>and</strong> N.Udupa,“Simultaneousestimation <strong>of</strong> paracetamol <strong>and</strong><strong>domperidone</strong> <strong>in</strong> tablets byreverse phase HPLC method,”Indian Journal <strong>of</strong>Pharmaceutical Sciences,vol.69, no. 1, pp. 142–144, 2007.10. M. Kobyli´nska <strong>and</strong> K.Kobyli´nska, “Highperformanceliquidchromatographic analysis forthe <strong>determ<strong>in</strong>ation</strong> <strong>of</strong>Domperidone <strong>in</strong> humanplasma,” Journal <strong>of</strong>Chromatography B, vol.744,no. 1, pp. 207–212, 2000.11. B.H.Patel, B.N.Suhagia,M.M.Patel<strong>and</strong>J.R.Patel,“HPTLC<strong>determ<strong>in</strong>ation</strong> <strong>of</strong> rabeprazole<strong>and</strong> Domperidone <strong>in</strong> capsules<strong>and</strong> its validation,” Journal <strong>of</strong>Chromatographic Science, vol.46, no.4, pp. 304–307, 2008.Volume 2, Issue 6, Nov. − Dec. 201212. C.X.Pan,X.Z.Xu,H.M.He,X.J.Cai,<strong>and</strong>X.J.Zhang, “Separation<strong>and</strong> identification <strong>of</strong> cis <strong>and</strong>trans isomers <strong>of</strong> 2butene-1,4-diol <strong>and</strong> <strong>lafutid<strong>in</strong>e</strong> by HPLC<strong>and</strong> LC-MS,”PharmaceuticalJournal, vol. 6, 2003.13. Salem, M.Y., E.S. El Zanfaly,M.F. El Tarras <strong>and</strong> M.G. ElBardicy, 2003. Simultaneous<strong>determ<strong>in</strong>ation</strong> <strong>of</strong> <strong>domperidone</strong><strong>and</strong> c<strong>in</strong>nariz<strong>in</strong>e <strong>in</strong> a b<strong>in</strong>arymixture us<strong>in</strong>g derivativespectrophotometry, partial leastsquares <strong>and</strong> pr<strong>in</strong>ciplecomponent regressioncalibration. Analytical <strong>and</strong>Bioanalytical Chemistry,375(2): 211-216.14. Ravi kumar, P., P. BhanuPrakash, M. Murali Krishna,M.Santha Yadav <strong>and</strong> C. Ashadeepthie, 2006.SimultaneousEstimation <strong>of</strong> Domperidone<strong>and</strong> Pantoprazole <strong>in</strong> SolidDosage Form by UVSpectrophotometry. E-Journal<strong>of</strong> Chemistry, 3(12): 142-145.15. Ramesh, S., B. Lokesh, J.Rupali <strong>and</strong> L. Prashant, 2010Validated spectrophotometricmethods for <strong>simultaneous</strong>estimation<strong>of</strong>Paracetamol,Domperidone <strong>and</strong>Tramadol HCl <strong>in</strong> pure <strong>and</strong>tablet dosage form, J. ChemicalMetrol., 4(1): 21-27.16. Sherje, A.P., A.V. Kasture,K.N. Gujar <strong>and</strong> P.G. Yeole,2008. SimultaneousSpectrophotometric6 | P a g ehttp://www.ijpi.org
INTERNATIONAL JOURNAL OFRESEARCH ARTICLEPHARMACEUTICAL INNOVATIONS ISSN 2249-1031<strong>determ<strong>in</strong>ation</strong> <strong>of</strong> Lansoprazole<strong>and</strong> Domperidone <strong>in</strong> capsuledosage form. Indian J.Pharmaceutical Sci., 70(1):102-105.17. Patel, B.H., B.N. Suhagia,M.M. Patel <strong>and</strong> J.R. Patel,2007. Simultaneous estimation<strong>of</strong> pantoprazole <strong>and</strong><strong>domperidone</strong> <strong>in</strong> pure powder<strong>and</strong> a pharmaceuticalformulation by highperfomanceliquidchromatography <strong>and</strong>high-performance th<strong>in</strong>-layerchromatography methods. J.AOAC International,18. Michaud, V., C. Simard <strong>and</strong> J.Turgeon, 2007. AnimprovedHPLC assay with fluorescencedetection for the <strong>determ<strong>in</strong>ation</strong><strong>of</strong> <strong>domperidone</strong> <strong>and</strong> threemajor metabolites forapplication to <strong>in</strong> vitro drugmetabolism studies, J.Chromatography B,AnalyticalTechnologies <strong>in</strong> Biomedical<strong>and</strong> Life Sci.,852(1-2): 611-616.19. Imran, A., V.K. Gupta, S.Prashanth <strong>and</strong> H.V. Pant, 2006.Screen<strong>in</strong>g <strong>of</strong> <strong>domperidone</strong> <strong>in</strong>wastewater by highperformanceliquidchromatography <strong>and</strong> solidphase extraction methods,Talanta, 68(3): 928-931.20. Dong Hang, X., L. Hong Gang,Y. Hong, B. Jiang, Q. Zhou, Z.Miao Zhang <strong>and</strong> Z. Rong Ruan,2008. Quantitative<strong>determ<strong>in</strong>ation</strong> <strong>of</strong> <strong>domperidone</strong><strong>in</strong> human plasma by ultraperformanceliquidchromatography with electrospray ionization t<strong>and</strong>em massspectrometry, BiomedicalChromatography,22(4): 433-440.21. Smit, M.J., F.C.W. Sutherl<strong>and</strong>,H.K.L. Hundt, K.J. Swart, A.F.Hundt <strong>and</strong> J. Els, 2002. Rapid<strong>and</strong> sensitive liquidchromatography-t<strong>and</strong>em massspectrometry method for thequantitation <strong>of</strong> <strong>domperidone</strong> <strong>in</strong>human plasma, Journal <strong>of</strong>Chromatography A., 949(1-2):65-70.22. Vogel’s Textbook <strong>of</strong>Quantitative ChemicalAnalysis, 6 th edition, 163-165.Volume 2, Issue 6, Nov. − Dec. 20127 | P a g ehttp://www.ijpi.org
VoltsDiluent1.547Domperidone4.867Lafutid<strong>in</strong>e6.120VoltsINTERNATIONAL JOURNAL OFRESEARCH ARTICLEPHARMACEUTICAL INNOVATIONS ISSN 2249-10312000000015000000y = 67859x + 28173R² = 0.99910000000500000000 50 100 150 200 250Fig -1: L<strong>in</strong>earity study <strong>of</strong> Domperidone70000006000000500000040000003000000200000010000000y = 76331x + 12902R² = 0.9990.000 20.000 40.000 60.000 80.000 100.000Fig 2: L<strong>in</strong>earity study <strong>of</strong> Lafutid<strong>in</strong>e500500400400300300200200100100000 1 2 3 4 5 6 7 8 9 10M<strong>in</strong>utesFig 3: The representative chromatogram for mixed st<strong>and</strong>ard <strong>of</strong> Domperidone <strong>and</strong>Lafutid<strong>in</strong>eVolume 2, Issue 6, Nov. − Dec. 20128 | P a g ehttp://www.ijpi.org
INTERNATIONAL JOURNAL OFRESEARCH ARTICLEPHARMACEUTICAL INNOVATIONS ISSN 2249-1031Table – 3:System precision for Lafutid<strong>in</strong>e <strong>and</strong> DomperidoneInjection No RT <strong>of</strong> DOM Area <strong>of</strong> DOM RT <strong>of</strong> LAF Area <strong>of</strong> LAF1 4.867 9610163 6.12 38796562 4.867 9678066 6.127 39105193 4.867 9721358 6.127 39167494 4.867 9701590 6.133 39048005 4.86 9701318 6.127 39160226 4.852 9701236 6.123 3915893Average 9685621.8 3907273STD0.003 39429.314 0.005 14282.82DEVIATION% RSD 0.45 0.39Table – 4: Method precession for DOM <strong>and</strong> LAFUAssay ResultsLafutid<strong>in</strong>eDomperidoneFound/Tab %Found Found/Tab %FoundSET1 29.670 98.901 9.925 99.254SET2 29.871 99.571 10.032 100.319SET3 30.363 101.211 10.062 100.621SET4 29.587 98.623 9.987 99.870SET5 29.930 99.767 10.012 100.120SET6 29.980 99.933 10.010 100.100Average Found 29.9 99.67 10.00 100.05(mg) =%RSD = 0.91 0.91 0.46 0.46Table – 5: Recovery study <strong>of</strong> Lafutid<strong>in</strong>eLevel <strong>of</strong> st<strong>and</strong>ardLafutid<strong>in</strong>eadded added sample added std Recovered %wt. (mg) wt. (mg) mg recovery80% 34.91 26.6 26.746 100.55100% 34.17 32.16 31.884 99.14120% 33.63 39.31 39.606 100.75Volume 2, Issue 6, Nov. − Dec. 201210 | P a g ehttp://www.ijpi.org
INTERNATIONAL JOURNAL OFRESEARCH ARTICLEPHARMACEUTICAL INNOVATIONS ISSN 2249-1031Table – 6: Recovery study <strong>of</strong> DomperidoneLevel <strong>of</strong> st<strong>and</strong>ardDomperidoneadded added sample added std Recovered % <strong>of</strong>wt. (mg) wt. (mg) mg recovery80% 26.85 20.29 20.629 101.67100% 26.28 25.37 25.524 100.61120% 25.87 30.24 29.901 98.88Table- 7 Robustness Data <strong>in</strong> terms <strong>of</strong> Retention Time for Lafutid<strong>in</strong>e <strong>and</strong> DomperidoneLevel Wave Length a* Flow Rate b* pH c*DOM LAFU DOM LAFU DOM LAFU- 4.835±0.066.125±0.0234.835±0.0026.125±0.0134.835± 0.02 6.125±0.033330 4835 6.125 4.835 6.125 4.835 6.125+ 4.835 ±0.0276.125 ±0.0354.835 ±0.0476.125±0.0054.835 ± 0.04 6.125±0.015a* Wavelength 220± 2 nm, b* Flow Rate 1.5 ± 0.2 ml/m<strong>in</strong>, c* pH 7.0±0.2Table- 8: System Suitability parametersParameterResults for Results for Lafutid<strong>in</strong>eDomperidoneCalibration Range (mcg/ml) 60-240 20 – 80Retention Time (m<strong>in</strong>) 4.835 6.125Theoretical Plate / meter 8245 5429Tail<strong>in</strong>g factor 0.965 0.983Resolution 3.34 ---LOD (mcg/ml) 15.09 16.46LOQ (mcg/ml) 45.73 49.89Volume 2, Issue 6, Nov. − Dec. 201211 | P a g ehttp://www.ijpi.org