scholarly journals HPLC METHOD DEVELOPMENT AND VALIDATION FOR AZITHRO-MYCIN IN ORAL SUSPENSION

2019 ◽  
pp. 7-12
Author(s):  
Alok Pratap Singh ◽  
Iti Chauhan ◽  
Snigdha Bhardwaj ◽  
Praveen Gaur ◽  
S Sadish Kumar ◽  
...  
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Validation Parameters ◽  
Wide Range ◽  
Tract Infections ◽  
Development And Validation

Introduction: Azithro-mycin a semi-synthetic, azalide congener of erythro-mycin indicated in the treatment of respiratory tract infections. Various methods available for determination of Azithro-mycin, but HPLC are most versatile one. Objective: The present study is based on the development and validation of a rapid, simple high performance liquid chromatography (HPLC) method equipped with UV detector for quantitative analysis of Azithro-mycin (AZN) in suspension. Material and methods: The Method was performed by using Hypersil BDS-C18 (250 mm × 4.6 mm i.d.) column MS-II, with an isocratic mobile phase of methanol, acetonitrile and phosphate buffer pH 8 (60:30:10; v/v) with run time 15 minutes. The determinations were performed at a flow rate of 1.0ml/min, and UV detector set at 212 nm. Result and Discussion: The method was found to be specific with relative standard deviation (RSD) less than 2.09%. The method showed accuracy with RSD less than 1.34% and precision in repeatability with RSD less than 1.42%. The method was found to be linear over a wide range of concentration from 1.0 to 50.0 μg/mL (R2 = .995). Limit of detection and limit of quantification were found to be 14.40 ng/mL and 43.66 ng/mL respectively. Conclusion: It was advantageous to use UV detector over other methods employing electrochemical, photodiode array etc. as the detector, because of cheap and easy availability. The developed method fulfilled all validation parameters as per ICH and can be successfully applied to quantify percent drug content in marketed oral Azithro-mycin suspension.

METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF THYMOL AND EUGENOL BY USING RP-HPLC IN PURE AND IN EMULGEL FORMULATION

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 59-65
Author(s):  
Vinita C. Patole ◽  
Shilpa P. Chaudhari ◽  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Peak Areas ◽  
80 A 20 ◽  
Development And Validation

An attempt was made to develop a simple, selective, rapid and precise high-performance liquid chromatography (HPLC) method for simultaneous estimation of thymol and eugenol. Analysis was performed on a C18 column with the mobile phase consisting of solvent %A (water) and solvent %B (acetonitrile) with the following gradient: 0–1 min, 80 % A, 20 % B; 1–7 min, 40 % A and 60 % B; 7–12 min, 10 % A and 90 % B; and 12–15min, 80 % A and 20 % B at a flow rate of 0.6 mL/min. The compounds were well separated on a Thermo Scientific Hypersil BDS RP C18 column (4.6 mm × 150 mm, dp = 5 µm) and ultraviolet detection at 280 nm. The retention times of eugenol and thymol were 10.5 min and 11.6 min, respectively. Validation of the proposed method was carried out according to the guidelines of the International Council on Harmonization (ICH). The linearity of the method is good for thymol and eugenol over the concentration range of 1–50 ppm, and the r 2 values were 0.9996 for both thymol and eugenol. The calculated limit of detection (LOD) value was 0.5ppm and the limit of quantification (LOQ) value was 1ppm for both the analytes. The intra and interday relative standard deviation (RSD) of the retention time and peak areas was less than 3 %.The established method was appropriate, and the two markers were well resolved, enabling efficient quantitative analysis of thymol and eugenol.

scholarly journals ULTRAVIOLET-SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF NORFLOXACIN PRESENT IN TASTE MASKED DRUG RESIN COMPLEX

2018 ◽  
Vol 11 (4) ◽  
pp. 244
Author(s):  
Ayya Rajendra Prasad ◽  
Jayanthi Vijaya Ratna
Keyword(s):  
Spectrophotometric Method ◽  
Absorption Maximum ◽  
Method Development ◽  
Limit Of Detection ◽  
Statistical Parameters ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Validation Parameters ◽  
Development And Validation

 Objective: The objective of this study was developed and validated a novel, specific, precise, and simple ultraviolet (UV)-spectrophotometric method for the estimation of norfloxacin present in taste masked drug-resin complex.Methods: UV-spectrophotometric determination was performed with ELICO SL 1500 UV-visible spectrophotometer using 0.1 N HCl as a medium. The spectrum of the standard solution was run from 200 to 400 nm range for the determination of absorption maximum (λ max). λ max of norfloxacin was found at 278 nm. The absorbance of standard solutions of 1, 2, 3, 4, and 5 μg/ml of drug solution was measured at an absorption maximum at 278 nm against the blank. Then, a graph was plotted by taking concentration on X-axis and absorbance on Y-axis which gave a straight line. Validation parameters such as linearity and range, selectivity and specificity, limit of detection (LOD) and limit of quantification (LOQ), accuracy, precision, and robustness were evaluated as per the International Conference on Harmonization (ICH) guidelines.Results: Linearity for the UV-spectrophotometric method was noted over a concentration range of 1–5 μg/ml with a correlation coefficient of 0.9995. The LOD and LOQ for norfloxacin were found at 0.39 μg/ml and 1.19 μg/ml, respectively. Accuracy was in between 99.00% and 99.17%. % relative standard deviation for repeatability, intraday precision, and interday precision was found to be 0.600, in between 0.291 and 0.410, and in between 0.682 and 1.439, respectively. The proposed UV spectrophotometric method is found to be robust.Conclusion: The proposed UV-spectrophotometric method was validated according to the ICH guidelines, and results and statistical parameters demonstrated that the developed method is sensitive, precise, reliable, and simple for the estimation of norfloxacin present in taste masked drug-resin complex.

scholarly journals A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

High performance liquid chromatography (HPLC) method development and validation for the determination of flunixin: Animal plasma based study

2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Mobile Phases ◽  
Hplc Method Development ◽  
Development And Validation

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.

scholarly journals NOVEL RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF TELMISARTAN AND NEBIVOLOL HCL IN PHARMACEUTICAL DOSAGE FORM

2018 ◽  
Vol 11 (9) ◽  
pp. 431 ◽  
Author(s):  
Heena Ar Shaikh ◽  
Vandana Jain
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Hplc Method Development

Objective: A simple, accurate, precise, robust reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the estimation of telmisartan and nebivolol hydrochloride (HCl) simultaneously in its combined dosage form.Methods: The compounds were well resolved in an isocratic method using the mobile phase composition of acetonitrile: Buffer (potassium dihydrogen orthophosphate pH adjusted 3.1 with orthophosphoric acid) in a ratio of 40:60 v/v at a flow rate of 1.2 ml/min using C18 Shim-pack (150 mm × 4.6 mm, 5 μ) column. The detection was carried out at 280 nm.Results: The retention time of telmisartan and nebivolol HCl was 4.8 min and 6.5 min, respectively. The developed method was validated by evaluating various validation parameters such as linearity, precision, accuracy, robustness, specificity, limit of detection, and limit of quantification according to the international council for harmonization guidelines. The standard calibration curve was obtained in the concentration range of 24–56 μg/ml for telmisartan and 3–7 μg/ml for nebivolol HCl. The overall average % recovery was found out to be 100.35 for telmisartan and 98.84 for nebivolol HCl.Conclusion: Statistical analysis of the data showed that the method is reproducible and selective for the estimation of telmisartan and nebivolol HCl. The proposed method could be used for analysis of telmisartan and nebivolol HCl in their dosage form.

scholarly journals Research Article on Development and Validation of RP-HPLC Method for Estimation of Canagliflozin

2019 ◽  
Vol 11 (02) ◽  
pp. 85-92
Author(s):  
Gudipally. Mounika ◽  
K. Bhavya Sri ◽  
R. Swethasri ◽  
M. Sumakanth
Keyword(s):  
Retention Time ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Validation Parameters ◽  
Liquid Chromatography Method ◽  
Development And Validation

To develop an accurate, precise, specific high performance liquid chromatography method for quantification of Canagliflozin in bulk and dosage forms. A C18 column (250mm X 4.6mm; 5μm phenomenex) was used with mobile phase containing Acetonitrile-0.1% sodium acetate buffer (pH-4.6), (20:80) in isocratic mode. The flow rate maintained was 1.0ml/min and the U.V detector was operated at 291nm. The retention time of Canagliflozin was 3.307min and showed a good linearity in concentration range of 2-14μg/ml with correlation coefficient of 0.999. The average percent recovery was found to be 99.98%. The developed method follows validation parameters such as system suitability, linearity, precision, accuracy, limit of detection and limit of quantification and robustness as per ICH guidelinesQ2(R1). The proposed method was found to provide faster retention time with sharp resolution with linearity at a lowest concentration as compared to previous methods and this method is validated as per International conference on harmonization guidelines and successfully applied for bulk and pharmaceutical dosage form.

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 Analytical Method Development and Validation and Forced Degradation Stability-Indicating Studies of Favipiravir by RP-HPLC and UV in Bulk and Pharmaceutical Dosage Form

2021 ◽  
pp. 254-271
Author(s):  
Sayyed Nazifa Sabir Ali ◽  
Lajporiya Mobina ◽  
Manjra Mehfuza ◽  
Patel Seema ◽  
Aejaz Ahmed ◽  
...  
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Development And Validation

Aims: To develop and validate a new, simple, rapid, precise, and accurate An Eco-friendly RP-HPLC and UV-Method Development and Validation for an estimation of Favipiravir in Bulk and pharmaceutical dosage form followed by Forced Degradation Studies. Study Design: This was employed for UV-visible (200-400 nm and 400-800 nm respectively) and RP-HPLC method development using C 18 inertsil column and optimization of variables for Favipiravir estimation in bulk and formulations. Place and Duration of the Study: The present work was carried out at Ali-allana College of Pharmacy, Akkalkuwa between the duration of November-2020 to February-2021. Methodology: UV-Spectroscopic method was developed for the estimation of Favipiravir in the bulk and pharmaceutical dosage form. The solvent selected for the Favipiravir UV analysis was water, the solution in a range of 2-10µg/ml was scanned in the UV region from 200-400 nm and the λmax value was determined. The RP-HPLC method was developed on inertsil ODS-3V C18 150 mm x 4.6mm x 5μ column using buffer pH 3.5: acetonitrile [90:10] as mobile phase at flow rate 1.0 ml/min and PDA detection at 358 nm. Results: The maximum absorbance was observed at 358 nm. The wavelength 358 nm was selected for further analysis of Favipiravir. The calibration curve was determined using drug concentrations ranging from 2-10 µg/ml. The % recovery for accuracy was 100.50-100.76%. The method was to be precise with a % RSD value 0.51-1.37 and 0.77-1.78 for intraday and Interday respectively. The limit of detection (LOD) and limit of quantification (LOQ) was found to be 0.0723 &0.219 µg/ml respectively by UV method. The RP-HPLC method was shown to be linear in the 50-250 μg/ml concentration range. The limit of detection (LOD) and limit of quantification (LOQ) was found to be 2.186 & 6.626 μg/ml respectively. The method was to be precise with a % RSD value 0.25-1.53 and 0.86-1.68 for intraday and inter-day respectively. Conclusion: Here we conclude that the developed UV and RP-HPLC methods are precise, accurate, sensitive, and reproducible for the quantitative estimation of Favipiravir bulk and its formulation. The developed method can be used by the pharmaceutical industries for the routine analysis of Favipiravir, in particular by UV and RP-HPLC. The main features of the proposed method are economic and eco-friendly with less retention time around 5.0 min.

scholarly journals UV-SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF LORNOXICAM IN MICROSPONGES

2018 ◽  
Vol 10 (1) ◽  
pp. 74 ◽  
Author(s):  
Ayya Rajendra Prasad ◽  
Bannaravuri Thireesha
Keyword(s):  
Spectrophotometric Method ◽  
Absorption Maximum ◽  
Method Development ◽  
Limit Of Detection ◽  
Statistical Parameters ◽  
Limit Of Quantification ◽  
Straight Line ◽  
Validation Parameters ◽  
Development And Validation

Objective: To develop and validate a novel, specific, precise and simple UV-spectrophotometric method for the estimation of lornoxicam present in microsponges.Methods: UV-spectrophotometric determination was performed with Thermo Scientific Evolution 201 UV-Vis spectrophotometer using methanol as a medium. The spectrum of the standard solution was run from 200-400 nm range for the determination of absorption maximum (λ max). λ max of lornoxicam was found at 353 nm. The absorbance of standard solutions of 3, 6, 9, 12 and 15, µg/ml of drug solution was measured at an absorption maximum at 353 nm against the blank. Then a graph was plotted by taking concentration on X-axis and absorbance on Y-axis which gave a straight line. Validation parameters such as linearity and range, selectivity and specificity, LOD and LOQ, accuracy, precision and robustness were evaluated as per ICH guidelines.Results: Linearity for the UV-spectrophotometric method was noted over a concentration range of 3.0-15.0 µg/ml with a correlation coefficient of 0.9995. The limit of detection (LOD) and limit of quantification (LOQ) for lornoxicam was found at 1.26 μg/ml and 3.82 μg/ml respectively. Accuracy was in between 99.21 and 99.60%. % RSD for repeatability, intraday precision and interday precision were found to be 0.473, in between 0.478 and 0.619 and in between 0.855 and 1.818 respectively. The proposed UV method is found to be robust.Conclusion: The proposed UV-Visible spectrophotometric method was validated according to the ICH guidelines and results and statistical parameters demonstrated that the developed method is sensitive, precise, reliable and simple for the estimation of lornoxicam present in microsponges.

scholarly journals Reverse phase-UPLC method of analysis for simultaneous estimation of Levosalbutamol sulphate, Guaiphenesin and Ambroxol hydrochloride in pharmaceutical cough, cold liquid dosage forms

2019 ◽  
Vol 10 (2) ◽  
pp. 927-934
Author(s):  
Kiran Kumar A ◽  
Balakrishnan M ◽  
Chandrasekhar K B ◽  
Kiran Jyothi R
Keyword(s):  
Limit Of Detection ◽  
Cost Effective ◽  
Dosage Forms ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Relative Standard ◽  
Validation Parameters ◽  
Ambroxol Hydrochloride

The three most drug combinations for cough, cold are widely used worldwide now a day. The purpose of the study was to build up an innovative RP-UPLC technique for simultaneous estimation of Levosalbutamol Sulphate (LEV), Guaiphenesin (GUA) and Ambroxol Hydrochloride (AMB) in liquid dosage forms. Chromatography was carried out on UHPLC (WATERS)_SYMMETRY® C18 4.6mm x 1000mm, 3.5µm, (Agilent - Zorbax Eclipse Plus C18 – Rapid Resolution) with an isocratic mobile phase with pH 3.0 composed of buffer, methanol and Acetonitrile (60:20:20) with a flow rate of 0.8mL/min. The detection was carried out with column temperature at 25°C using a UV detector at 276nm. Validation parameters like linearity, specificity, precision, accuracy, limit of detection (LOD), limit of quantification (LOQ), system suitability, Solutions stability and robustness were considered as affirmed in the ICH guidelines. Retention times for LEV, GUA & AMB were 1.07 min, 1.99 min & 3.55 min respectively. The assay of syrups with the relative standard deviation found to be less than 2%. The parameters values were found, and the method was found to be satisfactory. This validated UHPLC method is cost-effective, receptive and precise than other chromatographic methods.

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