Potentiometric PVC membrane sensor for the determination of phenylephrine hydrochloride in some pharmaceutical products

A new PVC membrane electrode for the determination of phenylephrine hydrochloride based on the formation of an ionassociation complex of phenylephrine hydrochloride with the phosphotungstate counter anion as an electroactive material dispersed in a PVC matrix is described. The sensor shows a fast, stable, near-Nernstian response for 1.0 × 10^?5 to 1.0 × 10^?1 M phenylephrine hydrochloride at 25 °C over the pH range of 3.5–8.0 with a cationic slope of 58.1 ± 0.6 mV decade^?1. The electrode was successfully used for potentiometric determination of phenylephrine hydrochloride in some pharmaceutical drugs.     

Quantitative Determination of Adrenaline Hydrochloride Injection and Noradrenaline Bitartrate Injection by a New HPLC Method via Substitute for Reference Substance

An HPLC method for quantitative determination of adrenaline hydrochloride injection and noradrenaline bitartrate injection was established and validated with a substitute for the reference substance.Phenylephrine hydrochloride was selected as the substitute for the reference substance of adrenaline and noradrenaline bitartrate.The correction factor of phenylephrine hydrochloride with respect to the reference substance of adrenaline and noradrenaline bitartrate was determined under defined conditions.Adrenal...     

Quantitation of memantine hydrochloride bulk drug and its tablet formulation using proton nuclear magnetic resonance spectrometry

The use of quantitative nuclear magnetic resonance spectrometry for the determination of non‐UV active memantine hydrochloride with relative simplicity and precision has been demonstrated in this study. The method was developed on a 500 MHz NMR instrument and was applied to determination of the drug in a tablet formulation. The analysis was performed by taking caffeine as an internal standard and D₂O as the NMR solvent. The signal of methyl protons of memantine hydrochloride appeared at 0.75 ppm (singlet) relative to the signal of caffeine (internal standard) at 3.13 ppm (singlet). The method was found to be linear (r² = 0.9989) in the drug concentration range of 0.025 to 0.80 mg/ml. The maximum relative standard deviation for accuracy and precision was <2. The limits of detection and quantification were 0.04 and 0.11 mg/ml, respectively. The robustness of the method was revealed by changing nine different parameters. The deviation for each parameter was also within the acceptable limits. The study highlighted possibility of direct determination of memantine hydrochloride in pure form and in its marketed tablet formulation by the use of quantitative NMR, without the need of derivatization, as is the requirement in HPLC studies. Copyright © 2016 John Wiley & Sons, Ltd.     

Charge-transfer complexes of phenylephrine with nitrobenzene derivatives

The molecular charge-transfer complexes of phenylephrine with picric acid and m-dinitrobenzene have been studied and investigated by IR, 1H NMR electronic spectra in organic solvents and buffer solutions, respectively. Simple and selective methods are proposed for the determination of phenylephrine hydrochloride in bulk form and in tablets. The two methods are based on the formation of charge-transfer complexes between drug base as a n-donor (D) and picric acid, m-dinitrobenzene as pi-acceptor (A). The products exhibit absorption maxima at 497 and 560 nm in acetonitrile for picric acid and m-dinitrobenzene, respectively. The coloured product exhibits an absorption maximum at 650 nm in dioxane. The sensitive kinetic methods for the determination phynylephrine hydrochloride are described. The method is based upon a kinetic investigation of the oxidation reaction of the drug with alkaline potassium permanganate at room temperature for a fixed time at 20 min.     

Determination of N,N-dimethylaminoethyl chloride and the dimethylaziridinium ion at sub-ppm levels in diltiazem hydrochloride by LC-MS with electrospray ionisation

An LC-MS method is described for the determination of the synthetic reagent N,N-dimethylaminoethyl chloride (DMC) in the drug substance diltiazem hydrochloride, for which the permissible limit is not more than 1 ppm (microgram g-1). The N,N-dimethylaziridinium ion (DMA), the reactive intermediate formed by cyclisation of DMC, is also detected. A column switching arrangement is used: diltiazem hydrochloride is trapped on a reversed-phase HPLC column, and the polar analytes are separated by ion exchange chromatography. Ionisation is effected by positive-ion electrospray, and the quadrupole filter mass spectrometer is operated in the selected ion recording mode. The detection limit (peak height-to-baseline noise ratio = 3) for DMC varies from day to day in the range < 0.05 to 0.1 ppm. The response for DMC is linear (r > 0.999) over the concentration range 0.2-10 ppm, and the repeatability is better than 7% (relative standard deviation) at 1.0 ppm. Concentrations of DMC in diltiazem hydrochloride from the manufacturing facility under study ranged from undetectable to about 0.07 ppm. An indirect TLC method has been published for the determination of DMC in mepyramine maleate, but it lacks the necessary sensitivity and specificity. The LC-MS method presented is direct, straightforward and suitable for routine use.     

Application of the Coupled Redox and Complexation Reactions to Flow Injection Spectrophotometric Determination of Promazine

Abstract

A flow injection (FI) spectrophotometric method is proposed for the determination of promazine hydrochloride. The method is based on the coupled redox - complexation reactions which proceed in the promazine-iron(III) and 1,10-phenantroline system. A linear calibration graph was obtained between 2–12 ppm of promazine hydrochloride with a sampling rate of 163 samples h^?1. The proposed method was applied to the determination of promazine in pharmaceuticals.     

Spectrophotometric determination of phenylephrine hydrochloride in pharmaceuticals by flow injection analysis exploiting the reaction with potassium ferricyanide and 4-aminoantipyrine

This paper presents a method for the determination of phenylephrine hydrochloride in pharmaceuticals by spectrophotometric flow injection analysis exploiting the reaction with potassium ferricyanide and 4-aminoantipyrine, which leads to the formation of a condensation product with strong absorptivity at 500 nm. The linear dynamic range was between 0.95 and 9 mg/L, with a limit of detection of 0.2 mg/L and a sampling throughput of 120 samples per hour. The method was applied to eyewashes and nasal decongestant liquid medicines.     

A chemical concentration x-ray determination of selenium in copper-, nickel-and iron-base alloys

A method is described for the determination of selenium in various metals and alloys at concentrations of 3-100ppm. A chemical separation is made by filtration after reduction of the selenious acid to elemental selenium with hydroxylamine hydrochloride. The pure selenium product is readily analysed by X-ray fluorescence; the method is free from errors due to matrix effects. The relative standard deviation is 6 % for a copper-nickel alloy at the 60 ppm level.     

Simultaneous determination of phenylephrine hydrochloride, guaifenesin, and chlorpheniramine maleate in cough syrup by gradient liquid chromatography

A simple and reliable high-performance liquid chromatographic method was developed for the simultaneous determination of mixture of phenylephrine hydrochloride (PHENYL), guaifenesin (GUAIF), and chlorpheniramine maleate (CHLO) either in pure form or in the presence of methylparaben and propylparaben in a commercial cough syrup dosage form. Separation was achieved on a C8 column using 0.005 M heptane sulfonic acid sodium salt (pH 3.4 +/- 0.1) and acetonitrile as a mobile phase by gradient elution at different flow rates, and detection was done spectrophotometrically at 210 nm. A linear relationship in the range of 30-180, 120-1800, and 10-60 microg/mL was obtained for PHENYL, GUAIF, and CHLO, respectively. The results were statistically analyzed and compared with those obtained by applying the British Pharmacopoeia (2002) method and showed that the proposed method is precise, accurate, and can be easily applied for the determination of the drugs under investigation in pure form and in cough syrup formulations.     

Development and validation of a generic high‐performance liquid chromatography for the simultaneous separation and determination of six cough ingredients: Robustness study on core–shell particles

A generally applicable high‐performance liquid chromatographic method for the qualitative and quantitative determination of pharmaceutical preparations containing phenylephrine hydrochloride, paracetamol, ephedrine hydrochloride, guaifenesin, doxylamine succinate, and dextromethorphan hydrobromide is developed. Optimization of chromatographic conditions was performed for the gradient elution using different buffer pH values, flow rates and two C₁₈ stationary phases. The method was developed using a Kinetex® C₁₈ column as a core–shell stationary phase with a gradient profile using buffer pH 5.0 and acetonitrile at 2.0 mL/min flow rate. Detection was carried out at 220 nm and linear calibrations were obtained for all components within the studied ranges. The method was fully validated in agreement with ICH guidelines. The proposed method is specific, accurate and precise (RSD% < 3%). Limits of detection are lower than 2.0 μg/mL. Qualitative and quantitative responses were evaluated using experimental design to assist the method robustness. The method was proved to be highly robust against 10% change in buffer pH and flow rate (RSD% < 10%), however, the flow rate may significantly influence the quantitative responses of phenylephrine, paracetamol, and doxylamine (RSD% > 10%). Satisfactory results were obtained for commercial combinations analyses. Statistical comparison between the proposed chromatographic and official methods revealed no significant difference.     

The Simultaneous Determination of Phenylephrine Hydrochloride,Paracetamol, Chlorpheniramine Maleate and Dextromethorphan Hydrobromide in Pharmaceutical Preparations

A new rapid and sensitive method has been developed and validated for the simultaneous determination of phenylephrine hydrochloride, paracetamol, chlorpheniramine maleate and dextromethorphan hydrobromide in pharmaceutical preparations. The separation was achieved on a C18 column using a gradient mobile phase of acetonitrile–sodium perchlorate (pH 3, 0.01 M) at a flow rate of 1.4 mL min⁻¹. Detection was at 204 nm. Pseudoephedrine hydrochloride was selected as internal standard. The recovery of the drugs ranged from 97.8 to 100.9%. Central composite design was used during validation to calculate method robustness and the percentage of sodium perchlorate, temperature and flow rate were investigated as factors. The method was found to be applicable for the determination of the four compounds in sugar-coated tablets.

     

Simultaneous determination of ingredients in an ointment by hydrophobic interaction electrokinetic chromatography

Hydrophobic interaction electrokinetic chromatography was used to simultaneously determine seven active ingredients (diphenhydramine hydrochloride, dibucaine hydrochloride, chlorhexidine hydrochloride, phenylephrine hydrochloride, hydrocortisone acetate, allantoin and tocopherol acetate) in an ointment. Not only hydrophobic but also ionic compounds were successfully separated by use of a separation solution composed of acetonitrile-water (80:20, v/v), tetradecylammonium salt and ammonium chloride. The migration behavior of the hydrophobic compound depended on tetradecylammonium concentration, while that of the ionic compounds depended on ammonium chloride concentration. An addition of triethylamine to the separation solution markedly improved the reproducibility of the peak areas of cations with a relative standard deviation (RSD) of less than 1.7% (n=6). The established method was validated and confirmed to be applicable to the determination of the active ingredients in a commercial ointment. Sample preparation was performed by liquid-liquid extraction and no interference from the formulation excipients was observed. Good linearities were obtained, with correlation coefficients above 0.999. Recoveries and precisions ranged from 98.0 to 100.8%, and from 0.4 to 2.9% RSD, respectively. These results suggest that hydrophobic interaction electrokinetic chromatography can be used for the determination of ionic compounds as well as hydrophobic compounds in ointment.     

H-point standard addition method for simultaneous determination of phenylephrine hydrochloride,chlorpheniramine maleate,and paracetamol as a ternary mixture in pharmaceutical formulations

The simultaneous analysis of a ternary mixture containing paracetamol (PAR), phenylephrine hydrochloride (PHE), and chlorpheniramine maleate (CPM) was conducted without prior separation and using an advanced spectrophotometric method. The H-point standard addition and absorbance correction methods were selected to determine the compounds, which are highly overlapped spectra in pharmaceutical formulations. The method is based on the use of three different wavelengths of 296, 272, and 227 nm for the ternary mixture. The concentration of PAR was calculated directly at 296 nm because no interferences existed. Absorbance correction method was used to remove the role of PAR at 272 and 227 nm. The concentrations of the PHE and CPM compounds in the mixture were determined by using the H-point standard addition method. The results showed that simultaneous determination of PAR, PHE, and CPM could be conducted within the range of 1–33 μg/mL, 1–23 μg/mL, and 1–36 μg/mL, respectively. The relative standard deviations for the simultaneous determination of PHE, CPM, and PAR were 0.617, 2.76, and 1.71, respectively. The proposed method was implemented successfully for the simultaneous determination of PAR, PHE, and CPM in pharmaceutical formulations.     

Flow-injection determination of phenylephrine hydrochloride in pharmaceutical dosage forms with on-line solid-phase extraction and spectrophotometric detection

A flow injection method is proposed for the determination of phenylephrine hydrochloride in pharmaceutical dosage forms. The method involves the use of on-line solid-phase extraction by means of a microcolumn containing Dowex 50W X8 ion-exchange resin for the separation of the analyte prior to colour development and spectrophotometric detection in the visible region.

The influence of preconcentration flow, preconcentration pH and elution volume was studied.

The method exhibits appropriate linearity (r² = 0.9999) which was proved statistically by means of the “F”-test. When applied to commercial samples containing several active ingredients and excipients, a significant reduction of interferences was found. Accuracy, evaluated by means of the spike recovery method was in the range 99.7–100.8%, with precision (R.S.D., %) better than 1%.

In order to achieve the automation the system was controlled from a notebook computer by means of a program written in QuickBASIC language. Under these conditions, a sampling frequency of 40 samples per hour could be attained.     

毛细管电泳-安培检测法测定3种拟肾上腺素药物

建立了毛细管电泳-安培检测法测定盐酸去氧肾上腺素(phenylephrine hydrochloride, PHE)、重酒石酸间羟胺(metaraminol bitartrate, MR)和盐酸异丙肾上腺素(isoprenaline hydrochloride, IP)3种拟肾上腺素药物的方法。检测电位为0.950 V(Ag/AgCl为参比电极),硼酸盐浓度为50 mmol/L(pH 10.00),分离电压为18 kV,进样时间为10 s。在最佳实验条件下,3种物质在18 min内达到基线分离,在2～100 μmol/L浓度范围内峰面积与浓度呈良好的线性关系,线性相关系数不小于0.9991。盐酸去氧肾上腺素、重酒石酸间羟胺和盐酸异丙肾上腺素的检出限分别为0.8、0.8和1.0 μmol/L。将所建立的方法应用于针剂样品的分析,结果令人满意。     

Selective spectrophotometric determination of ascorbic acid in drugs and foods

A new analytical method was developed for the determination of ascorbic acid. The method is based on the reaction of ascorbic acid with 4-chloro-7-nitrobenzofurazane (NBD-Cl) in the presence of 0.2M sodium hydroxide, where a bluish green colour (lambda(max) 582 nm) is developed after dilution with 50% (v/v) aqueous acetone solution. Beer's law was obeyed in a concentration range of 5-20 microg ascorbic acid/ml with a good correlation coefficient (r = 0.9990). The method was found to be highly specific for the determination of ascorbic acid in the presence of dehydro-ascorbic acid, all other vitamins and minerals possibly present in multivitamin preparations, rutin, salicylamide, acetyl salicylic acid, paracetamol, caffeine, phenylephrine hydrochloride and dipyrone. Moreover, the proposed procedure was also successfully applied for the determination of ascorbic acid in some canned and fresh fruit juices, some vegetables and infant milk products without interference from coloured and other substances present in the plant extracts.     

Determination of phenylephrine hydrochloride and chlorpheniramine maleate in binary mixture using chemometric-assisted spectrophotometric and high-performance liquid chromatographic-UV methods

Four methods have been developed for the simultaneous determination of phenylephrine hydrochloride and chlorpheniramine maleate without previous separation. In the first method both drugs are determined using first derivative UV spectrophotometry, with zero-crossing measurement. The second method depends on first derivative of the ratios spectra. The third method describes the use of multivariate spectrophotometric calibration for the simultaneous determination of the analyzed binary mixture where the resolution is accomplished by using partial least squares (PLS) regression analysis. In the fourth method (HPLC), a reversed-phase column and a mobile phase of methanol:water:acetonitrile (80:12:8 v/v/v/) at 0.9 ml/min flow rate have been used to separate both drugs with a UV detection at 270 nm. All the proposed methods are extensively validated. They have the advantage to be economic and time saving. All the described methods can be readily utilized for analysis of pharmaceutical formulations. The results obtained using the proposed methods are statistically analyzed and compared with some reported methods.     

紫尿酸–Fe(Ⅲ)分光光度法测定盐酸羟胺

在碱性介质及溴化十六烷基吡啶存在条件下,盐酸羟胺与Fe(Ⅲ)–紫尿酸体系发生显色反应形成离子缔合物,该离子缔合物在635 nm波长处有一个吸收峰,其表观摩尔吸光系数ε=2.05×104 L/(mol·cm),据此建立了测定盐酸羟胺的间接分光光度法。盐酸羟胺的质量浓度在0~2.4 mg/L范围内与吸光度与呈良好的线性,线性相关系数r=0.999 8,方法的检出限为0.01 mg/L。将该方法用于盐酸羟胺的测定,其测定结果与国标法测定结果相吻合,加标回收率为95.0%~104.0%,测定结果的相对标准偏差为0.51%~1.29%(n=5)。该方法灵敏度高,操作简便,可用于盐酸羟胺含量测定。     

Improvement of end-point detection in the non-aqueous titration of sulphacetamide sodium

The sluggish end-point in the non-aqueous titration of sulphacetamide sodium in glacial acetic acid can be improved by addition of acetic anhydride to the titration medium, and selective determination of sulphacetamide sodium in presence of phenylephrine hydrochloride in eye drops then becomes possible. A mixture of sulphacetamide sodium and the antihistamine drug phenyltoloxamine dihydrogen citrate can also be analysed.     

在丙酮增敏作用下硝普钠分光光度法测定盐酸吗啉胍

摘要：建立了可见分光光度法测定盐酸吗啉胍的新方法。研究表明,当NaOH浓度为0.13mol/L,在丙酮存在下硝普钠与盐酸吗啉胍反应生成紫色N-亚硝基类化合物,其最大吸收波长为508nm,表观摩尔吸光系数2.5×10³ L/（mol•cm）。盐酸吗啉胍浓度在0.38×10^-6~3.0×10^-4 g/mL范围内与吸光度呈现良好线性关系,线性回归方程A = 0.02292 + 0.01213c (10^-6 g/mL),线性相关系数r=0.9998,检测限(3σ/k)为0.25×10^-6 g/mL,RSD = 0.21%。本方法可用于药物样品和血清中盐酸吗啉胍含量的测定。