Simultaneous determination of procaine hydrochloride, procainamide hydrochloride and lidocaine by molecular absorption spectrometry (original) (raw)
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New simple and selective assay method has been presented for the binary mixtures of procaine hydrochloride and phenazone in pharmaceutical formulations. The method depends on derivative ultraviolet spectrophotometry with zero-crossing measurements. Calibration plots are linear at 316nm (procaine hydrochloride, first derivative) and 261nm (phenazone, third derivative). The assay was linear over the concentration ranges 0.90-20.0g mL-1 for procaine hydrochloride and 0.96-20.0g mL-1 for phenazone. The detection limits for procaine hydrochloride and phenazone were found to be 0.304 and 0.032 g mL-1, respectively. The developed derivative spectrophotometric method was applied to laboratory mixtures and to otic drops for these drugs. The procedures are rapid, accurate, precise and did not require any preliminary separation or treatment of the samples.
This paper involves batch and flow injection spectrophotometric determination of procaine-hydrochloride in pharmaceutical formulations. These methods were based on the diazotization reaction of procaine-HCl with sodium nitrite and hydrochloric acid to form diazonium salt, which is coupled with 8-hydroxyquinoline in alkaline medium to form orange-pink water soluble azo dye that was stable and has a maximum absorption at 509 nm. In batch method Beer’s law was obeyed in the concentration range of (0.8 - 8.0 µg/mL) and detection limit of 0.12 µg/mL with a correlation coefficient (r) of 0.9954 and a molar absorptivity of 2.0814x104 L mol-1cm-1. The flow injection analysis (FIA) system was applied for determination of procaine-HCl. The calibration graph is linear in the concentration range of (2.0 – 50 µg/mL) with detection limit (0.75 µg/mL) and correlation coefficient of (0.9927). The precision and accuracy of both methods were checked by calculating relative standard deviation (RSD) and relative error (E %) for two different levels of concentration.
https://www.ijrrjournal.com/IJRR\_Vol.7\_Issue.1\_Jan2020/Abstract\_IJRR0011.html, 2020
Objective: To develop extraction procedures for extracting Lidocaine from various pharmaceutical dosage forms (ointment, gel, injection, aerosol, transdermal patch) and to analyze them by development of accurate, precise and robust reverse phase high performance liquid chromatography method. Method: Chromatographic procedures were developed using Chromatopak, Peerless C18 column (Column dimensions: 250 mm x 4.6 mm, 5 μm) with mobile phase comprising of Dipotassium monohydrogen phosphate buffer (10Mm): ACN in ratio 20:80 at a flow rate of 1ml/min, with detection wavelength at 263nm. The retention time of Lidocaine was found to be at 5.43±0.03. Results: The method was validated according to ICH guidelines (Q2) R1.Linearity of LID was found in concentration range of 20-100ug/ml with r2=0.999. Limit of Detection and Limit of Quantification were found to be 1.54ug/ml and 4.68ug/ml. %RSD values for intraday and interday precision were also found to be >2%. Accuracy studies were also in range between 95%-105%. The method proved to be robust when chromatographic parameters like Ph, mobile phase ratio, flow rate, wavelength were altered. Conclusion: The % Assay values of marketed formulation were found to be within prescribed range. Thus this proposed RP-HPLC method can be used in routine quality control analysis of LID from its various pharmaceutical dosage forms.
Journal of Chromatographic Science, 2015
Two sensitive and selective analytical methods were developed for simultaneous determination of aminoacridine hydrochloride and lidocaine hydrochloride in bulk powder and pharmaceutical formulation. Method A was based on HPLC separation of the cited drugs with determination of the toxic lidocaine-related impurity 2,6-dimethylaniline. The separation was achieved using reversedphase column C18, 250 × 4.6 mm, 5 µm particle size and mobile phase consisting of 0.05 M disodium hydrogen phosphate dihydrate (pH 6.0 ± 0.2 adjusted with phosphoric acid) and acetonitrile (55 : 45, v/v). Quantitation was achieved with UV detection at 240 nm. Linear calibration curve was in the range of 1.00-10.00, 13.20-132.00 and 1.32-13.20 µg mL −1 for aminoacridine hydrochloride, lidocaine hydrochloride and 2,6-dimethylaniline, respectively. Method B was based on TLC separation of the cited drugs followed by densitometric measurement at 365 nm on the fluorescent mode for aminoacridine hydrochloride and 220 nm on the absorption mode for lidocaine hydrochloride. The separation was carried out using ethyl acetate-methanol-acetic acid (65 : 30 : 5 by volume) as a developing system. The calibration curve was in the range of 25.00-250.00 ng spot −1 and 0.99-9.90 µg spot −1 for aminoacridine hydrochloride and lidocaine hydrochloride, respectively. The results obtained were statistically analyzed and compared with those obtained by applying the manufacturer's method.
Spectrophotometric determination of procainamide hydrochloride using sodium periodate
Arabian Journal of Chemistry, 2015
A simple spectrophotometric method has been described for the determination of procainamide hydrochloride. The method is based on the oxidation of procainamide hydrochloride by sodium periodate in the presence of sulfuric acid and measurement of the absorbance of the violet color formed at 531 nm. Parameters affecting the reaction were studied and conditions were optimized. Linear calibration graph was obtained from 50 to 700 lg ml À1 of procainamide hydrochloride and the limit of detection was 25 lg ml À1. The method was successfully applied for the determination of procainamide hydrochloride in pharmaceutical preparation.
Journal of Current Pharma Research
To develop a simple, specific, accurate and precise high performance thin layer chromatography method for simultaneous estimation of Lidocaine and Prilocaine in a topical local anesthetic cream. The mixture of Prilocaine and Lidocaine separated on Aluminum precoated silica gel 60 F254 plates using di-isopropyl ether: methanol: ammonia (10: 0.5: 0.1 % v/v/v) as mobile phase and detection was carried a wavelength of 225 nm The method was validated as per ICH guidelines. The Rf value was found to be 0.45 ± 0.03 for Prilocaine and 0.55 ± 0.02 for Lidocaine, respectively. Linearity was observed in the concentration range of 100-600 ng/spot for both Lidocaine and Prilocaine, respectively. HPTLC method was validated according to ICH guideline and values of linearity, precision, robustness, LOD, LOQ, selectivity, recovery were found to be in good accordance with the prescribed value. Conclusion: The proposed method can be used successfully for routine analysis of Lidocaine and Prilocaine in their topical formulation.
Analytical Sciences, 2003
A simple, accurate and sensitive method for the microdetermination of benzocaine, lignocaine and procaine hydrochlorides in pure forms and in pharmaceutical formulations is described. The procedure is based on the reaction of those drugs in an aqueous acidic medium with p-benzoquinone to form charge-transfer complexes. The method has been used for the determination of 5.0-70, 5.0-60 and 5.0-90 µg ml-1 of benzocaine, lignocaine HCl and procaine HCl, respectively. The complexes have apparent molar absorptivities of 1.70 × 10 3 , 2.79 × 10 3 and 2.42 × 10 3 L mol-1 cm-1 and Sandell sensitivities of 9.72, 10.34 and 11.25 ng cm-2 , respectively. The proposed procedure of analysis is as accurate as the British Pharmacopoeial method (2003). The method was successfully used for the determination of those drugs in the presence of their degradation products, additives and excipients, which were normally encountered in pharmaceutical formulations.
Simultaneous determination of procaine and para-aminobenzoic acid by LC–MS/MS method
Journal of Chromatography B, 2007
A sensitive high performance liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed for simultaneous determination of procaine and its metabolite p-aminobenzoic acid (PABA). N-Acetylprocainamide (NAPA) was used as an internal standard for procaine and PABA analysis. This assay method has also been validated in terms of linearity, lower limit of detection, lower limit of quantitation, accuracy and precision as per ICH guidelines. Chromatography was carried out on an XTerra TM MS C 18 column and mass spectrometric analysis was performed using a Quattro Micro TM mass spectrometer working with electro-spray ionization (ESI) source in the positive ion mode. Enhanced selectivity was achieved using multiple reaction monitoring (MRM) functions, m/z 237 → 100, m/z 138 → 120, and m/z 278 → 205 for procaine, PABA and NAPA, respectively. Retention times for PABA, procaine and NAPA were 4.0, 4.7 and 5.8 min, respectively. Linearity for each calibration curve was observed across a range from 100 nM to 5000 nM for PABA, and from 10 nM to 5000 nM for procaine. The intra-and inter-day relative standard deviations (RSD) were <5%.
Journal of the Iranian Chemical Research, 2010
The multivariate calibration method, partial least square regression (PLS) was applied for the simultaneous spectrophotometric determination of Lidocaine (LID) and Hydrocortisone acetate (HCA) in their mixtures. The parameters of chemometric technique were optimized and the proposed method was validated with synthetic samples and applied to analyze these drugs in pharmaceutical products with good accuracy and precision. The results were compared with the HPLC method. The squares of correlation coefficients (R 2) for predicted LID and HCA with the proposed method in test samples were 0.9970 and 0.9964, respectively. The relative standard deviations for commercial products were less than 1%.