A green approach to the analysis of co-administered ampicillin/sulbactam and paracetamol in human urine

Abstract The novelty of this work is the simultaneous analysis of sulbactam (SUL), ampicillin (AMP), and paracetamol (PARA) in human urine samples, using the environmentally benign RP-HPLC method. A C18 column was used in chromatographic separation using potassium dihydrogen phosphate (10 mmol L–1, pH 5)/ethanol (90 %, V/V) as the mobile phase; flow rate was 1.00 mL min–1. UV detection at 220 nm was used for quantification. The proposed method showed good linearity in the concentration ranges of 2.20–250.00 μg mL–1 for SUL, 2.50–250.00 μg mL–1 for PARA, and 14.50–250.00 μg mL–1 for AMP. Direct injection of urine samples with no prior extraction was performed. This method was found successful in moving towards greener studies of drugs’ urinary excretion, by decreasing hazardous solvent consumption and waste. Moreover, the method was applied to investigate the urinary excretion of the drugs and possible interaction between ampicillin and paracetamol.

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Stability Indicating Assay Method Development and Validation of Simultaneous Estimation of Chlorzoxazone, Diclofenac Sodium and Paracetamol in Bulk Drug and Tablet by RP-HPLC

Research Journal of Pharmacy and Technology ◽

10.52711/0974-360x.2021.00876 ◽

2021 ◽

pp. 5024-5028

Author(s):

Krutika Patel ◽

Sudheer Kumar Verriboina ◽

S.G. Vasantharaju

Keyword(s):

Method Development ◽

Diclofenac Sodium ◽

Potassium Dihydrogen Phosphate ◽

Hplc Method ◽

Assay Method ◽

Simultaneous Estimation ◽

Dihydrogen Phosphate ◽

Stability Indicating ◽

Rp Hplc ◽

Bulk Drug

A simple, accurate, specific and stability-indicating RP-HPLC method was developed for simultaneous determination of chlorzoxazone, diclofenac sodium and paracetamol, using C18 Vydac Monomeric 120A (250 × 4.6mm, 5μ) at 40ºC. The mobile phase contains a mixture of 20mM potassium dihydrogen phosphate buffer (pH 6.2 adjusted with potassium hydroxide) and acetonitrile (30:70 v/v). The flow rate was 1ml/min and detection was carried out at 275nm using PDA detector. The retention time of paracetamol, chlorzoxazone and diclofenac sodium were 3.28mins, 13.27mins and 15.61mins respectively. The analytical curve was linear over a concentration range of 0.65- 6.5μg/ml for paracetamol, 1-10μg/ml for chlorzoxazone and 0.1-1μg/ml for diclofenac sodium. The drugs in bulk and tablet were subjected to acid and alkali hydrolysis, oxidation, thermal and photolytic degradation. This method can be successfully employed for simultaneous quantitative analysis of Chlorzoxazone, Diclofenac sodium and Paracetamol in bulk drug and tablet formulation.

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Development and validation of a reversed-phase HPLC method for determination of assay content of Teriflunomide by the aid of BOMD simulations

Current Chemistry Letters ◽

10.5267/j.ccl.2021.3.001 ◽

2021 ◽

pp. 281-294 ◽

Cited By ~ 1

Author(s):

Abolghasem Beheshti ◽

Zahra Kamalzadeha ◽

Monireh Haj-Maleka ◽

Meghdad Payaba ◽

Mohammad Amin Rezvanfar ◽

...

Keyword(s):

Mobile Phase ◽

Potassium Dihydrogen Phosphate ◽

Active Pharmaceutical Ingredient ◽

Reversed Phase ◽

Hplc Method ◽

Dihydrogen Phosphate ◽

Td Dft ◽

High Level ◽

Development And Validation

Due to the new hopes for treatment of multiple sclerosis (MS) diseases by Teriflunomide (TFN), in this project, a cheap, robust, and fully validated method has been developed both for determination of assay content in API (active pharmaceutical ingredient), and for related impurities analysis (RIA). To operate the method, a common C18, end-capped (250 × 4.6) mm, 5µm liquid chromatography column, was applied. The mobile phase A was prepared by dissolving 2.74 g (20mM) of PDP (potassium dihydrogen phosphate) and 3.72 g (50mM) of PC (potassium chloride) in water (1000 mL). Then, pH was adjusted to 3.0 by adding OPA (ortho-phosphoric acid) 85%; while, the mobile phase B was acetonitrile (ACN) (100%). In order to confirm the experimental data about the λmax of TFN, we have used the Born-Oppenheimer molecular dynamics (BOMD) simulations, quantum mechanics (QM), and TD-DFT calculations. According to the results, the method showed a high level of suitability, specificity, linearity, accuracy, precision, repeatability, robustness, and reliable detection limit.

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HPLC-UV method for quantification of favipiravir in pharmaceutical formulations

Acta Chromatographica ◽

10.1556/1326.2020.00828 ◽

2020 ◽

Cited By ~ 1

Author(s):

İbrahim Bulduk

Keyword(s):

High Performance ◽

Potassium Dihydrogen Phosphate ◽

Pharmaceutical Formulations ◽

Hplc Method ◽

Dihydrogen Phosphate ◽

Potential Candidate ◽

Column Temperature ◽

Candidate Drug ◽

System Suitability ◽

Relative Standard

AbstractFavipiravir (FVP), a pyrazine analog, has shown antiviral activity against a wide variety of viruses. It is considered to be worth further investigation as a potential candidate drug for COVID-19. It is not officially available in any pharmacopoeia. A rapid, simple, precise, accurate, and isocratic high performance liquid chromatography (HPLC) method has been developed for routine quality control of favipiravir in pharmaceutical formulations. Separation was carried out by C18 column. The mobile phase was a mixture of 50 mM potassium dihydrogen phosphate (pH 2.3) and acetonitrile (90:10, v/v) at a flow rate of 1 mL min−1. The ultraviolet (UV) detection and column temperature were 323 nm, and 30 °C, respectively. The run time was 15 min under these chromatographic conditions. Excellent linear relationship between peak area and favipiravir concentration in the range of 10–100 μg mL−1 has been observed (r2, 0.9999). Developed method has been found to be sensitive (limits of detection and quantification were 1.20 μg mL−1 and 3.60 μg mL−1, respectively), precise (the interday and intraday relative standard deviation (RSD) values for peak area and retention time were less than 0.4 and 0.2%, respectively), accurate (recovery, 99.19–100.17%), specific and robust (% RSD were less than 1.00, for system suitability parameters). Proposed method has been successfully applied for quantification of favipiravir in pharmaceutical formulations.

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Determination of Atenolol and Trimetazidine in Pharmaceutical Tablets and Human Urine Using a High Performance Liquid Chromatography-Photo Diode Array Detection Method

International Journal of Analytical Chemistry ◽

10.1155/2019/9625849 ◽

2019 ◽

Vol 2019 ◽

pp. 1-8 ◽

Cited By ~ 3

Author(s):

Walaa El-Alfy ◽

Omnia A. Ismaiel ◽

Magda Y. El-Mammli ◽

Abdalla Shalaby

Keyword(s):

Human Urine ◽

Limit Of Detection ◽

Pure Form ◽

Urine Samples ◽

Dihydrogen Phosphate ◽

Simple Liquid ◽

Pharmaceutical Tablets ◽

Limit Of Quantitation ◽

Precision And Accuracy

A simple RP-HPLC-PDA method for determination of atenolol (ATN) and trimetazidine (TMZ) in human urine and tablets has been developed. Analytes were separated on a Caltrex BI column (125× 4.0 mm, 5 μm) with 25mM potassium dihydrogen phosphate pH 3.3, methanol, and acetonitrile mobile phases. The PDA detector was operated at 210 nm for TMZ and 225 nm for ATN and the flow rate was 1.0 mL/ min. Linearity was obtained over a concentration range of (1.0-100 μg/mL) for both analytes in standard solutions and the method was successfully applied for determination of target analytes in their pharmaceutical tablets. Excellent linearity was also obtained over concentration ranges of (0.25-25 μg/mL) and (0.5-25 μg/mL) in human urine for TMZ and ATN, respectively. A simple liquid-liquid extraction was applied for urine sample clean-up and a gradient method was used for chromatographic separation. The lower limit of quantitation (LOQ) was 0.99 and 0.60 μg/mL for ATN and TMZ, respectively. The limit of detection (LOD) was 0.30 and 0.18 μg/mL for ATN and TMZ, respectively. Inter- and intraday precision and accuracy for ATN were within ±1.89% in pure form and within ±2.85% in urine samples. Inter- and intraday precision and accuracy for TMZ were within ± 3.99% in pure form and within ± 3.19% in urine samples.

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Stability-Indicating Method for Determination of Oxyphenonium Bromide and Its Degradation Product by High-Performance Liquid Chromatography

Journal of AOAC International ◽

10.1093/jaoac/90.5.1250 ◽

2007 ◽

Vol 90 (5) ◽

pp. 1250-1257 ◽

Cited By ~ 3

Author(s):

Alaa EL-Gindy ◽

Samy Emara ◽

Heba Shaaban

Keyword(s):

Degradation Product ◽

High Performance ◽

Potassium Dihydrogen Phosphate ◽

Order Rate Constant ◽

High Performance Liquid Chromatographic ◽

Hplc Method ◽

Dihydrogen Phosphate ◽

Stability Indicating Method ◽

Oxyphenonium Bromide

Abstract A high-performance liquid chromatographic (HPLC) method was developed for determination of oxyphenonium bromide (OX) and its degradation product. The method was based on the HPLC separation of OX from its degradation product, using a cyanopropyl column at ambient temperature with mobile phase of acetonitrile25 mM potassium dihydrogen phosphate, pH 3.4 (50 + 50, v/v). UV detection at 222 nm was used for quantitation based on peak area. The method was applied to the determination of OX and its degradation product in tablets. The proposed method was also used to investigate the kinetics of the acidic and alkaline degradation of OX at different temperatures, and the apparent pseudo first-order rate constant, half-life, and activation energy were calculated. The pH-rate profile of the degradation of OX in Britton-Robinson buffer solutions within the pH range 212 was studied.

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Urinary Excretion of Homocysteine-Thiolactone in Humans

Clinical Chemistry ◽

10.1373/clinchem.2004.042531 ◽

2005 ◽

Vol 51 (2) ◽

pp. 408-415 ◽

Cited By ~ 57

Author(s):

Grazyna Chwatko ◽

Hieronim Jakubowski

Keyword(s):

Urinary Excretion ◽

Human Body ◽

Human Urine ◽

Biological Fluids ◽

Hplc Method ◽

Biological Integrity ◽

Amino Group ◽

Urinary Ph ◽

Homocysteine Thiolactone ◽

Postcolumn Derivatization

Abstract Background: A metabolite of homocysteine (Hcy), the thioester Hcy-thiolactone, has been implicated in coronary heart disease in humans. Because inadvertent reactions of Hcy-thiolactone with proteins can lead to cell and tissue damage, the ability to detoxify or eliminate Hcy-thiolactone is essential for biological integrity. We examined the hypothesis that the human body eliminates Hcy-thiolactone by urinary excretion. Methods: We used a sensitive HPLC method with postcolumn derivatization and fluorescence detection to examine Hcy-thiolactone concentrations in human urine and plasma. Results: We discovered a previously unknown pool of Hcy-thiolactone in human urine. Urinary concentrations of Hcy-thiolactone (11–485 nmol/L; n = 19) were ∼100-fold higher than those in plasma (<0.1–22.6 nmol/L; n = 20). Urinary Hcy-thiolactone accounted for 2.5–28.3% of urinary total Hcy, whereas plasma Hcy-thiolactone accounted for <0.002–0.29% of plasma total Hcy. Urinary concentrations of Hcy-thiolactone, but not of total Hcy, were negatively correlated with urinary pH. Clearance of Hcy-thiolactone, relative to creatinine, was 0.21–6.96. In contrast, relative clearance of Hcy was 0.001–0.003. Conclusions: The analytical methods described here can be used to quantify Hcy-thiolactone in biological fluids. Using these methods we showed that the human body eliminates Hcy-thiolactone by urinary excretion. Our data also suggest that the protonation status of its amino group affects Hcy-thiolactone excretion.

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A validated stability-indicating RP-HPLC method for paracetamol and lornoxicam: Application to pharmaceutical dosage forms

Chemical Industry and Chemical Engineering Quarterly ◽

10.2298/ciceq120502106k ◽

2014 ◽

Vol 20 (1) ◽

pp. 109-114

Author(s):

Kulandaivelu Karunakaran ◽

Gurusamy Navaneethan ◽

Kuppanagounder Pitchaimuthu

Keyword(s):

Drug Product ◽

Potassium Dihydrogen Phosphate ◽

Reversed Phase ◽

Hplc Method ◽

High Dose ◽

Dihydrogen Phosphate ◽

Combination Drug ◽

Pharmaceutical Dosage Forms ◽

Column Temperature ◽

Stability Indicating

A new method for the simultaneous determination of paracetamol (PR) and lornoxicam (LR) has been developed by reversed phase HPLC from the combination drug product. The separation achieved on C18 column using acetonitrile and 0.02 M potassium dihydrogen phosphate was in the ratio of 35:65 (v/v) as mobile phase at a flow rate of 1.0 mL/min. Both the components were monitored at a single wavelength at 260 nm and the column temperature was maintained at 30?C throughout the analysis. A linear response was found in the concentration range of 125-375 ?g/mL for PR and 2-6 ?g/mL for LR, with the correlation coefficient of more than 0.999. Although the tablet contained a high dose of PR (500 mg) and a low dose of LR (8 mg), the single HPLC method was developed and the intra as well as inter day precision was obtained at less than 2% of RSD. The accuracy results obtained were between 98% and 102%. The drug was intentionally degraded under acidic, basic, peroxide, thermal, and photolytic conditions. The major degradation observed for both PR and LR under peroxide condition indicated that the drug product is susceptible to oxidation. The degraded peaks were properly resolved from PR and LR. Hence, the method is stability indicating.

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Simultaneous HPLC Determination of Chlordiazepoxide and Mebeverine HCl in the Presence of Their Degradation Products and Impurities

Journal of Chemistry ◽

10.1155/2015/293719 ◽

2015 ◽

Vol 2015 ◽

pp. 1-9

Author(s):

Rania N. El-Shaheny ◽

Fathalla F. Belal

Keyword(s):

Simultaneous Determination ◽

Degradation Product ◽

Mobile Phase ◽

Degradation Products ◽

Potassium Dihydrogen Phosphate ◽

Hplc Method ◽

Dihydrogen Phosphate ◽

Ir Studies ◽

Validation Procedure

A simple, rapid, and sensitive RP-HPLC method was developed and validated for the simultaneous determination of chlordiazepoxide (CDO) and mebeverine HCl (MBV) in the presence of CDO impurity (2-amino-5-chlorobenzophenone, ACB) and MBV degradation product (veratric acid, VER). Separation was achieved within 9 min on a BDS Hypersil phenyl column (4.5 mm × 250 mm, 5 µm particle size) using a mobile phase consisting of acetonitrile: 0.1 M potassium dihydrogen phosphate: triethylamine (35 : 65 : 0.2, v/v/v) in an isocratic mode at a flow rate of 1 mL/min. The pH of the mobile phase was adjusted to 4.5 with orthophosphoric acid and UV detection was set at 260 nm. A complete validation procedure was conducted. The proposed method exhibited excellent linearity over the concentration ranges of 1.0–100.0, 10.0–200.0, 2.0–40.0, and 2.0–40.0 µg/mL for CDO, MBV, VER, and ACB, respectively. The proposed method was applied for the simultaneous determination of CDO and MBV in their coformulated tablets with mean percentage recoveries of 99.75 ± 0.62 and 98.61 ± 0.38, respectively. The results of the proposed method were favorably compared with those of a comparison HPLC method using Studentt-test and the variance ratioF-test. The chemical structure of MBV degradation product was ascertained by mass spectrometry and IR studies.

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Validation of Simultaneous Volumetric and HPLC Methods for the Determination of Pridinol Mesylate in Raw Material

ISRN Pharmaceutics ◽

10.1155/2013/540676 ◽

2013 ◽

Vol 2013 ◽

pp. 1-5

Author(s):

Laura D. Simionato ◽

Leonardo Ferello ◽

Sebastián Stamer ◽

Patricia D. Zubata ◽

Adriana I. Segall

Keyword(s):

Mobile Phase ◽

Potassium Dihydrogen Phosphate ◽

Hplc Method ◽

Volumetric Method ◽

Raw Material ◽

Organic Layer ◽

Dihydrogen Phosphate ◽

Reverse Phase ◽

Potassium Dihydrogen

Simple, sensitive, and economical simultaneous volumetric and HPLC methods for the determination of pridinol mesylate in raw material have been developed. The volumetric method is based on the reaction of pridinol with sodium lauryl sulphate in diluted sulphuric acid. Dimethyl yellow was used as indicator to detect the end point of the titration in aqueous/organic layer. The HPLC method for the determination of pridinol mesylate employs a reverse phase C18 column at ambient temperature with a mobile phase consisting of acetonitrile: 0.05 M potassium dihydrogen phosphate, pH adjusted to 5.0 (1 : 2, v/v). The flow rate was 0.8 mL/min. Quantitation was achieved with UV detection at 258 nm based on peak area. Both methods were found to be suitable for the quality control of pridinol mesylate in raw material.

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The Determination of Metronidazole and Chlorhexidine Gluconate in Metronidazole and Chlorhexidine Lotion by HPLC

Journal of Physics Conference Series ◽

10.1088/1742-6596/2152/1/012016 ◽

2022 ◽

Vol 2152 (1) ◽

pp. 012016

Author(s):

Yun Yun ◽

Mingshi Lin

Keyword(s):

Potassium Dihydrogen Phosphate ◽

Hplc Method ◽

Chlorhexidine Gluconate ◽

Dihydrogen Phosphate ◽

Phosphate Solution ◽

Phase Detection ◽

Solution Ph ◽

Tetrabutylammonium Hydroxide ◽

Potassium Dihydrogen

Abstract Objective “To establish an HPLC method for the determination of metronidazole and chlorhexidine gluconate in metronidazole and chlorhexidine lotion. Method Using Agilent Eclipse-XDB-C18 chromatographic column, with 0.05 mol·L-1 potassium dihydrogen phosphate solution 1000 ml plus 13.2 ml 10% tetrabutylammonium hydroxide aqueous solution (pH adjusted to 3.5 by phosphoric acid)-acetonitrile (77:23) as Mobile phase, detection wavelength 230 nm. Results The two components could be separated well. The linear ranges of metronidazole and chlorhexidine acetate were 36.33~59.04 μg·ml-1 (r = 0.9994) and 35.45~220.11 μg·ml-1 (r = 1).); The average recoveries were 100.6% and 100.5 %, and the RSD were 0.42% and 0.58%. Conclusion: The method is simple and specific, and the result is more accurate and reliable. Which is suitable for simultaneous determination of two components in compound preparations.

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