scholarly journals Development and Validation of Ecofriendly HPLC-MS Method for Quantitative Assay of Amoxicillin, Dicloxacillin, and Their Official Impurity in Pure and Dosage Forms

2021 ◽  
Vol 2021 ◽  
pp. 1-9
Author(s):  
Atiah H. Almalki ◽  
Essraa A. Hussein ◽  
Ibrahim A. Naguib ◽  
Eglal A. Abdelaleem ◽  
Hala E. Zaazaa ◽  
...  
Keyword(s):  
High Performance ◽  
Assessment Method ◽  
Hplc Method ◽  
Liquid Chromatography Mass Spectrometry ◽  
Quadrupole Mass ◽  
Selected Ion Monitoring ◽  
Accuracy And Precision ◽  
Significant Difference ◽  
Amoxicillin Trihydrate ◽  
Development And Validation

Novel, accurate, selective, and rapid high-performance liquid chromatography mass spectrometry method was developed for simultaneous analysis of amoxicillin trihydrate, dicloxacillin sodium, and their official impurity 6-aminopenicillanic acid. The chromatographic separation was carried out by applying the mixture on a C18 column (3.5 µm ps, 100 mm × 4.6 mm id) using acetonitrile:water (65 : 35 by volume) as a mobile phase within only 4 min. The quantitative analysis was executed using single quadrupole mass spectrometer in which electrospray ionization, selected ion monitoring, and negative mode were operated. The retention times were 1.61, 2.54, and 3.50 mins for amoxicillin, 6-aminopenicillanic acid, and dicloxacillin, respectively. The method was validated in linear ranges of 2–28 µg mL−1, 2–35 µg mL−1, and 1–10 µg mL−1 for amoxicillin, dicloxacillin, and 6-aminopenicillanic acid, respectively. The results obtained from the suggested HPLC/MS were statistically compared with those obtained from the reported HPLC method, where no significant difference appeared respecting accuracy and precision. According to the analytical eco-scale assessment method, the proposed method was proved to be greener than the reported one, where the analysis time and the amount of the wasted effluent decreased.

Development and Validation of Two Chromatographic Methods for Simultaneous Determination and Quantification of Amiloride Hydrochloride, Hydrochlorothiazide, and Their Related Substances, in Pure and Tablet Forms

2020 ◽  
Vol 103 (3) ◽  
pp. 747-754
Author(s):  
Ibrahim A Naguib ◽  
Eglal A Abdelaleem ◽  
Fatma F Abdallah ◽  
Aml A Emam
Keyword(s):  
High Performance ◽  
Reversed Phase ◽  
Ammonia Solution ◽  
Hplc Method ◽  
Phosphoric Acid Solution ◽  
Related Substances ◽  
Rp Hplc ◽  
Significant Difference ◽  
Development And Validation ◽  
Amiloride Hydrochloride

Abstract Background Amiloride hydrochloride (AM) is a potassium sparing diuretic, while hydrochlorothiazide (HCZ) is the protype of thiazide diuretics. The combining of the studied drugs exhibits a synergistic effect. Moreover, HCZ prevents the potassium depletion side effect caused by AM. Objective Two accurate and precise simultaneous chromatographic separation methods were promoted and investigated to quantify AM, HCZ, official impurities of HCZ (cholorothiazide and salamide), and the official impurities of AM (methyl 3, 5-diamino-6-chloropyrazine-2-carboxylate). Methods The components of the quintuple mixture were quantified by two methods. The first method was high-performance thin layer chromatography (HPTLC), where exemplary separation was achieved on silica gel HPTLC F254 plates at the stationary phase using ethyl acetate–ethanol–ammonia solution (8 + 2 + 0.2, v/v) as a developing system. Scanning of bands at 273 nm was done. The second method was a reversed-phase chromatography (RP-HPLC) method using C18 (4.6 × 100 mm) column and mobile phase comprising 0.1% phosphoric acid solution–acetonitrile (90 + 10, v/v) with UV determination at 273 nm. Adjustment of the flow rate at 1 mL/min and pH at 3.6 was performed. Results Regarding RP-HPLC, optimum separation of the quintuple mixture was achieved within just five minutes. According to HPTLC, symmetric and sharp peaks were separated on the resulted chromatogram. Validity of the introduced methods was investigated by applying international conference on harmonization (ICH) guidelines. Conclusions The methods were successfully applied for assays of the studied drugs in their pure and tablet forms. No significant difference was revealed through application of statistical comparison between results of the suggested methods and those of the reported method regarding both accuracy and precision.

Determination of Selected Phthalates in Some Commercial Cosmetic Products by HPLC-UV

2020 ◽  
Vol 23 (10) ◽  
pp. 1010-1022
Author(s):  
Emrah Dural
Keyword(s):  
High Performance ◽  
Phthalate Esters ◽  
High Sensitivity ◽  
Hplc Method ◽  
Cosmetic Products ◽  
Limit Of Quantification ◽  
Nail Polish ◽  
Accuracy And Precision ◽  
Butyl Phthalate

Aim and scope: Due to the serious toxicological risks and their widespread use, quantitative determination of phthalates in cosmetic products have importance for public health. The aim of this study was to develop a validated simple, rapid and reliable high-performance liquid chromatography (HPLC) method for the determination of phthalates which are; dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl butyl phthalate (BBP), di-n-butyl phthalate (DBP), di(2- ethylhexyl) phthalate (DEHP), in cosmetic products and to investigate these phthalate (PHT) levels in 48 cosmetic products marketing in Sivas, Turkey. Materials and Methods: Separation was achieved by a reverse-phase ACE-5 C18 column (4.6 x 250 mm, 5.0 μm). As the mobile phase, 5 mM KH2PO4 and acetonitrile were used gradiently at 1.5 ml min-1. All PHT esters were detected at 230 nm and the run time was taking 21 minutes. Results: This method showed the high sensitivity value the limit of quantification (LOQ) values for which are below 0.64 μg mL-1 of all phthalates. Method linearity was ≥0.999 (r2). Accuracy and precision values of all phthalates were calculated between (-6.5) and 6.6 (RE%) and ≤6.2 (RSD%), respectively. Average recovery was between 94.8% and 99.6%. Forty-eight samples used for both babies and adults were successfully analyzed by the developed method. Results have shown that, DMP (340.7 μg mL-1 ±323.7), DEP (1852.1 μg mL-1 ± 2192.0), and DBP (691.3 μg mL-1 ± 1378.5) were used highly in nail polish, fragrance and cream products, respectively. Conclusion: Phthalate esters, which are mostly detected in the content of fragrance, cream and nail polish products and our research in general, are DEP (1852.1 μg mL-1 ± 2192.0), DBP (691.3 μg mL-1 ± 1378.5) and DMP (340.7 μg mL-1 ±323.7), respectively. Phthalates were found in the content of all 48 cosmetic products examined, and the most detected phthalates in general average were DEP (581.7 μg mL-1 + 1405.2) with a rate of 79.2%. The unexpectedly high phthalate content in the examined cosmetic products revealed a great risk of these products on human health. The developed method is a simple, sensitive, reliable and economical alternative for the determination of phthalates in the content of cosmetic products, it can be used to identify phthalate esters in different products after some modifications.

Selective Determination of Entecavir in the Presence of Its Oxidative Degradate by Spectrophotometric and Chromatographic Methods

2021 ◽  
Author(s):  
Heba M El-Sayed ◽  
Laila E Abdel Fattah ◽  
Hisham E Abdellatef ◽  
Maha A Hegazy ◽  
Mai M Abd El-Aziz
Keyword(s):  
High Selectivity ◽  
Oxidative Degradation ◽  
Hplc Method ◽  
Peak Amplitude ◽  
Quality Analysis ◽  
Official Method ◽  
Selective Determination ◽  
Significant Difference ◽  
Development And Validation

Abstract Background Entecavir (ENT) is an antiretroviral agent prescribed for treatment of HBV and HIV. Objective Development and validation of three simple, sensitive, selective, and precise methods for determination of ENT in presence of its oxidative degradation product (ENT deg.). Methods The first method was based on second derivative (D2) spectrophotometry through measuring the peak amplitude of D2 spectra at 293.6 nm. The second one is mean centering of the ratio spectra (MCR), which allowed measuring the peak amplitude at 280.0 nm. While the third method was HPLC; where ENT was separated from ENT deg. using Zobrax C18column and methanol: water (30:70, v/v), pH 3 as a mobile phase. The three developed methods were validated according to ICH guidelines. Results Linearity range of ENT was 5.00–50.00 μg/mL for both D2and MCR. However, higher sensitivity was achieved using HPLC (1.00–50.00 μg/mL). Accuracy of ENT were 100.60%±0.547, 101.55%±1.2071 and 100.61%±1.207 for D2, MCR and HPLC methods, respectively, and precision was within 1.280. Conclusions The developed methods were successfully applied for the determination of ENT in Tecavir® tablets without interference from ENT deg. They showed no significant difference compared with the official method as well as they could be applied in the quality analysis of ENT with high selectivity, accuracy, and precision. Highlights ENT was quantified using two spectrophotometric (D2 and MCR) methods and an HPLC method in presence of ENT deg. The proposed methods were applied to analysis of ENT tablets with high selectivity, sensitivity, and accuracy.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

Development and validation of a fast and simple HPLC method for the simultaneous determination of aniline and its degradation products in wastewater

2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Simple Method ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Development And Validation

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.

High performance liquid chromatography (HPLC) method development and validation for the determination of flunixin: Animal plasma based study

2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Mobile Phases ◽  
Hplc Method Development ◽  
Development And Validation

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.

DEVELOPMENT AND VALIDATION OF HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR SIMULTANEOUS ESTIMATION OF DEXTROMETHORPHAN HYDROBROMIDE AND QUINIDINE SULPHATE IN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (01) ◽  
pp. 35-40
Author(s):  
A. S. Bagde ◽  
V. V. Khanvilkar ◽  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Liquid Chromatography Method ◽  
Development And Validation ◽  
Dextromethorphan Hydrobromide

The present work describes a validated reverse phase high performance liquid chromatography (RPHPLC) method for simultaneous estimation of dextromethorphan hydrobromide and quinidine sulphate in pharmaceutical dosage from. The drugs were resolved using Hemochrom Intsil C18-5U column (250×4.6) mm in isocratic mode with mobile phase methanol: water (0.08% diethylamine, 0.02% of glacial acetic acid and pH 4.4 adjusted with orthophosphoric acid) in the ratio of 70:30 V/V at a flow rate of 1.0 mL/min. Retention time of dextromethorphan hydrobromide and quinidine sulphate were 4.9±0.2 and 3.6±0.2, respectively, at 292nm. The above mentioned method was validated as per International Conference on Harmonization (ICH) guidelines. Linear responses were obtained in concentration ranges of 5-35 μg/mL for dextromethorphan hydrobromide and 4-16 μg/mL for quinidine sulphate, with correlation coefficient (r2) of 0.999 for both the drugs. A simple, selective, accurate, precise, robust and reliable RP-HPLC method thus developed and validated for simultaneous estimation of dextromethorphan hydrobromide and quinidine sulphate.

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