scholarly journals Validated Simultaneous Gradient Ultra-Performance Liquid Chromatographic Quantification of Some Proton Pump Inhibitor Drug Residues in Saudi Pharmaceutical Industrial Wastewater

Molecules ◽  
2021 ◽  
Vol 26 (14) ◽  
pp. 4358
Author(s):  
Sherif A. Abdel-Gawad ◽  
Hany H. Arab ◽  
Alhumaidi B. Alabbas
Keyword(s):  
Proton Pump ◽  
Industrial Wastewater ◽  
Mobile Phase ◽  
Solid Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Ultra Performance Liquid Chromatography ◽  
Dihydrogen Phosphate ◽  
Separation Pattern ◽  
Inhibitor Drug ◽  
Wastewater Samples

Monitoring and quantification of active pharmaceutical ingredients (APIs) in the environment constitute important and challenging tasks, as they are directly associated with human health. Three commonly used proton pump inhibitors (PPIs), namely, omeprazole sodium (OMP), pantoprazole sodium (PNT), and lansoprazole sodium (LNZ) are well separated and quantified using ultra-performance liquid chromatography (UPLC) in pharmaceutical industrial wastewater. The separation of the studied drugs was performed on a stationary phase with a WatersTM column (100 × 2.1 mm, 1.7 µm). The mobile phase was composed of methanol:0.05 M potassium dihydrogen phosphate buffer (adjusted to pH 7.5 using NaOH) (50:50, v/v). The elution process was done in gradient mode by changing the relative proportions of the mobile phase components with time to get an optimum separation pattern. The flow rate of the developing system was adjusted to 0.8 mL/minute. Detection of the separated drugs was performed at 230 nm. The studied drugs were quantified in the concentration range of 10–200 ng/mL for all drugs. The cited method was fully validated according to the international conference on harmonization (ICH-Q2B) guidelines, then it was applied successfully for quantification of the studied PPIs in real wastewater samples after their solid phase extraction (SPE).

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

2021 ◽  
pp. 281-294 ◽  
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.

scholarly journals Simultaneous Assay of Olanzapine and Fluoxetine in Tablets by Column High-Performance Liquid Chromatography and High-Performance Thin-Layer Chromatography

2007 ◽  
Vol 90 (6) ◽  
pp. 1573-1578 ◽  
Author(s):  
Charmy R Shah ◽  
Nehal J Shah ◽  
Bhanubhai N Suhagia ◽  
Natvarlal M Patel
Keyword(s):  
Thin Layer ◽  
Mobile Phase ◽  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
High Performance Liquid Chromatographic ◽  
Ultraviolet Absorption ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Aluminum Sheets ◽  
Tablet Formulations

Abstract This paper describes validated high-performance liquid chromatographic (LC) and high-performance thin-layer chromatographic (TLC) methods for the simultaneous estimation of olanzapine and fluoxetine in pure powder and tablet formulations. The LC separation was achieved on a Lichrospher 100 RP-180, C18 column (250 mm, 4.0 mm id, 5 m) using 0.05 M potassium dihydrogen phosphate buffer (pH 5.6 adjusted with o-phosphoric acid) acetonitrile (50 + 50, v/v) as the mobile phase at a flow rate of 1 mL/min and ambient temperature. The TLC separation was achieved on aluminum sheets coated with silica gel 60F254 using methanoltoluene (40 + 20, v/v) as the mobile phase. Quantitation was achieved by measuring ultraviolet absorption at 233 nm over the concentration range of 1070 and 40280 g/mL with mean recovery of 99.54 0.89 and 99.73 0.58% for olanzapine and fluoxetine, respectively, by the LC method. Quantitation was achieved by measuring ultraviolet absorption at 233 nm over the concentration range of 100800 and 4003200 ng/spot with mean recovery of 101.53 0.06 and 101.45 0.35% for olanzapine and fluoxetine, respectively, by the TLC method with densitometry. These methods are simple, precise, and sensitive, and they are applicable for simultaneous determination of olanzapine and fluoxetine in tablet formulations.

scholarly journals High-Performance Liquid Chromatographic Determination of Dihydroergocristine in a Pharmaceutical Formulation with Fluorescence Detection

2010 ◽  
Vol 93 (1) ◽  
pp. 97-101
Author(s):  
Michal Douša ◽  
Michaela Dubovská
Keyword(s):  
Fluorescence Detection ◽  
Mobile Phase ◽  
High Performance ◽  
Pharmaceutical Preparation ◽  
Potassium Dihydrogen Phosphate ◽  
Sample Pretreatment ◽  
Chromatographic Determination ◽  
Hplc Determination ◽  
Dihydrogen Phosphate

Abstract A rapid procedure based on a direct extraction and HPLC determination of dihydroergocristine in a pharmaceutical preparation with fluorescence detection has been developed and validated. The optimized chromatographic conditions included a Purospher RP18e column, 5 µm particle size, 250 4.0 mm, and 25 mM potassium dihydrogen phosphate buffer (pH 2.8)acetonitrile (60 + 40, v/v) mobile phase at a flow rate of 1 mL/min. The separation was carried out at 50C, and the injection volume was 5 L. Fluorescence detection was performed at an excitation and emission wavelength of 224 and 344 nm, respectively. The mobile phase parameters such as organic solvent composition, temperature, and pH were studied. The proposed method has the advantages of a very simple sample pretreatment and fast HPLC determination.

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

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.

Simultaneous Determination of 11 Aminoglycoside Residues in Honey, Milk, and Pork by Liquid Chromatography with Tandem Mass Spectrometry and Molecularly Imprinted Polymer Solid Phase Extraction

2017 ◽  
Vol 100 (6) ◽  
pp. 1869-1878 ◽  
Author(s):  
Bixia Yang ◽  
Lian Wang ◽  
Chunying Luo ◽  
Xixi Wang ◽  
Chengjun Sun
Keyword(s):  
Simultaneous Determination ◽  
Molecularly Imprinted Polymer ◽  
Solid Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Dihydrogen Phosphate ◽  
Imprinted Polymer ◽  
Ionization Source ◽  
Molecularly Imprinted ◽  
Potassium Dihydrogen

Abstract An analytical method was developed for the simultaneous determination of 11 aminoglycoside (AG) antibiotics, including amikacin, paromomycin, dihydrostreptomycin, gentamicin C1a, hygromycin, kanamycin, netilmicin, spectinomycin, sisomicin, streptomycin, and tobramycin in honey, milk, and pork samples by LC with tandem MS and molecularly imprinted polymer (MIP) SPE. The AG antibiotics in milk and homogenated meat samples were extracted with a solution composed of 10 mmol/L potassium dihydrogen phosphate, 0.4 mmol/L EDTA-Na2, and 2% trichloroacetic acid. For honey samples, the extractant was 50 mmol/L potassium dihydrogen phosphate. The extracts were cleaned up with MIP SPE cartridges. The separation was performed on a zwitter ionic-HILIC column (50 × 2.1 mm, 3.5 μm), with the mobile phase consisting of methanol, 0.3% formic acid, and 175 mmol/L ammonium formate at 0.50 mL/min in gradient elution. A triple-quadrupole mass spectrometer equipped with an electrospray ionization source, which was operated in positive mode, was used for detection. The quantification was based on matrix-matched calibration curves. The method was applied to real samples with three different matrixes. The LODs of the method were 2–30 μg/kg and the LOQs were 7–100 μg/kg; the average recovery ranged from 78.2 to 94.8%; intraday RSDs and interday RSDs were ≤15 and ≤18%, respectively; and the absolute values of matrix effect for all AGs were RSDs ≤23%.

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

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.

scholarly journals KH2PO4 crystallisation from potassium chloride and ammonium dihydrogen phosphate

2016 ◽  
Vol 18 (1) ◽  
pp. 1-8 ◽  
Author(s):  
Kristina Jančaitienė ◽  
Rasa Šlinkšienė
Keyword(s):  
Aqueous Solutions ◽  
Potassium Chloride ◽  
Solid Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Molar Ratio ◽  
Dihydrogen Phosphate ◽  
Ammonium Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Increasing Temperature ◽  
Nitrogen Phosphorus

Abstract Seeking to obtain bulk (NPK – nitrogen, phosphorus, potassium), chlorine-free fertilizers, the influence of interaction between potassium chloride and ammonium dihydrogen phosphate in aqueous solutions at temperature of 20, 40, 60 and 80°C has been investigated. Components of the solid phase have been identified by methods of chemical and instrumental analysis: radiography (X – ray), infra – red molecular absorption spectroscopy (IR) and scanning electron microscopy (SEM). It has been observed that the largest amount of solid state potassium dihydrogen phosphate was obtained at 60–80°C, when the potassium chloride and ammonium dihydrogen phosphate molar ratio is equal 0.8:0.2. Changing the molar ratio of 0.5:0.5 to 0.8:0.2, and with increasing temperature, various shaped crystals have developed in the remaining aqueous solutions with a morphology shifting from sharp needles to tetragonal prism.

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