scholarly journals Derivatization and Spectrophotometric Quantification of Pamidronate in Bulk and Dosage Forms

2020 ◽  
pp. 40-46
Author(s):  
Sherif A. Abdel- Gawad
Keyword(s):  
Quality Control ◽  
Method Validation ◽  
Heating Time ◽  
Dosage Forms ◽  
Optimum Temperature ◽  
Reaction Conditions ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Optimum Ph ◽  
Optimum Heating

Aims: To quantify pamidronate in a sensitive and accurate way either in bulk or dosage forms. Methodology: The quantification of this group of drugs is a challenging task as they lack the presence of chromophore groups in their structure. The proposed method depends on the derivatization of the studied drug by its reaction with 4-Chloro-7-nitro-2,1,3-benzoxazole and the product is measured spectrophotometrically at 470 nm. The conditions for the reaction are optimized regarding the volume of the reagent, the optimum pH for the reaction completion, the buffer volume, the optimum temperature for the reaction and the optimum heating time. Results: The studied drug can be determined in the range of 9-30 µg/mL after optimizing the reaction conditions. Method validation is performed according to ICH guidelines and different validation parameters like, linearity, accuracy, precision and robustness are calculated and found to be excellent. Conclusion: The proposed method is accurate, sensitive and can be applied for the routine analysis of pamidronate in quality control laboratories.

scholarly journals Analysis of Flavonoids and Iridoids in Vitex Negundo by HPLC-PDA and Method Validation

2013 ◽  
Vol 8 (9) ◽  
pp. 1934578X1300800
Author(s):  
Somendu K. Roy ◽  
Khemraj Bairwa ◽  
Jagdeep Grover ◽  
Amit Srivastava ◽  
Sanjay M. Jachak
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Method Validation ◽  
Hplc Method ◽  
Vitex Negundo ◽  
Good Recovery ◽  
Bioactive Constituents ◽  
Ich Guidelines ◽  
Validation Parameters

The leaves of Vitex negundo have been reported to contain various bioactive constituents including iridoids and flavonoids. This is the first report on the simultaneous determination of iridoids and flavonoids by HPLC in three different samples of V. negundo leaves collected from three regions of India. Separation of iridoids and flavonoids was accomplished by HPLC and further elaborated for their quantification in V. negundo leaves using a C-18 column with detection at 254 and 330 nm, respectively. The developed HPLC method showed good linearity (r2≥0.999), high precision (RSD<5%) and a good recovery (99.3–103.0%) of the compounds. All the validation parameters of the developed HPLC were found to be within the permissible limits according to the ICH guidelines. The developed method was robust, accurate and reliable for the quality control of V. negundo leaves.

scholarly journals Pemanfaatan Gulma Siam (Chromolaena odarata L.) Sebagai Adsorben Logam Timbal

2020 ◽  
Vol 2 (1) ◽  
pp. 27-34
Author(s):  
Erni Mohamad ◽  
Intan J. Oputu ◽  
Julhim S. Tangio
Keyword(s):  
Activated Carbon ◽  
Activated Charcoal ◽  
Heating Time ◽  
Ion Adsorption ◽  
Chromolaena Odorata ◽  
Carbon Quality ◽  
Industry Standard ◽  
Optimum Ph ◽  
Optimum Heating ◽  
Time Required

This study aims to utilize (Chromolaena odorata L) as a metal adsorbent. The methods used to make activated charcoal are dehydration, carbonization, and activation. The activated carbon is then characterized to obtain activated charcoal that can be applied, then optimized. The results of activated carbon characterization obtained have reached the activated carbon quality requirements based on the Indonesian Industry Standard (SII No. 0258-88). Based on the adsorption test, the optimum pH of Pb2+ (Pb (NO3) 2 (in distilled water) Chromolaena odorata L charcoal activated by NaOH 0.2 M under varying pH (2,3,4,5,6) is at pH 5 with 69.00% absorption. The optimum contact time required for Pb ion adsorption is 4 hours at variation (1-5 hours) with 70.19% absorption. The optimum concentration at variation (concentration 20; 40; 60; 80; 100 ppm) on Pb ion adsorption is 100 ppm with 76.15% absorption. The optimum heating time is a variation of 1.5; 2; 2.5; and 3 hours of Pb ion adsorption is one hour 30 minutes with an absorption of 65.95%. Based on the optimization results, the activated carbon from the Chromolaena odorata L can be used as an adsorption material against the contamination of lead heavy metals (Pb).

Key Aspects of Analytical Method Development and Validation

2019 ◽  
Vol 31 (1) ◽  
pp. 32-39
Author(s):  
Suman Shrivastava ◽  
Pooja Deshpande ◽  
S. J. Daharwal
Keyword(s):  
Method Validation ◽  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Key Aspects ◽  
Development And Validation

Development of a method is crucial for discovery, development, and analysis of medicines in the pharmaceutical formulation. Method validation could also be thought to be one in all the foremost well-known areas in analytical chemistry as is reproduced within the substantial variety of articles submitted and presented in peer review journals every year. Validation of an analytical procedure is to demonstrate that it's appropriate for its intended purpose. Results from method validation are often wont to decide the quality, reliability and consistency of analytical results. Analytical methods need to be validated or revalidated. This review describes general approach towards validation process and validation parameters to be considered during validation of an analytical method. It also refers to various regulatory requirements like WHO, USFDA, EMEA, ICH, ISO/IEC. The parameters described here are according to ICH guidelines which include accuracy, precision, specificity, limit of detection, limit of quantification, linearity range and robustness.

scholarly journals A Selective and Sensitive Method for Simultaneous Quantification of Genotoxic Impurities in Penciclovir drug substance and its dosage forms using UPLC-MS/MS

2020 ◽  
Vol 11 (4) ◽  
pp. 5772-5776
Author(s):  
Rao P.Y.G ◽  
Sreenivasa Rao B ◽  
Suresh Reddy K.V.N ◽  
Sudhakar Ch
Keyword(s):  
Limit Of Detection ◽  
High Sensitivity ◽  
Dosage Forms ◽  
Drug Substance ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Genotoxic Impurities ◽  
Chromatographic Parameters ◽  
Sensitive Method ◽  
Bromo Compound

A selective, rapid and sensitive method was developed for the determination of genotoxic impurities (2-Amino-6-chloro purine and Bromo compound) in Penciclovir drug substance using RPUPLC-MS/MS. The chromatographic separation was performed on Kromasil C8 column (150 mm x 4.6 mm, 5 μm) maintained at 45°C using 0.1%formic acids in water as buffer and acetonitrile through gradient programme. The flow rate was maintained at 0.5mL/min with an injection volume of 10 μL. For the quantification of genotoxic impurities, positive-electrospray ionisation (ESI) mode was selected. Penciclovir and its impurities were well separated within the shortest run time of 16min. The chromatographic method was developed, and the results of all validation parameters showed that the technique is well confined to the limits of ICH guidelines. The method has high sensitivity, and the limit of detection was found to be as low as 0.15 and 0.30 ppm for 2-Amino-6-chloro purine and Bromo compound. The recovery of 2-Amino-6-chloro purine and Bromo compound are found in the range of 80-120%. The linearity of peak area versus concentration was demonstrated in the range of LOQ - 150% level of impurities with a correlation coefficient of 0.9999. The method has proved too robust by introducing minuscule changes in the chromatographic parameters. The method was successfully validated and applied for Penciclovir drug substances and their dosage forms to determine the mentioned genotoxic impurities.

scholarly journals Simultaneous Spectrophotometric Estimation of Telmisartan and Amlodipine Besylate in Tablet Dosage Form

2015 ◽  
Vol 3 (03) ◽  
pp. 50-54 ◽  
Author(s):  
N. K. Gupta ◽  
A. Peepliwal ◽  
D. S. Rathore ◽  
P. Gupta
Keyword(s):  
Quality Control ◽  
Dosage Form ◽  
Simultaneous Equation ◽  
Dosage Forms ◽  
Simultaneous Estimation ◽  
Amlodipine Besylate ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Tablet Dosage ◽  
Routine Quality Control

A simple, accurate and reproducible spectrophotometric methods have been developed for the simultaneous estimation of Telmisartan (TEL) and Amlodipine Besylate (AML) in combined tablet dosage forms. The method involves determination using the simultaneous equation method, the sampling wavelengths selected are ‘TLM’ = 297nm.and ‘AML’ =238nm., over the concentration ranges of 8-48μg/ml for ‘TEL’ and 1-6 μg/ml for ‘AML’ respectively. The method was validated for linearity, accuracy, precision, robustness and application for assay as per ICH guidelines. The proposed method is simple, economical, accurate and precise, and could be successfully employed in routine quality control for the simultaneous analysis of Telmisartan (TEL) and Amlodipine Besylate (AML).

scholarly journals NOVEL HPTLC-DENSITOMETRIC METHOD FOR THE ESTIMATION OF TERIFLUNOMIDE IN TABLET DOSAGE FORM

2019 ◽  
pp. 80-84
Author(s):  
T. S. Vishwas ◽  
B. M. Gurupadayya ◽  
Rupshee Jain
Keyword(s):  
Quality Control ◽  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Glacial Acetic Acid ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Aluminum Plates ◽  
Tablet Dosage ◽  
Hptlc Method

Objective: The current work is intended towards the development of a novel, simple and precise high-performance thin layer chromatographic (HPTLC) method coupled with a densitometer for the estimation of teriflunomide (TEF) present in the marketed formulation. Methods: The chromatographic development was performed on aluminum plates coated with silica gel 60 F254 using toluene: ethyl acetate: glacial acetic acid (7.5:2: 0.5 v/v/v) as the mobile phase. Densitometric scanning was achieved at the absorbance maxima, UV 284 nm. Results: Well separated band was observed with Rf value 0.46. The calibration curve plotted in the concentration range 100-700ng/band exhibited an excellent linear relationship with the r2 value of 0.9928. The method was found to comply with all the validation parameters as per the ICH guidelines. Conclusion: The method ensures minimal use of mobile phase with minimal run time compared to other reported analytical methods. This validated method can be used by quality control laboratories for the routine quantitative analysis of tablets consisting of Teriflunomide.

scholarly journals Peroxidase from infected fruit of Solanum sp. grown in Nsukka

2019 ◽  
Vol 54 (2) ◽  
pp. 131-138
Author(s):  
Omeje KO ◽  
Eze SOO ◽  
FC Chilaka
Keyword(s):  
Molecular Weight ◽  
Quality Control ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Size Exclusion ◽  
Optimum Temperature ◽  
Ammonium Sulfate Precipitation ◽  
Optimum Ph ◽  
Exclusion Chromatography ◽  
The Ideal

In this study, we characterized the activity of peroxidase a quality control enzyme from the infected fruit of Solanum sp. Peroxidase was purified to homogeneity by ammonium sulfate precipitation, dialysis, ion exchange chromatography and size exclusion chromatography. The molecular weight of the native enzyme was 63000 da. The enzyme was shown to have two iso-enzymes with distinct optimum pH of 4.5 and 7.0 and optimum temperature of 40 and 70⁰C. The purified enzyme had broad substrate specificity with o-dianisidine being the ideal substrate. Na+, Ca2+, Mg2+, Mn2+, Cu2+, Al3+ were shown to be activators of the enzyme, while the peroxidase activity was severely inhibited by Co2+. Bangladesh J. Sci. Ind. Res.54(2), 131-138, 2019

scholarly journals Spectrophotometric determination of ranitidine hydrochloride (RNH) in pharmaceutical formulation using 9-fluorenylmethyl chloroformate (FMOC-Cl)

2018 ◽  
Vol 6 (6) ◽  
pp. 7-14
Author(s):  
Abdalla Ahmed Elbashir ◽  
Shahd Moutasim Merghani
Keyword(s):  
Quality Control ◽  
Absorption Maximum ◽  
Limit Of Detection ◽  
Pharmaceutical Formulation ◽  
Reaction Conditions ◽  
Limit Of Quantification ◽  
Ranitidine Hydrochloride ◽  
Ich Guidelines ◽  
Sensitive Spectrophotometric Method

A new, simple and sensitive spectrophotometric method is developed for the determination of ranitidine hydrochloride (RNH). The proposed method is based upon reaction of RNH with 9-fluorenylmethyl chloroformate (FMOC-Cl) in borate buffer of pH 8.0 producing an absorption maximum at 255 nm. All parameters required for the reaction conditions are investigated. Linearity is verified with a range of 2-16 μg/mL and is described by the regression equation y = 61129 x + 0.0354 with a correlation coefficient of 0.9998 (n = 7). The limit of detection (LOD) and the limit of quantification (LOQ) were calculated as per ICH guidelines and were found to be 0.2219 and 0.6724 μg/mL, respectively. The method was successfully applied for the determination of RNH in pharmaceutical formulation. Therefore, the method can be used for routine analysis of RNH in quality control laboratories.

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