High-Performance Liquid Chromatography of two Peripheral Vasodilators, Nylidrin Hydrochloride and Isoxsuprine Hydrochloride, in Pharmaceutical Dosage Forms

Volpe, Frank; Zintel, J. A.; Spiegel, Donald

doi:10.1002/jps.2600681018

Cited by 18 publications

(3 citation statements)

References 2 publications

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“…The major degradationp roducts of ISX.H Cl are: 4-hydroxybenzaldehyde, phydroxyacetophenone, 4-hydroxybenzyl alcohol, and p-hydroxybenzoica cid [ 27] did not interfere with the determination of ISX by the proposed method, since the main reaction depends on the presence of secondarya liphatica mine. So, the proposed method proved to be specific for intact molecule in the presence of its degradation products .H encet he proposed method can be considered as stability indicating assay for the determination of ISX in the presence of its degradation products.…”

Section: Specificity Of the Proposed Methodsmentioning

confidence: 90%

Kinetic Spectrophotometric Determination of Isoxsuprine in Dosage Forms Through Derivatisation with 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl)

2006

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As imple and sensitivek inetic spectrophotometric method was developedf or the determinationo fi soxsuprine in pharmaceutical preparations.T he method is basedupon akinetic investigationofthe coupling reaction between isoxsuprine HCl and4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) in borate buffer of pH 7.8f or af ixedt ime of 30 min. The absorbance of the yellow coloured product was measured at 395 nm. The absorbance-concentrationp lot was rectilinear over the rangeo f2 -20 µg mL -1 (r= 0.9994) with minimum detectability of 0.6 µg mL -1 (1.75 x10 -6 M). The different experimental parameters affecting the development and stability of the colourw ere carefully studied and optimized. The determination of isoxsuprine by the fixed-concentration and rate-constantm ethods is also feasible with the calibratione quations obtained, but the fixed time methodh as been found to be more applicable.T he proposed methodw as further applied to the determination of the drug in formulations. The results obtained were in good agreementw ith thoseo btained usingar eferencem ethod. The reaction pathway wasproposed. KeywordsKineticd etermination,i soxsuprine HCl, (NBD-Cl),p harmaceutical preparations.Scientia Pharmaceutica (Sci. Pharm.) 74, 99-119

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Section: Specificity Of the Proposed Methodsmentioning

confidence: 90%

Kinetic Spectrophotometric Determination of Isoxsuprine in Dosage Forms Through Derivatisation with 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl)

2006

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“…Various analytical methods have been used to determine isoxoprene hydrochloride, including high performance liquid chromatography [6][7][8], fluorescence [9], flow injection [10,11], spectrophotometry [12][13][14][15][16][17], gas chromatography [18] and for the determination of oxymetazoline hydrochloride, including HPLC [19][20][21][22], spectrophotometry [23][24][25][26][27][28][29], flow injection chemistry Luminescence [30], Ion Selective Electrode [31][32][33][34][35][36] and Fluorescence Spectrophotometry[37] methods.…”

Section: Introductionmentioning

confidence: 99%

Development HPLC technique for determining Oxymetazoline and Isoxspurine in pharmaceutical formulations

ICC¹,

Alnedawi

Hassana

et al. 2022

Egypt. J. Chem.

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A fast, high-performance liquid chromatography method was established to estimate Oxymetazoline hydrochloride and Isoxsuprine hydrochloride in pharmaceutical preparations HPLC. It consists of an Azorbax-C8 (250mm ×4.6 mm, 5µm ) column with a mobile phase composed of methanol:acetonitrile: buffer (0.01 M) potassium dihydrogen phosphate with triethylamine (pH 5.5) (50: 10:40, V/V/V ) eluted at 1.5 ml/min flow rate. The detection was done using a photodiode array (PDA) detector. The proposed method was validated in linearity, precision, and accuracy. The retention times of IsoxsuprineHCl and OxymetazolineHCl are 3.6 and 6.2 ±0.4 min, respectively. For both drugs, the linear range and detection limits were 1-250 µg/ml and 0.5 µg/ml, respectively. The proposed method was successfully applied to determine ISX and OXY in pharmaceutical preparations.

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“…Different analytical techniques reported for the determination of ISX in both pharmaceuticals and biological matrices include UV spectrophotometry [4,5], ion selective electrode potentiometry [6], chemilu minescence [7], high performance liquid chromatog raphy (HPLC) [8][9][10], gas chromatography (GC) [11], GC MS [12], LC MS [13], affinity chromatog raphy [14], polarography [15] and fluorimetry [16]. Very recently, a comprehensive literature on visible spectrophotometry method for the determination of ISX has been compiled by same authors [17].…”

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confidence: 99%

Non-aqueous and two-phase titrimetric assay of isoxsuprine hydrochloride in pharmaceuticals

2012

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tance in large scale analysis. Therefore, highly precise stoichiometric reaction with a reagent possessing antagonistic properties for the assay of pharmaceutical using titrimetric procedure is still the choice of many pharmacopoeias [18,19]. There is only one titrimetric procedure reported for ISX [3] and this scarcity could be due to the non vulnerability of the basic nitrogen group. Although two electron releasing α methyl groups tend to raise the basicity of the amino group present in ISX, because it is a hydrochloride salt, the ISX exists in structure (b) form of Fig. 1 in solution wherein the transfer of non bonding electrons is restricted, and hence the basicity of the amino group gets decreased. The present work removes the proton from the nitrogen utilizing the well known reaction between mercuric acetate and hydrochloride (Fig. 2) prior to the titration with perchloric acid in method A. The ion association reaction of method B provides an alternative to method A because they vary largely in reaction selectivity. The selectivity of the acidimetric method (method A) is based on differences in base strength, whereas method B is specific for protonated amine. Based on the difference in reaction selectivity, both methods found diverse application in tablets, injection and spiked human urine analyses. In order to demonstrate high selectivity of method B, recovery of ISX from the urine matrix was studied. Proposed methods have been validated and found to be accurate and precise. Abstract-Based on the nitrogenous base or quaternary ammonium moiety in isoxsuprine hydrochloride (ISX), two highly accurate and selective titrimetric methods are proposed f or the determination of ISX in spiked human urine, injection and tablets. Non aqueous titration (Method A) involves removal of protonated amine using mercuric acetate for enhanced basic nitrogen prior to titration with perchloric acid in an acetic acid medium using crystal violet as indicator. Two phase titration (Method B) is based on ion association complex formation between sodium lauryl sulphate (SLS) and protonated amine of ISX at pH 2.5 in aqueous phase, end point being detected by change in dimethyl yellow color in chloroform layer. The methods are applicable over the concentration range 2.0-20.0 mg and 1.0-10.0 mg for method A and method B, respec tively. Calculations are based on 1 : 1 molar ratio, i.e., JSX : HClO 4 for method A and ISX : SLS for method B, owing to the presence of one nitrogen atom. Method A is applicable to the determination of ISX in tablets whereas method B is applicable to spiked human urine, injection and tablets. The methods are vali dated statistically by comparing the results with those of the reference method by applying the Student's t test and F test. The accuracy was further ascertained by recovery studies via standard addition technique. Non Aqueous and Two

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High-Performance Liquid Chromatography of two Peripheral Vasodilators, Nylidrin Hydrochloride and Isoxsuprine Hydrochloride, in Pharmaceutical Dosage Forms

Cited by 18 publications

References 2 publications

Kinetic Spectrophotometric Determination of Isoxsuprine in Dosage Forms Through Derivatisation with 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl)

Kinetic Spectrophotometric Determination of Isoxsuprine in Dosage Forms Through Derivatisation with 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl)

Development HPLC technique for determining Oxymetazoline and Isoxspurine in pharmaceutical formulations

Non-aqueous and two-phase titrimetric assay of isoxsuprine hydrochloride in pharmaceuticals

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