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.

Simultaneous Liquid Chromatographic Determination of Water-Soluble Vitamins, Caffeine, and Preservative in Oral Liquid Tonics

1989 ◽  
Vol 72 (2) ◽  
pp. 244-247 ◽  
Author(s):  
Yumie Maeda ◽  
Masatoshi Yamamoto ◽  
Kazuhiro Owada ◽  
Shiro Sato ◽  
Hiroyuki Nakazawa
Keyword(s):  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Water Soluble ◽  
Dihydrogen Phosphate ◽  
Coefficients Of Variation ◽  
Oral Liquid ◽  
Liquid Chromatographic

Abstract A rapid, simple, and reliable liquid chromatographic method has been developed for the simultaneous determination of nicotinamide (niacinamide), thiamine, riboflavin, riboflavin sodium phosphate, pyridoxine, caffeine, and sodium benzoate in commercial oral liquid tonics. The 7 components are separated on a reverse phase C18 column using a mobile phase of acetonitrile-O.OlM potassium dihydrogen phosphate-triethylamine (8 + 91.5 + 0.5 v/v/v) containing 5mM sodium octanesulfonate and adjusted to pH 2.8 with phosphoric acid. Components are detected at 254 nm with attenuation 0.02 AUFS. Acetanilide is used as an internal standard. In addition to the 7 components mentioned, nicotinic acid (niacin), cyanocobalamin, and folic acid are also separated under the same conditions. Sample preparation involves only addition to internal standard solution and dilution with mobile phase and then filtration. Recoveries of the 7 components and cyanocobalamin from spiked preparations ranged from 97 to 104% with coefficients of variation of 0.9-4.2%.

scholarly journals Determination of amino acid profile for argininosuccinic aciduria disorder using High-Performance Liquid Chromatography with fluorescence detection

2020 ◽  
Author(s):  
Hossein Salmanizadeh ◽  
Neda Sahi
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Amino Acid ◽  
Fluorescence Detection ◽  
Mobile Phase ◽  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Amino Acid Profile ◽  
Dihydrogen Phosphate ◽  
Argininosuccinic Aciduria

Argininosuccinic aciduria is an autosomal, recessive amino acid disorder that is caused by a deficiency of the argininosuccinate lyase enzyme. Citrulline is the most significant marker to detect this disorder. We used the High-performance liquid chromatography with fluorescence detection with 450 nm emission and 330 nm excitation wavelengths, 15 mmol/L potassium dihydrogen phosphate and 5 mmol/L dipotassium hydrogen phosphate as Mobile Phase A, and 50 mL water, 250 mL acetonitrile, and 200 mL methanol as Mobile Phase B in gradient mode with flow rate of 1.2 mL/min. The citrulline concentration was 22 µmol/L in healthy infants and 220 µmol/L in infants suffering from the disorder.

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 Stability indicating HPLC-Fluorescence detection method for the simultaneous determination of linagliptin and empagliflozin in their combined pharmaceutical preparation

2021 ◽  
Vol 12 (2) ◽  
pp. 168-178
Author(s):  
Mohamed Rizk ◽  
Ali Kamal Attia ◽  
Heba Yosry Mohamed ◽  
Mona Elshahed
Keyword(s):  
Fluorescence Detection ◽  
Mobile Phase ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Significant Difference

A sensitive, accurate, and precise liquid chromatographic method has been developed and validated for the determination of Linagliptin (LNG) and Empagliflozin (EMP) in their combined tablets. Chromatographic separation was carried out on ODS-3 Inertsil® C18 column (150×4.6 mm, 5 µm). The mobile phase A (consisting of 0.30% Triethyl amine buffer (TEA) at pH = 4.5, adjusted using ortho-phosphoric acid); the mobile phase B (consisting of acetonitrile) was pumped through the column whose temperature was maintained at 40 °C, with a flow rate 1.7 mL/min, using gradient elution from 0-3 min A:B (75:25, v:v), then from 3-6 min the ratio changed to be A:B (60:40, v:v). Fluorescence detection (FLD) was performed at 410 nm after excitation at 239 nm. Acceptable linearity, accuracy and precision values of the proposed method were found over the concentration ranges of 0.5-15 µg/mL for LNG and 1.0-30 µg/mL for EMP with correlation coefficients of 0.9997 and 0.9998 in the case of LNG and EMP, respectively. The recoveries and relative standard deviations percentages were found in the following ranges: 98.56-101.85 and 0.53-1.52% for LNG and 98.00-101.95 and 0.31-1.05% for EMP. The detection and quantification limits were 0.15 and 0.45 µg/mL for LNG and 0.22 and 0.67 µg/mL for EMP. The optimized method was validated and proved to be specific, robust, accurate and reliable for the determination of the drugs in pure form or in their combined pharmaceutical preparations. No significant difference was found regarding accuracy and precision upon statistical comparison between the obtained results of the proposed method and those of the reported method. Furthermore, the proposed method is proved to be a stability-indicating assay after exposure of the studied drugs to variable forced degradation parameters, such as acidic, alkaline and oxidative conditions, according to the recommendations of the International Conference on Harmonization guidelines. The simplicity and selectivity of the proposed method allows its use in quality control laboratories.

Improved liquid-chromatographic determination of haloperidol in plasma.

1984 ◽  
Vol 30 (7) ◽  
pp. 1228-1230 ◽  
Author(s):  
A K Dhar ◽  
H Kutt
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Room Temperature ◽  
Internal Standard ◽  
Isoamyl Alcohol ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract This method for determination of haloperidol in plasma is based on "high-performance" isocratic liquid chromatography with the use of a C8 bonded reversed-phase column at room temperature. Haloperidol and the internal standard (chloro-substituted analog) are extracted from alkalinized plasma into isoamyl alcohol/heptane (1.5/98.5 by vol) and back-extracted into dilute H2SO4. The aqueous phase is directly injected onto the column. The mobile phase is a 30/45/25 (by vol) mixture of phosphate buffer (16.5 mmol/L, pH 7.0), acetonitrile, and methanol. Unlike other liquid-chromatographic procedures for haloperidol, commonly used psychotropic drugs do not interfere. Analysis can be completed within an hour. The procedure is extremely sensitive (1.0 microgram/L) and is well reproducible (CV 5.6% for a 2.5 micrograms/L concentration in plasma).

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.

High Performance Liquid Chromatographic Determination of Primidone in Tablets

1982 ◽  
Vol 65 (5) ◽  
pp. 1063-1065
Author(s):  
Stanley E Roberts
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Average Recovery ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic (HPLC) method is described for the quantitative determination of primidone in tablets. A ground tablet sample is diluted directly in the mobile phase, at a concentration of about 1 mg/mL of primidone, mixed and deaerated, and filtered. The resulting solution is then quantitated by HPLC. The average spike recoveries for the 50 mg and 250 mg tablets were 101.2% and 99.0%, respectively. The average recovery for an authentic mixture formulated at the 250 mg level was 100.1% with a relative standard deviation of 0.45%.

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