scholarly journals UPLC Method Optimisation and Validation for the Estimation of Sodium Cromoglycate in Pressurized Metered Dosage Form

2017 ◽  
Vol 2 (02) ◽  
pp. 18-24
Author(s):  
Anas Rasheed ◽  
Osman Ahmed
Keyword(s):  
Sodium Cromoglycate ◽  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Calibration Graph ◽  
Assay Method ◽  
Dose Inhaler ◽  
Limit Of Quantification ◽  
Adequate Accuracy ◽  
Metered Dose ◽  
Ich Guideline

UPLC assay method optimised and validated for sodium cromoglycate in metered dose inhaler (MDI) using metronidazoleas an internal standard.The separation of Sodium Cromoglycate was achieved on Hypersil BDS C18 (100 mm x 2.1 mm, 1.7 μm) with gradient mobile phase containing methanol, orthophosphoric acid and acetonitrile in the ratio of 50:15:35 %v/v/v. The flow rate was 0.25 mLmin-1, injection volume 20μl and detection wavelength was set at 326nm, at ambient temperature. The validation of the proposed method was carried outfor linearity, accuracy, precision, robustness, limit of detection and limit of quantification test as per ICH guideline. The retention time of sodium cromoglycate found to be 4.73 min. Calibration graph was found to be linear at range 8- 40μg/ml. The regression coefficient (r2) was found tobe 0.9978.The proposed method was rapid with adequate accuracy, precision, ruggedness and robustness and hence be suitable for theroutine analysis of sodium cromoglycate in meter dose inhalation and in bulk.

Determination of Potential Genotoxic Impurity, 5-Amino-2-Chloropyridine, in Active Pharmaceutical Ingredient Using the HPLC-UV System

2020 ◽  
Author(s):  
Murat Soyseven ◽  
Rüstem Keçili ◽  
Hassan Y Aboul-Enein ◽  
Göksel Arli
Keyword(s):  
Analytical Method ◽  
High Performance ◽  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Detection System ◽  
Active Pharmaceutical Ingredient ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Water Ph

Abstract A novel analytical method, based on high-performance liquid chromatography with a UV (HPLC-UV) detection system for the sensitive detection of a genotoxic impurity (GTI) 5-amino-2-chloropyridine (5A2Cl) in a model active pharmaceutical ingredient (API) tenoxicam (TNX), has been developed and validated. The HPLC-UV method was used for the determination of GTI 5A2Cl in API TNX. The compounds were separated using a mobile phase composed of water (pH 3 adjusted with orthophosphoric acid): MeOH, (50:50: v/v) on a C18 column (150 × 4.6 mm i.d., 2.7 μm) at a flow rate of 0.7 mL min−1. Detection was carried out in the 254 nm wavelength. Column temperature was maintained at 40°C during the analyses and 10 μL volume was injected into the HPLC-UV system. The method was validated in the range of 1–40 μg mL−1. The obtained calibration curves for the GTI compound was found linear with equation, y = 40766x − 1125,6 (R2 = 0.999). The developed analytical method toward the target compounds was accurate, and the achieved limit of detection and limit of quantification values for the target compound 5A2Cl were 0.015 and 0.048 μg mL−1, respectively. The recovery values were calculated and found to be between 98.80 and 100.03%. The developed RP-HPLC-UV analytical method in this research is accurate, precise, rapid, simple and appropriate for the sensitive analysis of target GTI 5A2Cl in model API TNX.

scholarly journals A Validated RP-HPLC Method for Estimation of Related Compounds in Hydroxy Naproxen

2020 ◽  
Vol 32 (5) ◽  
pp. 1158-1164
Author(s):  
L. Vaikunta Rao ◽  
K. Tirumala Rao ◽  
V.V. Krishna Mohan Kandepi
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Assay Method ◽  
Array Detector ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Related Substance ◽  
Mobile Phase Flow Rate ◽  
Rp Hplc ◽  
Related Compounds

A simple, linear gradient liquid chromatographic method (RP-HPLC) is proposed for the simultaneous estimation of related compounds in hydroxy naproxen samples. Chromatographic separation was achieved on Zorbax SB C8 (150 × 4.6) mm, 3.5 μm particle size RRLC short column and eluent A used as 0.1% v/v trifluoroacetic acid in water and eluent B used as acetonitrile using Agilent RRLC (UHPLC) system. The mobile phase flow rate was 1.0 mL/min and the eluted compounds were monitored at 235 nm for related substance method and assay method. The excellent resolution was obtained between hydroxy naproxen and its related compounds, which were eluted within 25 min. The performance of the method was validated with respect to ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision and robustness. The correlation coefficient(r) was > 0.995 for both the methods from linearity data and percentage of recovery is 98.0 to 102.0 for assay method and 80.0 to 120.0% for related substance method. Sensitivity of the method was found be less than 0.5 μg/mL. Peak homogeneity data for naproxen in the chromatograms from the selectivity solution obtained by use of the photodiode array detector demonstrated the specificity of the method for analysis of hydroxy naproxen in presence of the related compounds

scholarly journals A Stability Indicating Assay Method Development and Validation for the Frovatriptan Succinate Monohydrate by Using UV: A Spectrophotometric Technique

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Hitesh Verma ◽  
Surajpal Verma ◽  
Harmanpreet Singh
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Assay Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Limit Of Quantification ◽  
Experimental Conditions ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Relative Standard

A new simple, reliable, inexpensive, and accurate method was developed for the quantification of Frovatriptan Succinate Monohydrate in different physiological media at 244 nm in bulk and in tablet dosage forms. The developed method is an attempt to surpass the disadvantages associated with the reported methods, namely, less sensitive and tedious in usage for routine purposes. Beer’s law was followed over the range of 1.0 µg/mL to 4.5 µg/mL. Stability indicating assay method was developed and validated as per the ICH guidelines using various parameters, for example, accuracy, precision, limit of quantification, limit of detection, robustness, ruggedness, solution stability, recovery, forced degradation (hydrolysis, photo degradation, thermal degradation, and oxidation), and so forth. Percent relative standard deviation associated with all the parameters was less than 2, showing compliance with the acceptance criteria of ICH guidelines. The developed method was very sensitive as limit of quantification and limit of detection were found to be 0.025 µg/mL and 0.00625 µg/mL, respectively. Forced degradation studies of drug reveal good stability under the chosen experimental conditions.

Determination of levofloxacin by HPLC with fluorescence detection in human breast milk

Bioanalysis ◽  
2021 ◽  
Author(s):  
Sıdıka Ertürk Toker ◽  
Gamze Ergin Kızılçay ◽  
Olcay Sagirli
Keyword(s):  
Breast Milk ◽  
Fluorescence Detection ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Reversed Phase ◽  
Calibration Graph ◽  
Human Breast Milk ◽  
Human Breast ◽  
Limit Of Quantification

Aim: A new HPLC method with fluorescence detection has been developed and validated for the determination of levofloxacin, one of the fluoroquinolone class antibiotics, in breast milk. Materials & methods: Chromatographic separation was carried out on a reversed phase C18 column with acetonitrile and 10 mM o-phosphoric acid (25:75,v/v) mobile phase composition. Moxifloxacin was used as internal standard and the peaks were detected by fluorescence detection. Results & conclusion: Calibration graph was found linearly within the range of 2.5–500 ng/ml. Limit of detection and limit of quantification were found to be 0.63 and 2.11 ng/ml, respectively. Mean absolute recovery was 96.18%. The developed method has been successfully applied to the determination of levofloxacin in human breast milk taken from two healthy volunteers.

scholarly journals Rapid, Simple, and Sensitive Spectrofluorimetric Method for the Estimation of Ganciclovir in Bulk and Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Garima Balwani ◽  
Emil Joseph ◽  
Satish Reddi ◽  
Vibhu Nagpal ◽  
Ranendra N. Saha
Keyword(s):  
Standard Deviation ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Ich Guidelines ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A new, simple, rapid, sensitive, accurate, and affordable spectrofluorimetric method was developed and validated for the estimation of ganciclovir in bulk as well as in marketed formulations. The method was based on measuring the native fluorescence of ganciclovir in 0.2 M hydrochloric acid buffer of pH 1.2 at 374 nm after excitation at 257 nm. The calibration graph was found to be rectilinear in the concentration range of 0.25–2.00 μg mL−1. The limit of quantification and limit of detection were found to be 0.029 μg mL−1and 0.010μg mL−1, respectively. The method was fully validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%) and can be successfully applied for the determination of ganciclovir in its commercial capsules with average percentage recovery of 101.31 ± 0.90.

scholarly journals PENETAPAN KADAR METANOL HASIL DESTILASI PENGUAP VAKUM PUTAR EKSTRAK METANOL DAUN UBI UNGU MENGGUNAKAN RAMAN SPEKTROFOTOMETER

2018 ◽  
pp. 13
Author(s):  
Santi Maha Dewi
Keyword(s):  
Limit Of Detection ◽  
Pressure Variation ◽  
Vacuum Pressure ◽  
Assay Method ◽  
Absolute Methanol ◽  
Limit Of Quantification ◽  
Purple Sweet Potato ◽  
Non Destructive ◽  
Curve Equation ◽  
Rotary Vacuum

Solvent extracted results are often not utilized for re-extraction. Methanol is a universal solvent which is often used as an extract of simplicia. The result of a rotary vacuum evaporator distillation is not known purity and level. Raman spectrosphotometer is a non destructive method of analysis that can be applied to determine the levels and purity of distilled methanol. The objective of this research is to know the change of vacuum pressure to the level and purity of methanol, so that methanol from rotary vacuum distillation can be reused for re-extraction. Purple sweet potato leaves are macerated using 95% methanol : 3% citric acid. The extract was evaporated using a rotary vacuum evaporator at 100 mbar, 150 mbar, and 200 mbar vacuum pressure with a range of 5 to 180 min. Purity and methanol levels were determined using a Raman Handheld 1064 nm spectrophotometer. Validation of methanol assay method with Raman spectrophotometer was obtained: precision: KV 0.19% -1.70%, accuracy: 94.4-103.8%, limit of detection: 1.77% (v/v), limit of quantification: 5.89% (v/v), the range of linearity of 1.77% -99.9% (v/v), with a calibration curve equation: y = 216,88x + 1437.1 and the value of R2 = 0.9997. Methanol content of distillation product with pressure variation 100 - 200 mbar in the span of 5 to 180 minutes obtained methanol level 59.8-81.2% (v/v). All distilled methanol yields a spectrum similarity of 86-99% when compared with absolute methanol.

scholarly journals CONTENT VARIATIONS OF CARBAMAZEPINE TABLETS IN IRAQI COMMUNITY PHARMACIES: APPLICATION OF HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY ASSAY METHOD

2018 ◽  
Vol 11 (2) ◽  
pp. 117
Author(s):  
Mohanad Naji Sahib
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
High Standard ◽  
Assay Method ◽  
Solution Stability ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Middle East Countries

 Objective: There is paucity in the literature and documentation regarding the post-marketing product quality in Iraq and Middle East countries in general. Therefore, a simple reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the determination of carbamazepine (CMZ) content in post-marketed tablet dosage form.Methods: The RP-HPLC analysis was run at a flow rate of 1 ml/min with a mixture of methanol: water (70:30) mobile phase using a Thermo Synchronise C18 column at a UV detection wavelength of 230 nm. The method was validated for selectivity, linearity, precision, accuracy, limit of detection (LOD), limit of quantification (LOQ), solution stability, and robustness.Results: The calibration curve was linear over a concentration range of 1–20 μg/ml (r2=0.9999) with LOD and LOQ of 0.01 and 0.04 μg/ml, respectively. The intraday and interday precision and accuracy were between 0.04–1.67% and 0.04–0.78%, respectively. The results of analysis of the four brands of CMZ tablets were passed the European Pharmacopoeia specification but with a high standard deviation of mean drug content of some brands.Conclusion: This study shows that the quality of post-marketed drugs and/or the storage conditions in developing countries must be carefully assessed for a better therapeutic response.

scholarly journals Determination of Enalapril maleate from tablets using a new HPLC method

2021 ◽  
Vol 32 (1) ◽  
pp. 70-75
Author(s):  
Simona Gherman ◽  
Daniela Zavastin ◽  
Adrian Şpac ◽  
Alina Diana Panainte
Keyword(s):  
Detection Limit ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Calibration Graph ◽  
Limit Of Quantification ◽  
Enalapril Maleate ◽  
Ich Guidelines ◽  
System Suitability

Abstract For the determination of enalapril maleate in tablets a new, simple and economical HPLC method was developed and fully validated. Chromatographic separation was achieved on Hewlett Zorbax SB-C 18 (150 x 4.6 mm, 5 μm) column and the mobile phase consisted of acetonitrile: 0.025 M phosphate buffer adjusted to pH 3 (70:30 v/v) pumped at a flow rate 0.8 mL/min and UV-detection was performed at 210 nm. The proposed method was validated according to ICH guidelines (linearity, limit of detection, limit of quantification, precision, accuracy, recovery and system suitability). The total run time was less than 3 min and the retention time for Enalapril maleate was 2.3 min. The calibration graph was linear in the concentration range between 10 – 100 μg/mL with the correlation coefficient r2 = 0.9998. The developed and validated method was successfully applied to determine the Enalapril maleate in tablets. Therefore, this method proved to be sensitive, specific and reproducible and can be applied for routine analysis of enalapril maleate from pharmaceutical formulation due to its simplicity of application.

Fast HPLC Method for the Determination of Piroxicam and its Application to Stability Study

2017 ◽  
Vol 68 (4) ◽  
pp. 701-706 ◽  
Author(s):  
Alina Diana Panainte ◽  
Madalina Vieriu ◽  
Gladiola Tantaru ◽  
Mihai Apostu ◽  
Nela Bibire
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Calibration Graph ◽  
Stability Study ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
System Suitability ◽  
Optimum Separation

A fast and robust RP-HPLC isocratic method was developed for determination of piroxicam in bulk materials and pharmaceutical formulations. Optimum separation of piroxicam and stress induced degradation a product was achieved using a SB-C18 Eclipse column (150x4.6; 5�m). The mobile phase was a mixture of water: acetonitrile (50:50) with a flow rate of 0.5mL/min. The UV detection was performed at 360nm. The method was validated in accordance with the current ICH guidelines in terms of linearity, limit of detection, limit of quantification, precision, accuracy, recovery and system suitability. The retention time for piroxicam was 2.55 min. The calibration graph was linear in the concentration range 5-90�g/mL. The assay proved to be sensitive, specific and reproducible. The method was applied for the determination of piroxicam in tablets.

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