Detection and Evaluation of process related impurities in Obeticholic Acid Drug material using HPLC Method

2021 ◽  
pp. 5618-5624
Author(s):  
Kishore Gaddam ◽  
Srinivas Kumbam ◽  
Trivikram Reddy Gundala ◽  
Surendranath Reddy Reddiwary ◽  
Gangi Reddy Nallagondu Chinna
Keyword(s):  
Orthophosphoric Acid ◽  
Detection Method ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Biliary Cirrhosis ◽  
Potassium Phosphate Buffer ◽  
Obeticholic Acid ◽  
Related Substances ◽  
Refractive Index Detection

Obeticholic acid (OBE) is being used to treat primary biliary cirrhosis and cholangitis. An HPLC with refractive index detection method for eight process related substances of OBE was developed and verified for use in quality assurance laboratories for regular analysis. The separation and analysis were performed on YMC Triart C18 (3.0 µm particle size, 250 mm × 4.6 mm) column. Mobile phase employed consisted of 0.01N potassium phosphate buffer (3.0 ± 0.05 pH, set with 0.1% orthophosphoric acid) and acetonitrile at 45:55 (v/v) ratio. The method established for determination of eight impurities in OBE was validated and verified in keeping with International Council for Harmonisation guidelines. This method can be used for routine analysis of eight impurities in OBE bulk samples.

HPLC method for measurement of purine nucleotide degradation products in cerebrospinal fluid

1996 ◽  
Vol 42 (5) ◽  
pp. 756-760 ◽  
Author(s):  
L Kuracka ◽  
T Kalnovicová ◽  
B Líska ◽  
P Turcáni
Keyword(s):  
Cerebrospinal Fluid ◽  
Uric Acid ◽  
Neurological Disorders ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Potassium Phosphate Buffer ◽  
Nucleotide Degradation

Abstract We describe a convenient method for the separation and quantification of xanthine, hypoxanthine, and uric acid in 20 microL of cerebrospinal fluid (CSF) with use of HPLC and ultraviolet detection. The analysis is performed on a Sepharon SGX C18 column and the elution system consists of potassium phosphate buffer, pH 5.1, with 20 mL/L methanol. The lower limit of detection was 4 pmol for hypoxanthine and xanthine and 6 pmol for uric acid. Analytical recoveries of purine metabolites ranged from 98.6% to 102.9%. The intra- and interassay CVs were <3%. The applicability of the method is illustrated with the determination of micromolar concentrations of xanthine, hypoxanthine, and uric acid in CSF samples obtained from 113 patients with various neurological disorders.

scholarly journals Development and Validation of an HPLC Method for Mefloquine Hydrochloride Determination in Tablet Dosage Form

2011 ◽  
Vol 94 (4) ◽  
pp. 1089-1093 ◽  
Author(s):  
Fernando Henrique Andrade Nogueira ◽  
Letícia De Paula Lana Goulart ◽  
Isabela Da Costa César ◽  
Lígia Maria Moreira De Campos ◽  
Gérson Antônios Pianetti
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Stability Studies ◽  
Potassium Phosphate Buffer ◽  
Photolytic Degradation ◽  
Development And Validation ◽  
Tablet Dosage

Abstract A simple HPLC method for determination of mefloquine hydrochloride in tablets was developed and validated. The separation was carried out on an Xterra RP18 (250 × 4.6 mm id, 5 µm particle size) analytical column. The mobile phase was 0.05 M monobasic potassium phosphate buffer (pH 3.5)–methanol (40 + 60, v/v). The flow rate and wavelength were set to 1 mL/min and 283 nm, respectively. The method was specifc for mefloquine hydrochloride in the presence of hydrolytic, oxidative, and photolytic degradation products. It was also linear, precise, accurate, and robust, being suitable for routine QC analyses and stability studies. The developed HPLC method was compared to a previously described spectrophotometric method.

scholarly journals HPLC Determination of Majdine in Vinca herbacea

2011 ◽  
Vol 6 (12) ◽  
pp. 1934578X1100601
Author(s):  
Natia Gagua ◽  
Beatrice Baghdikian ◽  
Fathi Mabrouki ◽  
Riad Elias ◽  
Valentina Vachnadze ◽  
...  
Keyword(s):  
Quality Control ◽  
Chromatographic Separation ◽  
Phosphate Buffer ◽  
Potassium Phosphate ◽  
Solvent System ◽  
Hplc Method ◽  
Potassium Phosphate Buffer ◽  
Good Linear ◽  
Linear Behavior

A reliable HPLC method coupled with DAD detection was developed and validated for determination of majdine in Vinca herbacea. The chromatographic separation was carried out on a Symmetry C18 column (250 mm x 4.6 mm, 5 μm, Waters) with an isocratic solvent system of 25 mM potassium phosphate buffer (pH=3.0)-acetonitrile. UV detection was performed at 225 nm. Good linear behavior over the investigated concentration range was observed with the value of r2 > 0.9978. The method was reproducible with intra- and inter-day variations of less than 4.38%. The proposed method was linear, accurate, precise and specific. The validated method was successfully applied to quantify majdine in various parts of V. herbacea, which was collected during the flowering months of April and May. The results indicated that the developed HPLC method could be used for the quality control of V. herbacea and for the standardization of its extracts in majdine.

A comparative technique using as Joint studying to prove structure and determination the Quantitative estimation of organic compound (Irbesartan) as drug in multicomponent tablet form

2019 ◽  
Vol 9 (o3) ◽  
Author(s):  
Imad Tarek Hanoon ◽  
Abed Mohammed Daheir AL-Joubory 2 ◽  
Marwa Mohamed Saied 3
Keyword(s):  
Mobile Phase ◽  
Chemical Structure ◽  
Quantitative Estimation ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Tablet Form ◽  
Rp Hplc ◽  
Percent Recovery

A simple , specific, accurate and precise RP-HPLC method was developed for determination of Irbesartan (IRB) in pharmaceutical dosage forms in tablets products and sachet using symmetry (L 1 ) column at 30°C . The signal was detected at 225 nm. A mobile phase dissolve 0.5 g of buffer potassium phosphate in 100 ml distilled water and adjust pH 2.7 , methanol and acetonitrile at ratio (40 :30 :30 ) . and flow rate 1.2ml/min -1 at pH=7.2 a mobile phase The percent recovery was detected 101 % and the linearity of concentration was 10-50 µg.ml -1 and supported this method by using (FT.I.R.) spectrum method for organic spectrophotometer to prove the chemical structure of this drug and some physical properties . we are obtained the result is identical of other literature . The proposed method was applied successfully for determination of the IRB in tablets products.

scholarly journals SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Internal Diameter ◽  
Related Substances ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

scholarly journals Validation of a Stability-Indicating RP-HPLC Method for the Determination of Entecavir in Tablet Dosage Form

2010 ◽  
Vol 93 (2) ◽  
pp. 523-530 ◽  
Author(s):  
Sérgio Luiz Dalmora ◽  
Maximiliano da Silva Sangoi ◽  
Daniele Rubert Nogueira ◽  
Lucélia Magalhães da Silva
Keyword(s):  
Dosage Form ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Forced Degradation ◽  
Photodiode Array Detection ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Tablet Dosage

Abstract An RP-HPLC method was validated for the determination of entecavir in tablet dosage form. The HPLC method was carried out on a Gemini C18 column (150 4.6 mm id) maintained at 30C. The mobile phase consisted of acetonitrilewater (95 + 5, v/v)/potassium phosphate buffer (0.01 M, pH 4; 9 + 91, v/v) pumped at a flow rate of 1.0 mL/min. Photodiode array detection was at 253 nm. The chromatographic separation was obtained with a retention time of 4.18 min, and the method was linear in the range of 0.5200 g/mL (r2 0.9998). The specificity and stability-indicating capability of the method was proven through forced degradation studies, which also showed that there was no interference of the excipients and an increase of the cytotoxicity only by the basic condition. The accuracy was 101.19, with bias lower than 1.81. The LOD and LOQ were 0.39 and 0.5 g/mL, respectively. Method validation demonstrated acceptable results for precision and robustness. The proposed method was applied for the analysis of tablet formulations, to improve QC and assure therapeutic efficacy.

P-Nitrophenol-alpha-D-glucopyranoside as substrate for measurement of maltase activity in human semen.

1978 ◽  
Vol 24 (2) ◽  
pp. 208-211 ◽  
Author(s):  
P Chapdelaine ◽  
R R Tremblay ◽  
J Y Dubé
Keyword(s):  
Seminal Plasma ◽  
Reduced Glutathione ◽  
Rapid Determination ◽  
Potassium Phosphate ◽  
Potassium Phosphate Buffer ◽  
Michaelis Constant ◽  
Maltase Activity ◽  
Constant Rate ◽  
Hydrolysis Of

Abstract Hitherto, seminal plasma maltase has been measured with maltose as substrate; this method is time consuming and lacks specificity. The use of a synthetic substrate, p-nitrophenol-alpha-D-glucopyranoside, allows accurate and rapid determination of this activity. When maltase is added to the incubation medium (the substrate and reduced glutathione in potassium phosphate buffer, pH 6.8), maintained at 37 degrees C, hydrolysis of the original substrate to p-nitrophenol goes at a constant rate during 4 h. Under optimal conditions of incubation, the Michaelis constant of the reaction, calculated by the Hanes method, was 2.92 +/- 0.84 (SD) X 10(-3) for six different semen samples. Isomaltase appeared to be absent from seminal plasma. The enzyme is stable to freezing and slow thawing and can be stored for at least 26 days at -80 degrees C. Its molecular weight is 259 000. Tris(hydroxymethyl)aminomethane (pH 6.8) exerts a noncompetitive inhibition on the enzyme activity. In 68 men 23 to 45 years old, whose semen analyses were normal, the seminal plasma maltase activity was 467 +/- 135 (SD) mU/g of protein. It was generally decreased in patients with infertility disorders.

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