Simultaneous determination of procaine and para-aminobenzoic acid by LC–MS/MS method (original) (raw)
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Journal of Chromatography B, 2008
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%.
Analytical and Bioanalytical Chemistry, 2002
A first derivative spectrometric method has been developed for the determination of the para-aminobenzoic acid (PABA), a related substance and degradation product of the local anesthetic procaine hydrochloride (PH). The wavelength selected for the determination of para-aminobenzoic acid in the presence of procaine was 290 nm. At this wavelength the calibration graphs relating the amplitude of the signals to the concentration of paraaminobenzoic acid were linear up to 10 mg L -1 . The detection limit of para-aminobenzoic acid was 0.70 mg L -1 . The method is simple and rapid and does not require preliminary treatment of the sample. The method was validated.
SIMI 2019
Two spectrometric methods have been developed for quantitative simultaneous determination of procaine hydrochloride (PH·HCl), procainamide hydrochloride (PHA·HCl) and lidocaine (Lid) from synthetic mixture. The methods employed are first derivative spectrometry, using zero crossing method and multicomponent analysis which is based on the additivity law. Using first derivative spectrometry, the wavelength selected for the quantitative determination of PH·HCl was 237 nm for Lid was 242 nm and for PHA·HCl was 290 nm in mixture. The method is linear when the concentration ranged between 6.62-9.93 μg/mL for PH·HCl, 6.43-9.64 for PHA·HCl and 5.56-8.35 for Lid. The multicomponent analysis is a direct method and involves the absorbance measurements of at three different wavelengths. The molar absorption coefficients values were calculated at each wavelength and the concentration of PH·HCl, PHA·HCl and Lid from mixture was determined by solving matrix using Cramer's rule. The recovery of...
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.
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.
Journal of Chromatography B, 2014
Two rugged liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods for the determination of propylparaben, its major metabolite, p-hydroxybenzoic acid (pHBA), and their sulfate conjugates have been developed and validated in citric acid-treated rat plasma. To prevent propylparaben being hydrolyzed to pHBA ex vivo, rat plasma was first treated with citric acid; then collected and processed at a reduced temperature (ice bath). Stable isotope labeled internal standards, d 4-propylparaben, 13 C 6-pHBA, and the d 4-labeled internal standards of their sulfate conjugates were used in the methods. The analytes were extracted from the matrix using protein precipitation, followed by chromatographic separation on a Waters ACQUITY UPLC HSS T3 column. Quantification using negative ion electrospray was performed on a Sciex API 4000 mass spectrometer. The analytical ranges were established from 2.00 to 200 ng/mL for propylparaben, 50.0-5000 ng/mL for pHBA, 50.0-10,000 ng/mL for the sulfate conjugate of propylparaben (SPP) and 200-40,000 ng/mL for the sulfate conjugate of pHBA (SHBA). Inter-and intra-run precision for the quality control samples were less than 5.3% and 4.4% for all analytes; and the overall accuracy was within ±5.7% of the nominal values. The validated bioanalytical methods demonstrated excellent sensitivity, specificity, accuracy and precision and were successfully applied to a rat toxicology study under the regulations of Good Laboratory Practices (GLP). Strategies have been developed and applied toward overcoming the challenges related to analyte stability, and environmental and endogenous background.
Indian Journal of Pharmaceutical Education and Research, 2019
Background: A simple, sensitive and accurate method for the determination of procaterol in human urine was developed and validated using Gas Chromatography coupled to tandem mass spectrometry (GC-MS/MS) as per the requirements of World Anti-Doping Agency (WADA) and ICH guidelines. Methodology: The sample processing includes deconjugation with enzymatic hydrolysis, Solid Phase Extraction (SPE) procedure using XAD2 column and Liquid-liquid Extraction (LLE) followed by the derivatisation using N-methyl trimethylsilysl trifluoroacetamide (MSTFA). Results: The method included a chromatographic run of 17 min and the calibration curve was linear over the concentration range of 5-40 ng/mL with a correlation coefficient (r) of 0.98. The intra-and inter-day assay precision ranged from 0.75 to 0.94% and 1.2 to 1.70%, respectively. The absolute recovery percentage for procaterol was found to be 83%. The recovery was sufficient to reliable identify the procaterol at or below the level prescribed by WADA ie MRPL 20ng/ ml. The LOQ and LOD was found to be 5 and 3 ng/ml respectively. Conclusion: A simple and sensitive GC-MS/MS method for quantitative estimation of Procaterol was developed and validated as per the WADA ISL and ICH guidelines. This developed method could be also used for therapeutic drug monitoring purposes.
DETERMINATION OF m-AMINOBENZOIC ACID BY POTENTIOMETRIC TITRATION
Cerium (IV) sulfate solution in sulfuric acid was used for the determination of them-aminobenzoic acid in sulfuric acid solution by potentiometric titration. The optima workingconditions were set up for the quantitative determination of m-aminobenzoic acid. The method issimple, rapid and reliable.
Asian Journal of Chemistry
This study reports a new stability indicating HPLC method using Spursil C18 column as stationary phase, and mixture of 0.1 M Na2HPO4 and methanol (50:50 v/v) as mobile phase for the chromatographic determination of paracetamol and prochlorperazine in tablets and in bulk form. The linearity range is 250-750 μg/mL for paracetamol and 2.5-7.5 μg/mL for prochlorperazine. The limit of detection values are 2.650 μg/mL for paracetamol and 0.175 μg/mL for prochlorperazine. The minor values of the relative standard deviation (≤ 2.0 %) as well as good percent assay values (nearer to 100 %) confirm the high precision and accuracy of the present method. From the degradation study chromatograms found that there was no interference from degradants when paracetamol and prochlorperazine are quantified in tablets through the proposed method. A good agreement between results obtained and labeled claim for the determination of paracetamol and prochlorperazine in tablet samples demonstrates that the pr...