scholarly journals Quick simultaneous analysis of bambuterol and montelukast based on synchronous spectrofluorimetric technique

2020 ◽  
Vol 7 (12) ◽  
pp. 201156
Author(s):  
Rania El Gamal ◽  
Samah Abo El Abass ◽  
Heba M. Elmansi
Keyword(s):  
Raw Materials ◽  
Emission Spectra ◽  
Comparison Method ◽  
Simultaneous Estimation ◽  
Good Precision ◽  
Analytical Methodology ◽  
Ich Guidelines ◽  
Validation Criteria ◽  
20 Nm ◽  
Combined Medication

Sensitive, simple and green analytical methodology for simultaneous estimation of bambuterol and montelukast as a combined medication based on their native fluorescence character was developed. The method relies on synchronous spectrofluorimetry to solve the problem of the overlapping emission spectra of the studied drugs. Using second derivative synchronous spectra enabled the simultaneous quantitation of bambuterol and montelukast without interference. The peak amplitudes of the aqueous solutions at Δ λ = 20 nm were estimated at 284 and 304 nm for bambuterol and at 374 and 384 nm for montelukast. A linear relationship was achieved over the concentration range of 0.2–1.00 µg ml –1 for bambuterol and 0.4–2.00 µg ml −1 for montelukast. All factors and parameters were carefully studied to obtain the highest sensitivity and good precision of the proposed method. Additionally, the validation criteria were assessed in accordance with International Council of Harmonization (ICH) guidelines. The method was used for the estimation of both drugs in their raw materials, synthetic mixtures as well their combined tablets with good agreement between its results and those from the comparison method.

scholarly journals Sequential Spectrophotometric Method for the Simultaneous Determination of Amlodipine, Valsartan, and Hydrochlorothiazide in Coformulated Tablets

2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Hany W. Darwish ◽  
Said A. Hassan ◽  
Maissa Y. Salem ◽  
Badr A. El-Zeany
Keyword(s):  
Standard Deviation ◽  
Spectrophotometric Method ◽  
Ternary Mixture ◽  
Raw Materials ◽  
Pharmaceutical Preparation ◽  
Point Theory ◽  
Simultaneous Estimation ◽  
Ich Guidelines ◽  
Direct Spectrophotometry

A new, simple and specific spectrophotometric method was developed and validated in accordance with ICH guidelines for the simultaneous estimation of Amlodipine (AML), Valsartan (VAL), and Hydrochlorothiazide (HCT) in their ternary mixture. In this method three techniques were used, namely, direct spectrophotometry, ratio subtraction, and isoabsorptive point. Amlodipine (AML) was first determined by direct spectrophotometry and then ratio subtraction was applied to remove the AML spectrum from the mixture spectrum. Hydrochlorothiazide (HCT) could then be determined directly without interference from Valsartan (VAL) which could be determined using the isoabsorptive point theory. The calibration curve is linear over the concentration ranges of 4–32, 4–44 and 6–20 μg/mL for AML, VAL, and HCT, respectively. This method was tested by analyzing synthetic mixtures of the above drugs and was successfully applied to commercial pharmaceutical preparation of the drugs, where the standard deviation is <2 in the assay of raw materials and tablets. The method was validated according to the ICH guidelines and accuracy, precision, repeatability, and robustness were found to be within the acceptable limits.

NOVEL RPHPLC-PDA METHOD FOR SIMULTANEOUS ESTIMATION OF HEPARIN AND ITS CO-ADMINISTERED DRUG (FENOFIBRIC ACID) IN MIXTURE

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (01) ◽  
pp. 73-75
Author(s):  
M. Gandhimathi ◽  
◽  
Sneha M. John ◽  
T. K. Ravi
Keyword(s):  
High Performance ◽  
Simultaneous Estimation ◽  
Good Precision ◽  
Fenofibric Acid ◽  
Chromatography Method ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Array Detection ◽  
Liquid Chromatography Method ◽  
Potassium Dihydrogen Orthophosphate

The poly prescription and co-administration of more than two drugs to treat patients for the disease conditions are inexorable. Heparin is and anticoagulant often administered with fenofibric acid in cardiac treatments. A reverse phased high-performance liquid chromatography method based on photo diode array detection has been developed for their simultaneous determination from admixture. They were separated using potassium dihydrogen orthophosphate: acetonitrile (20:80, V/V), on C18 column, at a flow rate of 0.8 mL/min. The retention time of Heparin and fenofibric acid was 3.8 and 13.1 min, respectively. The validation parameters were studied as per ICH guidelines to ascertain the validity of the method for the purpose intended. The linearity was observed between 0.5-3 I.U./mL of heparin and 0.25-1.5 µg/mL of fenofibric acid. The method was applied to a synthetically prepared admixture, and found to be satisfactorily resolving two drugs without any interference, with good precision and reproducibility in the established condition.

scholarly journals Development and application of a spectrophotometric method in quality evaluation of benzimidazole anthelminthics in Nairobi city county

2020 ◽  
Vol 6 (1) ◽  
Author(s):  
Johnson K. Murage ◽  
Beatrice K. Amugune ◽  
Peter Njogu ◽  
Stanley Ndwigah
Keyword(s):  
Spectrophotometric Method ◽  
High Performance ◽  
Neglected Tropical Diseases ◽  
Developing Economies ◽  
Raw Materials ◽  
Poor Quality ◽  
Prolonged Treatment ◽  
Good Precision ◽  
Market Surveillance

Abstract Background Neglected tropical diseases (NTDs) are a group of communicable diseases which are prevalent in the tropics affecting more than one billion people. Treatment and prevention of these infections is very costly to developing economies. Helminthiases are classified among NTDs. The communities afflicted are poor and have limited access to essential resources for their livelihood. Poor-quality drugs for NTDs may lead to death or prolonged treatment without achieving the desired results. The limited resources used in purchasing poor-quality drugs will therefore be wasted instead of being put to good use. Most of the methods available for the analysis of benzimidazole anthelminthics utilize high-performance liquid chromatography. They are therefore time consuming, require sophisticated and expensive equipment, utilize rare and expensive reagents and solvents, and call for skilled personnel. A simple, rapid, and inexpensive ultraviolet spectrophotometric method of analysis would therefore come in handy especially in the analysis of many samples as occurs during post-authorization market surveillance for quality. Results The suitable solvent for the spectroscopic analysis was established as 0.1 M methanolic HCl. The wavelength of analysis was set at 294 nm. Upon validation, the method was found to have good linearity. The range over which linearity was established was way beyond the 80 to 120% of the working concentration specified by the ICH. The method exhibited good precision. Out of 32 commercial samples analyzed, five (15.6%) did not comply with compendial specifications. Intra-brand batch variation was also observed. Out of three batches of product A002T analyzed, one did not comply with compendial specifications. Conclusion A major limitation in the analysis of benzimidazole anthelminthics is the lack of reliable, simple, rapid, and low-cost methods of analysis with high throughput. The developed method serves to fill this gap. It can be used in the analysis of raw materials and finished products. It can also be used in the establishment of the quality of products prior to registration. The method will prove very useful in post-market surveillance of quality of benzimidazole anthelminthics.

Synthesis and Characterization of Y2O3:Eu3+ Film Derived by Sol-Gel Processing

2007 ◽  
Vol 336-338 ◽  
pp. 593-596
Author(s):  
Chun Yang ◽  
Jun Ying Zhang ◽  
Hai Bing Feng ◽  
Wei Chang Hao ◽  
Tian Min Wang
Keyword(s):  
Raw Materials ◽  
Sol Gel ◽  
Emission Spectra ◽  
Luminescent Properties ◽  
Dip Coating ◽  
Organic Additive ◽  
Excitation Spectra ◽  
Excitation Peak ◽  
Close Relationship ◽  
Dip Coating Technique

Y2O3:Eu3+ thin film was synthesized by sol-gel method with inorganic salt raw materials, and the crystal structure and luminescent properties were investigated. By adding organic additive to the sol, a homogeneous film with high luminescent intensity could be obtained by dip-coating technique on the surface of alumina sheet and quartz glass. Structures of the films were studied by XRD and SEM. The excitation spectra of the films showed a wide excitation peak from 200nm to 260nm, and the emission spectra had a strongest emission peak at 611nm which revealed a close relationship with the calcining temperature.

Development and Validation of the Analytical method for the estimation of a combination of 5-fluorouracil and Imiquimod by RP-HPLC

2021 ◽  
pp. 3313-3318
Author(s):  
Bhupender Tomar ◽  
Ankita Sharma ◽  
Inder Kumar ◽  
Sandeep Jain ◽  
Pallavi Ahirrao
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Pharmaceutical Ingredients ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, precise, and accurate reverse phase high performance liquid chromatographic method (RP-HPLC) was developed and validated for the estimation of the combination of 5- Fluorouracil (5-FU) and Imiquimod in active pharmaceutical ingredients (APIs). The method was carried out on Phenomenex C18 (250 × 4.6mm I.D., 5𝜇m) using isocratic elution mode. The mobile phase was used as Acetonitrile: 10mM potassium dihydrogen orthophosphate: triethylamine (40:59.9:0.1, v/v, pH 4.5 with orthophosphoric acid) and Water: ACN (50:50 v/v) was used as a diluent. The concentration of solvents was 1-20µg/ml and the volume of injection was 20µl with the flow rate of 1.2ml/min. The retention times for 5-FU and Imiquimod were found to be 1.9±0.5 and 6.6±0.5 min respectively. The absorption maxima of 5FU and Imiquimod were found 267nm and 227nm respectively. The method was validated as per ICH guidelines. All the data were found within the specified limits. The limit of detection (LOD) and limit of quantification (LOQ) of 5- Fluorouracil were found to be 0.015μg/mL and 0.048 μg/mL, respectively, and Imiquimod was found to be 0.078μg/mL and 0.237μg/mL, respectively. The method developed in the present study was found to be sensitive, specific, and precise and can be applied for the simultaneous estimation of 5-FU and Imiquimod.

DEVELOPMENT OF HPTLC METHOD FOR SIMULTANEOUS ESTIMATION OF CIPROFLOXACIN AND ORNIDAZOLE IN COMBINED DOSAGE FORM

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 36-43
Author(s):  
N. R Dighade ◽  
◽  
M. D Shende ◽  
A. V Kasture
Keyword(s):  
Quality Control ◽  
High Resolution ◽  
Thin Layer ◽  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Ich Guidelines ◽  
Hptlc Method ◽  
Routine Quality Control

A simple and accurate high performance thin layer chromatographic (HPLTC) method has been developed and validated as per ICH guidelines for estimations of Ciprofloxacin (CP) and Ornidazole (ORN) in combined dosage form. The mobile phase was acetonitrile: toluene: water and triethylamine (5.5:1.8:1.5:1.6 V/V) was found to be best which gave high resolution with Rf 0.16 and 0.84 for ciprofloxacin and ornidazole respectively. The linearity of ciprofloxacin and ornidazole was found to be in the range of 0.4 to 0.8 µg/mL and 0.4 to 0.8 µg/mL, respectively. The coefficient of correlation (r2 ) was found to be greater than 0.989 for both the components by this method. The tablet analyses result (n = 5) were found to be > 100.84 % by HPTLC for both the components. The proposed method was found to be simple, accurate and suitable for routine quality control of marketed formulations containing these drugs.

DEVELOPMENT, VALIDATION OF RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF TENOFOVIR DISPROXIL FUMARATE, EMTRICITABINE AND RILPIVIRINE HYDROCHLORIDE IN BULK, FORMULATION AND USED IN NANOSUSPENSION

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (09) ◽  
pp. 43-54
Author(s):  
K Vijaya Sri ◽  
M. Madhuri ◽  
V. Anusha ◽  
V.R.K. Siresha ◽  
Keyword(s):  
Research Work ◽  
Multicomponent System ◽  
Hplc Method ◽  
Combination Method ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Line Of Therapy ◽  
Development And Validation

The present research work illustrates the development and validation of RP HPLC method for simultaneous estimation of tenofovir disproxil fumarate, emtricitabine and rilpivirine hydrochloride in bulk and formulated in a pharmaceutical dosage form as a nanosupension. Antiretroviral drug treatment is the primary line of therapy for treating HIV. The multicomponent system formulated as a nanosuspension evidenced increased hydrophilicity, potency and decreased side effects. The separation was carried out by using efficient BDS hypersil C18 HPLC column with empower software. Combination method of Precipitation—ultrasonic homogenization was used for the preparation of the nanosuspension. The mobile phase used was methanol, water, acetonitrile (80:13.4:6.6) v/v and flow rate 1mL /min. The developed method was thus validated as per ICH guidelines for various parameters whose results advocated the reliability of the method. The results for parameters viz. retention times of tenofovir disproxil fumarate, emtricitabine and rilpivirine were 3.09 min, 2.78 min and 3.68 min, linearity range was between 7.5-90, 5-60, 0.625-7.5µg/mL, respectively. Thus the new RP-HPLC method is optimum, reliable and can be used for the simultaneous estimation of tenofovir disproxil fumarate, emtricitabine and rilpivirine hydrochloride.

scholarly journals Analytical Study for the Charge-Transfer Complexes of Risperidone in Pure and Dosage Forms

2016 ◽  
Vol 8 (3) ◽  
pp. 1745-1753
Author(s):  
F. Ibrahim ◽  
N. El-Enany ◽  
Sh. Shalan ◽  
Rasha Mostafa Elsharawy
Keyword(s):  
Charge Transfer ◽  
Reaction Pathway ◽  
Pharmaceutical Preparations ◽  
Comparison Method ◽  
Charge Transfer Complexes ◽  
Chloranilic Acid ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Optimum Reaction ◽  
Recovery Percentage

Two simple, accurate and sensitive spectrophotometric methods were carried out to investigate through charge-transfer reactions of risperidone (RIS) as n-electron donor with various π acceptors: 7, 7, 8, 8-tetracyanoquinodimethane (TCNQ) and p-chloranilic acid (pCA). The absorbance of reaction product was measured at 842 and 520 nm for TCNQ and pCA reagents respectively. Different experimental parameters affecting the reactions were carefully studied. The reaction pathway was postulated. The proposed spectrophotometric method was utilized for the analysis of RIS in pure form as well as in its pharmaceutical preparations. Under the optimum reaction conditions, Beer’s law is obeyed over the concentration range of 1-12 µg mL-1 and 10-180 µg mL-1 for TCNQ and pCA respectively. The limit of assays detection (LOD) is 0.114 µg mL-1 and 2.55 µg mL-1 for TCNQ and pCA respectively. The mean recovery percentage was 99.72 ± 1.06 and 100.50 ± 1.07 for TCNQ and pCA respectively. The results were compared favorably with those obtained by comparison method. The proposed method was validated statistically according to ICH guidelines.

QBD BASED RP-HPLC METHOD FOR SCREENING AND ANALYSIS OF TELAPRAVIR AND 7 OTHER ANTIRETROVIRAL AGENTS

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (02) ◽  
pp. 20-33
Author(s):  
N. S Kumar ◽  
◽  
R Kumaraswamy ◽  
S. Shantikumar ◽  
D. Paul
Keyword(s):  
Quality By Design ◽  
Pharmaceutical Formulations ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Array Detector ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Full Factorial

The present study describes the separation and simultaneous estimation of eight anti-retroviral drugs, namely, Telaprevir (TPV), Emtricitabine (ECB), Fosamprenavir (FANV), Tenofavir (TNF), Ritonavir (RNV), Raltegravir (RGV) and Oseltamivir (OSMV) and Zidovudine (ZDV) as an active pharmaceutical ingredient, by RP-HPLC method by applying the principles of Quality by Design (QbD). An application of DoE (Design of Experiments) full factorial design was used for initial screening and optimization. The final optimized method consists of separation being carried out on a Fortis C18 column (150 mm × 4.6 mm, 5μ particle size) using acetonitrile and 10 mm ammonium formate buffer (pH 3 adjusted with formic acid) using a gradient program. The quantitative evaluation was performed with a diode array detector at 251 nm and 230 nm with a flow rate of 1 mL min–1. Suitability of this method for the quantitative determination of the drugs was proved by validation in accordance with the International Conference on Harmonization (ICH) guidelines. The method is selective, precise, robust and accurate and can be used for routine analysis of pharmaceutical formulations in quality control and counterfeit screening.

Analytical Method Development and Validation of Glipizide to Determine Residual solvents by head Space-Gas Chromatography

2021 ◽  
pp. 2440-2444
Author(s):  
Sanapala Srinivasa Rao ◽  
A. Vijayalakshmi
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Limit Of Detection ◽  
Dimethyl Formamide ◽  
Analytical Methodology ◽  
Residual Solvents ◽  
Flame Ionization ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation

Residual solvents in Pharmaceuticals are termed as organic volatile impurities. These are the chemicals that are used in the manufacture of drug substance or excipients or use in the preparation of final formulation. Most of the available methods use liquid chromatography which could be expensive and time consuming. Hence, an analytical methodology was developed for the quantification of residual solvents in Glipizide using a headspace gas chromatography (HSGC) with the help of flame ionization detector (FID). Methanol, acetone and dimethyl formamide as residual solvents were determined in Glipizide. Analysis was performed by headspace GC/FID method on Auto system- HS40. Nitrogen was used as a carrier gas and the separation of residual solvents was achieved by DB-Wax 0.25mm, 0.3mcm column. The thermostat temperature was 115 °C for 40 minutes for each vial. % RSD for nine injections obtained are in acceptance criteria. The correlation coefficient R2 obtained greater than 0.99. The method parameters were validated includes specificity, limit of detection and quantification, accuracy, linearity, precision, and robustness. According to the International Conference on Harmonization (ICH) guidelines, a new simple, specific, accurate and precise method was developed and validated.

Sign in / Sign up

Export Citation Format

Share Document