scholarly journals Development and validation of a gas chromatography method for the determination of β-caryophyllene in clove extract and its application

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Mi Hee Park ◽  
Chul Jin Kim ◽  
Jin Young Lee ◽  
In Seon Kim ◽  
Sung-Kyu Kim
Keyword(s):  
Active Constituent ◽  
Chromatography Method ◽  
Ich Guidelines ◽  
Specificity Test ◽  
Detection Response ◽  
Standard Solution ◽  
Clove Extract ◽  
Pharmaceutical Uses ◽  
Development And Validation

AbstractThe purpose of this study is to check the effectiveness of the analysis method that separates and quantifies β-caryophyllene among clove extracts and validate according to current ICH guidelines. The β-caryophyllene was active constituent of clove buds. The developed method gave a good detection response. In the specificity test, the standard solution was detected at about 17.32 min, and the test solution was detected at 17.32 min. The linearity of β-caryophyllen was confirmed, and at this time, the correlation coefficient (R2) of the calibration curve showed a high linearity of 0.999 or more in the concentration range. The levels of LOD and LOQ were 1.28 ug/mL and 3.89 ug/mL, respectively. The accuracy was confirmed to be 101.6–102.2% and RSD 0.95 ~ 1.31%. As a result of checking the repeatability and inter-tester reproducibility to confirm the precision, the RSD was found to be 1.34 ~ 2.69%. This validated GC method was successfully applied to a soft capsule containing clove extract and other materials for clinical trials. Therefore, this method can be used as an analytical tool for quality control of various samples, including clove extracts and their products of food and pharmaceutical uses.

scholarly journals Development and validation of a gas chromatography method for the determination of β -caryophyllene in clove extract and its application

2021 ◽  
Author(s):  
Mi Hee Park ◽  
Chul Jin Kim ◽  
Jin Young Lee ◽  
In Seon Kim ◽  
Sung-kyu Kim
Keyword(s):  
Active Constituent ◽  
Chromatography Method ◽  
Ich Guidelines ◽  
Specificity Test ◽  
Detection Response ◽  
Standard Solution ◽  
Clove Extract ◽  
Pharmaceutical Uses ◽  
Development And Validation

Abstract The purpose of this study is to check the effectiveness of the analysis method that separates and quantifies β-caryophyllene among clove extracts and validate according to current ICH guidelines. The beta caryophyllene was active constituent of clove buds. The developed method gave a good detection response. In the specificity test, the standard solution was detected at about 17.316 minutes, and the test solution was detected at 17.317 minutes. The linearity of β-caryophyllen was confirmed, and at this time, the correlation coefficient (R 2 ) of the calibration curve showed a high linearity of 0.999 or more in the concentration range. The levels of LOD and LOQ were 1.28 ug/mL and 3.89 ug/mL, respectively. The accuracy was confirmed to be 101.6 ~ 102.2% and RSD 0.95 ~ 1.31%. As a result of checking the repeatability and inter-tester reproducibility to confirm the precision, the RSD was found to be 1.34 ~ 2.69%. This validated GC method was successfully applied to a soft capsule containing clove extract and other materials for clinical trials. Therefore, this method can be used as an analytical tool for quality control of various samples including clove extracts and their products for food and pharmaceutical uses.

Development and Validation of an Eco-Friendly and Low-Cost Method for the Quantification of Cefepime Hydrochloride in Powder for Injectable Solution Using Infrared (IR) Spectroscopy

2020 ◽  
Vol 16 (4) ◽  
pp. 456-464
Author(s):  
Danilo F. Rodrigues ◽  
Hérida R.N. Salgado
Keyword(s):  
Ir Spectroscopy ◽  
Low Cost ◽  
Pharmaceutical Preparations ◽  
Potassium Bromide ◽  
Pharmaceutical Products ◽  
Injectable Formulation ◽  
Ich Guidelines ◽  
Lactam Ring ◽  
Development And Validation

Background: A simple, eco-friendly and low-cost Infrared (IR) method was developed and validated for the analysis of Cefepime Hydrochloride (CEF) in injectable formulation. Different from some other methods, which employ organic solvents in the analyses, this technique does not use these types of solvents, removing large impacts on the environment and risks to operators. Objective: This study aimed at developing and validating a green analytical method using IR spectroscopy for the determination of CEF in pharmaceutical preparations. Methods: The method was validated according to ICH guidelines and the quantification of CEF was performed in the spectral region absorbed at 1815-1745 cm-1 (stretching of the carbonyl group of β- lactam ring). Results: The validated method showed to be linear (r = 0.9999) in the range of 0.2 to 0.6 mg/pellet of potassium bromide, as well as for the parameters of selectivity, precision, accuracy, robustness and Limits of Detection (LOD) and Quantification (LOQ), being able to quantify the CEF in pharmaceutical preparations. The CEF content obtained by the IR method was 103.86%. Conclusion: Thus, the method developed may be an alternative in the quality control of CEF sample in lyophilized powder for injectable solution, as it presented important characteristics in the determination of the pharmaceutical products, with low analysis time and a decrease in the generation of toxic wastes to the environment.

DEVELOPMENT AND VALIDATION OF UV-SPECTROPHOTOMETRIC METHOD FOR DETERMINATION OF SELEGILINE HYDROCHLORIDE LOADED SOLID LIPID NANOPARTICLES

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (08) ◽  
pp. 57-60
Author(s):  
J. B Prajapati ◽  
H Rao ◽  
H Shah ◽  
Keyword(s):  
Correlation Coefficient ◽  
Spectrophotometric Method ◽  
Solid Lipid Nanoparticles ◽  
Lipid Nanoparticles ◽  
Laboratory Scale ◽  
Solid Lipid ◽  
Ich Guidelines ◽  
Development And Validation

The present paper discusses about a simple, precise and validated method for the determination of selegiline loaded solid lipid nanoparticles. The study was carried as per the parameters laid down in ICH guidelines. Maximum wavelength of selegiline in 8:2 methanol: chloroform mixture was selected at 258nm. The method was found to be linear in the range of 200μg/mL to 1000μg/mL with correlation coefficient R2 of 0.994. Method was successfully validating as per ICH guidelines. Moreover, this method was simple, sensitive and easy to apply and can be performed at laboratory scale. Hence, the proposed method can be used for analysis of determination of selegiline loaded solid lipid nanoparticles.

Stability Indicating RP-HPLC Method Development and Validation for the Determination of Solifenacin Succinate in Bulk and its Pharmaceutical Formulation

2021 ◽  
pp. 3509-3514
Author(s):  
A. Tanuja ◽  
S. Ganapaty ◽  
Varanasi S N Murthy
Keyword(s):  
Method Development ◽  
Current Method ◽  
Hplc Method ◽  
Pharmaceutical Ingredients ◽  
Solifenacin Succinate ◽  
Ich Guidelines ◽  
Degradation Studies ◽  
Hplc Method Development ◽  
Development And Validation

The current work aims to establish a novel and advanced reverse phase isocratic liquid chromatography system followed by validation and to conduct stability analysis in active pharmaceutical ingredients and formulations for the quantification of Solifenacin Succinate. The optimized elution was achieved with column Sunfire C8 (4.6 x 150mm, 5µm), using the mobile phase of Buffer: Methanol: Acetonitrile in the composition ratio of 45:45:10 v/v. The wavelength of detection was selected as 220nm with 1.0ml/ min flow rate and 30μl injection volume. The retention time of Solifenacin Succinate was found 2.94 min respectively. The method developed has been validated for various analytical parameters according to ICH guidelines. The Linearity was attained at 20 to100 μg/ml of concentration range. The established method was proved as reproducible. The Assay was obtained as 100.40%. The degradation studies were carried out at all degradative conditions and the results of degradation studies denote that the current method was specific, reliable, and economical. Hence, the developed method can be applied for the qualitative and quantitative determination of the selected drug and its commercial formulations.

LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION OF RELATED IMPURITIES OF LURASIDONE AND ITS FORMULATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (09) ◽  
pp. 41-48
Author(s):  
R. N Kachave ◽  
◽  
P. B. Mandlik ◽  
S. R. Nisal
Keyword(s):  
Method Development ◽  
Gradient Elution ◽  
Hplc Method ◽  
Chromatography Method ◽  
Related Impurities ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Liquid Chromatography Method ◽  
The Stability ◽  
Development And Validation

An RP-HPLC method was developed for the quantification of related impurities of lurasidone and its formulation. The chromatographic separation employs gradient elution using an Inertsil ODS C18 (150x4.6) mm, 5μm columns. Mobile phase consisting of solvent A-buffer (pH 3.0): methanol (90:10 %v/v) and solvent B-acetonitrile: water (80:20 % v/v) delivered at a flow rate of 1.0 mL/min. The analytes were detected and quantified at 210 nm using PDA. The method was validated as per ICH guidelines, demonstrating to be a simple, precise, selective, linear and accurate within the corresponding range of impurities of lurasidone. Linearity was observed in the concentration range of 2-6 µg/mL. The RT for Lurasidone was about 18.5 min and three known impurities at RRT about 0.15, 0.21 and 0.36. The specificity of the method was investigated under different stress conditions including hydrolytic, oxidative, photolytic and thermal as recommended by ICH guidelines. Relevant degradation was found to take place under oxidative conditions. Degradation impurities did not interfere with the RT of drug. The peak purity obtained with the aid of PDA detection and satisfactory resolution between related impurities established the specificity of the determination. All these results provide the stability indicating capability of the method.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING HPTLC METHOD FOR DETERMINATION OF APIXABAN AS BULK DRUG

2019 ◽  
pp. 37-42
Author(s):  
Mrinalini C. Damle ◽  
Swapnil S Waghmare ◽  
PURUSHOTAM SINHA
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Limit Of Detection ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Chromatographic Condition ◽  
Bulk Drug ◽  
Development And Validation ◽  
Hptlc Method

Objective: To develop and validate simple, sensitive stability indicating HPTLC (High performance thin layer chromatography) method for apixaban. Methods: The chromatographic separation was performed on aluminium plates precoated with silica gel 60 F254 using toluene: ethyl acetate: methanol (3:6:1 v/v/v) as mobile phase followed by densitometric scanning at 279 nm. Results: The chromatographic condition shows sharp peak of apixaban at Rf value of 0.38±0.03. Stress testing was carried out according to international conference on harmonization (ICH)Q1A (R2) guidelines and the method was validated as per ICH Q2(R1) guidelines. The calibration curve was found to be linear in the concentration range of 100-500 ng/band for apixaban. The limit of detection and quantification was found to be 11.66ng/bandand35.33ng/band, respectively. Conclusion: A new simple, sensitive, stability indicating high performance thin layer chromatographic (HPTLC) method has been developed and validated for the determination of apixaban.

scholarly journals Absorbance Correction Method for Simultaneous Estimation of Nifedipine and Metoprolol Succinate in Their Synthetic Mixture Using From Spectrophotometry

2015 ◽  
Vol 1 (3) ◽  
pp. 151
Author(s):  
Sojitra Rajanit ◽  
Paras Virani ◽  
Hashumati Raj
Keyword(s):  
Accurate Method ◽  
Correction Method ◽  
Synthetic Mixture ◽  
Simultaneous Estimation ◽  
Metoprolol Succinate ◽  
Absorption Correction ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage

A new simple, economical, precise and accurate method are described for the simultaneous determination of Nifedipine (NIF) and Metoprolol Succinate (MET) in combined tablet dosage form. The proposed method was applied for the determination of Nifedipine and Metoprolol Succinate in synthetic mixture, for determination of sampling wavelength, 10?g/ml of each of NIF and MET were scanned in 200-400 nm range and sampling wavelengths were 313nm for NIF and 275.40nm for MET are selected for development and validation of absorption correction method. For this method linearity observed in the range of 5-25?g/ml for NIF and 25-125?g/ml for MET, and in their pharmaceutical formulation with mean percentage recoveries 100.68 and 100.33, respectively. The method was validated according to ICH guidelines and can be applied for routine quality control testing.

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