scholarly journals VALIDATION METHODS FOR QUANTITATIVE DETERMINATION OF 4,4'-DIMETHYL-7,7'-ETHYLENDIOXY-2H-1-DIBENZOPYRAN2,2'-DIONE SUBSTANCE

2019 ◽  
Vol 8 (1) ◽  
pp. 59-65
Author(s):  
C. B. Nguyen ◽  
A. Z. Abyshev

Introduction. One of the most promising synthetic compounds of coumarin derivatives is immunacor-4,4'-dimethyl-7,7'-ethylenedioxy-2H-1- dibenzopyran-2,2'-dione. As a result of preclinical studies, it has been shown that it is promising in medical practice as an immunomodulator for the treatment and prevention of secondary immunodeficiency diseases. Aim. The objective of this work is to develop methods for HPLC and UV spectrophotometry to determine the quantitative determination of the immunacor substance and to study the complex of validation characteristics of the developed methods. Materials and methods. Quantitative analysis of the substance was carried out by UV-Spectrophotometry and HPLC. Validation procedures were performed on parameters: specificity, linearity, accuracy and precision in accordance with the requirements of FP XIV. Results and discussion. Validation characteristics have been determined, and their compliance with the relevant eligibility criteria has been experimentally verified. Conclusion. Methods for quantitative determination of the active component in 4,4'-dimethyl-7,7'-ethylenedioxy-2H-1-dibenzopyran-2,2'-dione (immunacor) pharmaceutical substance by HPLC and UV spectrophotometry has been developed. It is established that methods are specific, accurate, precise and linear in the analytical field. The precision HPLC method far exceeds the UV-spectrophotometry.

2021 ◽  
Vol 10 (3) ◽  
pp. 70-75
Author(s):  
T. A. Kobeleva ◽  
A. I. Sichko ◽  
A. I. Zamaraeva ◽  
N. S. Bessonova

Introduction. The creation of new effective antibacterial drugs for the treatment and prevention of purulent-inflammatory diseases is an urgent task of modern pharmacy. Active use in the treatment of purulent infection is found by chemotherapeutic agents from the class of fluoroquinolones, which include ofloxacin.Aim. Development of a method for the quantitative determination of ofloxacin in the complex preparation "Ofloxazol".Materials and methods. For the analysis, the substance ofloxacin, titanium-containing gel "Tizol", solutions of ofloxacin on 95 % ethanol, hydrochloric acid 0.01 mol/l, ointment under the conditional name "Ofloxazol" containing 0.5 % of the drug in the gel "Tizol" were used. The study was carried out by near-UV spectrophotometry.Results and discussion. When studying the absorption spectra, it was found that for the quantitative spectrophotometric analysis of ofloxacin, it is rational to use the wavelength range of 275-320 nm (λmax = 294 nm). Statistical processing of the analysis results showed that the relative error of quantitative determination does not exceed ±1.66 %. The sensitivity of the determination of ofloxacin is 0.245 mcg/ml at A(min) = 0.02. The developed method is validated. Its specificity, linearity, correctness and precision are confirmed. According to the calibration schedule, the content of ofloxacin in the soft dosage form is determined, it is in the range of 0.0483-0.0562 g, which corresponds to the permissible deviations.Conclusion. The conducted studies allowed us to develop and propose a method for the quantitative determination of ofloxacin in the ointment "Ofloxazol", obtained on a titanium-containing basis. The method allows you to evaluate the quality of manufacturing the dosage form, including setting the content of the drug with an error that does not exceed the standard deviations.


Author(s):  
Sirazhudin Dzh. Mekhtikhanov ◽  
◽  
Dzhamilya P. Babaeva ◽  
Kusum M. Magomedova ◽  
Patimat A. Gamzatova ◽  
...  

2018 ◽  
Vol 8 (4) ◽  
pp. 42-47
Author(s):  
Tien Nguyen Huu ◽  
Tram Le Thi Bao ◽  
Ngoc Nguyen Thi Nhu ◽  
Thang Phan Phuoc ◽  
Khan Nguyen Viet

Background: Curcumin is a major ingredient in turmeric (Curcuma longa L., Zingiberaceae), which has important activities such as anti-tumor, anti-inflammatory, antioxidant, anti-ischemia, protection of gastric mucosa etc,. Curcumin can be considered as a biological marker of turmeric and turmeric products. Objectives: Developing an HPLC method for quantification of curcumin in turmeric powder and turmeric - honey ball pills; applying this method for products on the market. Materials and methods: turmeric powder and turmeric - honey ball pills collected in Thua Thien Hue province. After optimization process, the method was validated and applied to evaluate the content of curcumin. Results: The chromatography analysis was performed with: Zorbaz Eclipse XDB-C18 (150 × 4.6 nm; 5 µm); Mobile phase: acetonitril: 2% acetic acid (45:55), Flow rate was kept constant at 1.0 ml/min; Detector PDA (420 nm). The method was validated for the HPLC system compatibility, specificity, linearity range, precision and accuracy; the recovery greater than 98%. Conclusion: The developed HPLC method can determine curcumin in turmeric powder and turmeric - honey ball pills. Key words: Curcumin, turmeric powder, turmeric-honey ball pills, quantitative determination, HPLC


2020 ◽  
Vol 23 (10) ◽  
pp. 1010-1022
Author(s):  
Emrah Dural

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.


2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar

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.


2021 ◽  
Vol 32 (4) ◽  
pp. 867-873
Author(s):  
Helmy Yusuf ◽  
Nina Wijiani ◽  
Rizka Arifa Rahmawati ◽  
Riesta Primaharinastiti ◽  
M. Agus Syamsur Rijal ◽  
...  

Abstract Objectives Curcumin belongs to the family of curcuminoids, natural polyphenolic compounds that possesses neuroprotective properties, anti inflammatory and anticancer. Its entrapment in the developed casein-based micellar powder (CMP) and poloxamer-based micellar powder (PMP) was to enhance the solubility and improve the bioavailability. Henceforth, the present study aimed to acquire an efficient analytical method for the curcumin analysis in polymeric micellar formulations. Methods A fast and specific HPLC method was developed for analyzing curcumin in two different micellar matrices using casein and poloxamer. The HPLC was equipped with a C18 column (250 × 4 mm, 5 µm) and diode array detector. A designated isocratic elution of curcumin was employed using mobile phase with a composition of water (1%, v/v acetic acid) and acetonitrile in a ratio of 50:50 v/v. The employed flow rate was 1.0 mL/min and the analyte was examined at 421 nm. Results An effective analysis in HPLC was successfully achieved by the predetermined HPLC condition. A good resolution of peaks at the employed flow rate was achieved. The linearity was excellent in two different range of concentrations, 2–20 and 10–50 μg/mL. The selectivity, accuracy and precision fulfilled the acceptable requirements. Conclusions The developed method was practically effective to qualitatively identified curcumin. In addition, the assay also effectively quantified the amount of curcumin in the polymeric entrapping matrices which demonstrates that it has great potential to be used in natural compound analysis.


INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (03) ◽  
pp. 44-51
Author(s):  
B. Sabbagh ◽  
B. V. S. Lokesh ◽  
G. A. Akouwah ◽  

Two methods were developed for the determination of dapagliflozin (DAPA) in pure form and in tablets. The procedure utilized was UV-Visible Spectroscopy and RP-HPLC with PDA detector to quantify DAPA in bulk and tablets. The sensitive linear range was identified for both methods within 0.5-5.0μg/mL. The linear regression analysis was identified for both methods with correlation coefficient(r)>0.99. The LOD and LOQ values were found to be 0.05 μg/mL and 0.5 μg/mL for the method by UV-Spectroscopy. The molar absorptivity (ε) was calculated as 1.27 X 105 L.mol-1cm-1. The RP-HPLC method produced LOD and LOQ values of 1.0 ng/mL and 0.5 μg/mL. Both methods were simple, precise, reproducible to quantify the amount of unknown in bulk as well as in tablets and estimated accurately within the range of 100.0±0.5%. Statistical analysis was performed on the data obtained. There was no significant difference between the developed and reported methods with p>0.05. Both methods can be applied for routine analysis of DAPA in bulk and tablets with good accuracy and precision.


2018 ◽  
Vol 4 (5) ◽  
pp. 702-705 ◽  
Author(s):  
Sreenivasa Charan Archakam ◽  
Sridhar Chenchugari ◽  
Chandrasekhar Kothapalli Banoth

Sign in / Sign up

Export Citation Format

Share Document