DEVELOPMENT AND VALIDATION OF AN RP-HPLC METHOD FOR THE DETERMINATION OF ULIPRISTAL ACETATE IN BULK AND PHARMACEUTICAL DOSAGE FORM

Ulipristal Acetate ◽

Relative Standard ◽

Objective: This work makes an attempt to establish a sensitive and accurate method for the development and validation of an analytical method for estimation of ulipristal acetate (UPA) in bulk and pharmaceutical dosage form. Methods: A mixture of 20 mM acetate buffer pH 3.7 and methanol in the ratio of 70:30 (v/v %) was used as the mobile phase. An xBridge™ C18 column (250 mm × 4.6 mm, 5μ) was used for the analysis at a flow rate of 1 ml/min, injection volume of 20 μl, run time of 15 min, and detection wavelength of 309 nm. The repeatability (within-day in triplicates) and intermediate precision (for 2 days) were carried out by six injections and the obtained results within and between the days of trials were expressed as percent relative standard deviation (% RSD). The linearity of the method was determined by the analysis of analyte concentration across a range of 10 μg/ml–60 μg/ml. Results: The % RSD values of precision studies were found to be below the accepted limit of 2%. The method was found to be linear with a correlation coefficient (R2) of 0.98. The method was also found to be accurate and robust with suitable values. Limit of detection (LOD) and limit of quantification (LOQ) of the method were found to be 0.371 μg/ml and 1.23 μg/ml, respectively. Conclusion: The results of analysis prove that this method can be used for the routine determination of UPA in bulk drug and in pharmaceutical dosage forms.

Development and validation of novel RP-UPLC method for estimation of atropine sulphate in pharmaceutical dosage form

Chemical Industry and Chemical Engineering Quarterly ◽

10.2298/ciceq120319068a ◽

2013 ◽

Vol 19 (3) ◽

pp. 333-337 ◽

Cited By ~ 2

Author(s):

A.C. Arvadiya ◽

P.P. Dahivelker

Keyword(s):

Mobile Phase ◽

Dosage Form ◽

Limit Of Detection ◽

Atropine Sulphate ◽

Limit Of Quantification ◽

Column Temperature ◽

Ich Guidelines ◽

A simple, precise, accurate, sensitive and repeatable RP-UPLC method was developed for quantitative determination of atropine sulphate in pharmaceutical dosage form. The method was developed by using C18 column Hiber HR Purospher Star (100mm?2.1mm id, 2?m particle size) as stationary phase with Phosphate Buffer: Acetonitrile (87:13, %v/v) as a mobile phase, pH was adjusted to 3.5 by ortho-phosphoric acid at a flow rate of 0.5 mL/min and column temperature maintained at 30?C. Quantification of eluted compound was achieved with PDA detector at 210 nm. Atropine sulphate followed linearity in concentration range of 2.5-17.5 ?g/mL with r2=0.9998 (n=6). Limit of detection (LOD) and limit of quantification (LOQ) values were 0.0033 and 0.0102 ?g/mL for atropine sulphate. The validation study is carried out as per International Conference on Harmonization (ICH) guidelines. This method was successfully applied for estimation of atropine sulphate in pharmaceutical formulation.

DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMETRICMETHOD FOR QUANTITATIVE ESTIMATION OF GLIPIZIDEIN PHARMACEUTICAL DOSAGE FORM

International Journal of Current Pharmaceutical Research ◽

10.22159/ijcpr.2020v12i2.37502 ◽

2020 ◽

pp. 104-107

Author(s):

ANUJA SURYAWANSHI ◽

AFAQUEANSARI ◽

MALLINATH KALSHETTI

Keyword(s):

Dosage Form ◽

Limit Of Detection ◽

Quantitative Estimation ◽

The Novel ◽

Limit Of Quantification ◽

Novel Method ◽

Bulk Drug ◽

Objective: The present work is aimed to develop a simple, rapid, selective and economical UV spectrophotometric method for quantitative determination of Glipizideinbulk and pharmaceutical dosage form. Methods: In this method Dimethyl Form amide (DMF) was used as solvent, the absorption maxima was found to be275 nm in DMF. The developed method was validated for linearity, accuracy, precision, ruggedness, robustness, LOD and LOQ in accordance with the requirements of ICH guideline. Results: The linearity was found to be 10-60 µg/ml having linear equation y=0.017x-0.006 with correlation coefficient of 0.997. The% recovery was found to be in the range of 98.7-100%. The % RSD for intra-day and inter-day precision was found to be 0.569923 and 0.40169 respectively. The limit of detection (LOD) and limit of quantification (LOQ) was found to be3.06 µg/ml and 9.27 µg/ml respectively. Conclusion: The developed method was validated as per ICH Q2(R1) guidelines. The novel method is applicable for the analysis of bulk drug in its pharmaceutical dosage form.

Development and Validation of UV Spectrophotometric Method For Determination of Bisoprolol Fumarate in Bulk and Pharmaceutical Dosage Forms

Mediterranean Journal of Chemistry ◽

10.13171/mjc65/01710181149-shantier ◽

2017 ◽

Vol 6 (5) ◽

pp. 196-199 ◽

Cited By ~ 2

Author(s):

Shahinaz Mohammed ◽

Mohammed Adam ◽

Shaza Shantier

Keyword(s):

Spectrophotometric Method ◽

Limit Of Detection ◽

Limit Of Quantification ◽

Intermediate Precision ◽

Ich Guidelines ◽

Recovery Percentage ◽

Development And Validation ◽

Tablet Dosage

In this study a simple, accurate and precise UV- spectrophotometric method was developed for the estimation of bisoprolol fumarate (BF) in bulk and tablet dosage form. The method was based on measurement of absorbance of BF aqueous solution at 271nm. Validation was conducted in accordance to ICH guidelines. The calibration curve was linear in the concentration range 5-25 µg/mL with correlation coefficient not less than 0.9986. The limit of detection and limit of quantification were 0.22 μg/ml and 0.66 μg/ml, respectively. Intraday and intermediate precision of the developed method were reflected by the low RSD% values (1.19 and 0.854, respectively). The recovery percentage was 105.0 ± 1.3%, n=3. The proposed method was applied for the assay of BF in three different brands

UV Spectrophotometric Determination of Bioflavonoids from a Semisolid Pharmaceutical Dosage Form Containing Trichilia catigua Adr. Juss and Ptychopetalum olacoides Bentham Standardized Extract: Analytical Method Validation and Statistical Procedures

Journal of AOAC International ◽

10.1093/jaoac/89.6.1532 ◽

2006 ◽

Vol 89 (6) ◽

pp. 1532-1537 ◽

Cited By ~ 8

Author(s):

AndrÉ Rolim Baby ◽

Carolina P M Maciel ◽

Telma M Kaneko ◽

Maria Valria R Velasco

Keyword(s):

Spectrophotometric Method ◽

Dosage Form ◽

Limit Of Detection ◽

Complex Matrix ◽

Limit Of Quantification ◽

Analytical Method Validation ◽

Oil In Water ◽

Relative Standard

Abstract A precise, accurate, and sensitive UV spectrophotometric method was developed and validated for routine quantification of total bioflavonoids, expressed as rutin, from a topical oil-in-water pharmaceutical emulsion containing the extract of Trichilia catigua Adr. Juss and Ptychopetalum olacoides Bentham. The method was validated experimentally, and the data were treated rigorously by statistical analysis. The following analytical parameters were assessed: linearity, specificity, intra- and interrun precision measured as relative standard deviation (RSD, %), intra- and interrun accuracy (E, %), recovery (Rec., %), limit of detection (LOD, μg/mL), and limit of quantification (LOQ, μg/mL). The UV spectrophotometric method was linear (r2 0.9995) for standard rutin over the concentration range of 5.015.0 g/mL with specificity for total bioflavonoids (expressed as rutin) at 361.0 nm with an absence of interferents from the complex matrix; RSD of ≤1.79%, intrarun (E 97.88 ±1.75 to 99.0 ± 0.33%) and interrun (E 98.38 ± 1.12 to 100.79 ± 1.30%) accuracy; Rec. 98.64 ± 0.42 to 100.74 ± 0.41%; LOD 0.20 μg/mL; and LOQ 0.30 μg/mL.

Development and Validation of Stability Indicating Reverse Phase High Performace Liquid Chromatography Method for the Determination of Umeclidinium and Vilanterol in Pharmaceutical Dosage Form

Journal of Pharmaceutical Research International ◽

10.9734/jpri/2021/v33i42a32398 ◽

2021 ◽

pp. 208-219

Author(s):

Ahsaana Hamsa ◽

K. Praseetha ◽

K. P. Dijin Raj ◽

T. V. Ashira ◽

O. V. Athira ◽

...

Keyword(s):

Liquid Chromatography ◽

Dosage Form ◽

Limit Of Detection ◽

Limit Of Quantification ◽

Chromatography Method ◽

Relative Standard ◽

Validation Parameters ◽

The Stability

A Sensitive, fast, linear and accurate liquid chromatography technique was developed for the simultaneous determination of Umeclidinium and Vilanterol in Powder dosage form. The estimation was carried out using Phenomenex C18 column (150 × 4.6 mm, 5μ) with ammonium acetate: acetonitrile taken in the ratio 60:40 as mobile phase and pumped at a flow rate of 0.9 ml/min at 300C. Detection wavelength selected was 245 nm. Retention times of Umeclidinium and Vilanterol were found to be 2.219 min and 2.794 min. The method was validated in terms of linearity, precision, accuracy, limit of detection, limit of quantification as per International council for harmonization guidelines. Degradation studies performed indicated the stability of the drug. All of these analytical validation parameters were evaluated, and the percent relative standard deviations were calculated, indicating the method's suitability for determination of Umeclidinium and Vilanterol in pharmaceutical dosage form.

UV Spectrophotometric Method Development and Validation of Esomeprazole in Bulk and Pharmaceutical Dosage Forms

International Journal of Research in Pharmaceutical Sciences ◽

10.26452/ijrps.v12i3.4855 ◽

2021 ◽

Vol 12 (3) ◽

pp. 2286-2290

Author(s):

Gowtham Reddy Cheruku ◽

Sai Laasya Mithinti ◽

Purushotham Saidu

Keyword(s):

Method Development ◽

Limit Of Detection ◽

Regression Equations ◽

Limit Of Quantification ◽

Technical Requirements ◽

Relative Standard ◽

Method Development And Validation ◽

The work discusses method development and validation. An uncomplicated, accurate, and straightforward method was developed for the drug Esomeprazole in bulk as well as Pharmaceutical dosage form. NaOH was used as the solvent. The maximum wavelength (ʎ max) for Esomeprazole was found to be 305nm. The validation was performed as per International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH) guidelines for Accuracy linearity, precision, Limit of Detection (LOD) and Limit of Quantification (LOQ). Esomeprazole's recovery percentage (%) was 100.20%, respectively. Linearity for Esomeprazole was observed between 5-25µg/ml, respectively. Regression equation y=0.0407x-0.0122, regression coefficient (r²) is 0.9963 for Esomeprazole. Inter day and intraday precision were checked, % relative standard deviation values were less than 2. The regression equations were used to derive the Limit of Detection (LOD) and Limit of Quantification (LOQ) values. LOD value was found to be 0.734 µg/mL and LOQ value was 2.224 µg/mL for Esomeprazole. The assay of the marketed formulation was performed, which was between 98-102%. So the method developed was simple and economical that can be adopted for routine tests.

Development and validation of RP-HPLC method for the determination of Darifenacin Hydrobromide in bulk drug and pharmaceutical dosage form

Kathmandu University Journal of Science Engineering and Technology ◽

10.3126/kuset.v13i1.21251 ◽

2018 ◽

Vol 13 (1) ◽

pp. 36-44

Author(s):

Ankit Acharya ◽

N.K. Satish ◽

L. Manoj ◽

Renukaradhya Chitti

Keyword(s):

Limit Of Detection ◽

Hplc Method ◽

Limit Of Quantification ◽

Rp Hplc ◽

High Concentrations ◽

Bulk Drug ◽

The main objective of present study is to develop and validate a new, simple, precise and accurate RP-HPLC method for the determination of Darifenacin Hydrobromide (DFH) in bulk and pharmaceutical dosage forms. The separation and quantification of the drug was achieved on a RP C18 column (250×4.6mm, 5μm) using a mobile phase of acetonitrile: buffer (50:50), pH 3.0 ± 0.2 at a flow rate of 1 mL/min with detection of analyte at 287 nm. The separation was achieved with in 4.0 ± 0.3 min. The method showed good linearity in the range of 10-100 μg/mL. The intra and inter day RSD ranged from 0.20-0.58%. The recovery (mean ± SD) of low, medium and high concentrations were 98.50 ± 0.20, 100.27 ± 0.15 and 100.90 ± 0.09 respectively. The limit of detection and limit of quantification were 0.31 and 0.61 μg/mL, respectively. It can be concluded that the present method could be superior over the methods which were reported earlier. Kathmandu University Journal of Science, Engineering and TechnologyVol. 13, No. 1, 2017, Page: 36-44

A New Second-Derivative Spectrophotometric Method for the Determination of Vildagliptin in Pharmaceutical dosage form

International Journal of Research in Pharmaceutical Sciences ◽

10.26452/ijrps.v12i4.4914 ◽

2021 ◽

Vol 12 (4) ◽

pp. 2610-2614

Author(s):

Subhadip C ◽

Nalanda Baby R ◽

Pridhvi Krishna G ◽

Suraj M ◽

Shyamdeo Kumar T

Keyword(s):

Spectrophotometric Method ◽

Dosage Form ◽

Limit Of Detection ◽

Standard Addition ◽

Second Derivative ◽

Limit Of Quantification ◽

Precision Data ◽

Relative Standard

An accurate derivative spectrophotometric method was developed and validated for the determination of dipeptidyl peptidase inhibitor vildagliptin in the pharmaceutical dosage form. The second derivative of the UV spectra has enabled the estimation of vildagliptin absorbance at 217 nm without any interferences. Linearity, precision, accuracy, detection (LOD), and quantification (LOQ) limits were established for method validation. Calibration curve was linear in the range of 10-60 µg/mL with a regression coefficient of 0.998. The method was validated as per the International Conference on Harmonization (ICH Q2 (R1)). The limit of detection and the limit of quantification were found to be 2.06 µg/mL and 6.25 µg/mL, respectively. Intra and interday precision data illustrated that the method has acceptable reproducibility as the percentage relative standard deviation (RSD) was less than 2 %, which indicates the precision of the method. The recovery was 98.39 % by the standard addition method. The percentage assay of vildagliptin was 98.06 % which showed good applicability. The following results indicate that the procedure is accurate, precise, and reproducible while being simple and less time-consuming. The method was demonstrated to be adequate for routine analysis in quality control.

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

Future Journal of Pharmaceutical Sciences ◽

10.1186/s43094-020-00175-2 ◽

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.

Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

E-Journal of Chemistry ◽

10.1155/2010/470785 ◽

2010 ◽

Vol 7 (3) ◽

pp. 807-812 ◽

Cited By ~ 2

Author(s):

Vanita Somasekhar ◽

D. Gowri Sankar

Keyword(s):

Limit Of Detection ◽

Hplc Method ◽

Detector Response ◽

Reverse Phase Hplc ◽

Limit Of Quantification ◽

Rp Hplc ◽

Accuracy And Precision ◽

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.