Development and validation of RP-HPLC and ultraviolet spectrophotometric methods of analysis for the quantitative estimation of antiretroviral drugs in pharmaceutical dosage forms

A simple, precise, specific, and accurate reversed phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for determination of vinpocetine in pure and pharmaceutical dosage forms. The different analytical performance parameters such as linearity, accuracy, specificity, precision, and sensitivity (limit of detection and limit of quantitation) were determined according to International Conference on Harmonization ICH Q2 (R1) guidelines. RP-HPLC was conducted on Zorbax C18 (150 mm length × 4.6 mm ID, 5 μm) column. The mobile phase was consisting of buffer (containing 1.54% w/v ammonium acetate solution) and acetonitrile in the ratio (40 : 60, v/v), and the flow rate was maintained at 1.0 mLmin−1. Vinpocetine was monitored using Agilent 1200 series equipped with photo diode array detector (λ = 280 nm). Linearity was observed in concentration range of 160–240 μgmL−1, and correlation coefficient was found excellent (R2 = 0.999). All the system suitability parameters were found within the range. The proposed method is rapid, cost-effective and can be used as a quality-control tool for routine quantitative analysis of vinpocetine in pure and pharmaceutical dosage forms.

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DEVELOPMENT AND VALIDATION OF RP-HPLC-PDA METHOD FOR THE ESTIMATION OF SARPOGRELATE HYDROCHLORIDE IN BULK AND DOSAGE FORMS

INDIAN DRUGS ◽

10.53879/id.55.04.10915 ◽

2018 ◽

Vol 55 (04) ◽

pp. 77-80

Author(s):

M Vijaya Lakshmi ◽

◽

K Hima Bindu ◽

M. Pravallika ◽

B. N. Nalluri

Keyword(s):

Dosage Forms ◽

Hplc Method ◽

Control Analysis ◽

Pharmaceutical Dosage Forms ◽

Rp Hplc ◽

Ich Guidelines ◽

Anti Platelet Drug ◽

Sarpogrelate Hydrochloride ◽

The Mean ◽

Development And Validation

A simple and precise RP-HPLC method has been developed and validated for the estimation of sarpogrelate hydrochloride, an anti-platelet drug in bulk and pharmaceutical dosage forms. Sarpogrelate is an antagonist at 5HT2A and 5HT2B receptors which blocks serotonin induced platelet aggregation and has application in the treatment of diseases including diabetes mellitus, Raynaud’s disease, angina pectoris and atherosclerosis. Chromatography was carried out on a Phenomenex C18 (250 x 4.6mm, 5μm) column with a mobile phase of 10mM ammonium acetate and acetonitrile (45:55% v/v). The flow rate was 1.2mL/min. The detection wavelength was carried out at 220nm. The retention time is 3.356 minutes for sarpogrelate hydrochloride. The linearity was found in the range of 10-50 μg/ml (R = 0.999) and % RSD is less than 2%. The mean recoveries obtained for sarpogrelate hydrochloride were in the range of 98.73-100.67%. The method is validated as per ICH guidelines and can be applied for the estimation of percentage purity in Sarpogrelate hydrochloride for quality control analysis in bulk and its dosage forms.

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Development and Validation of a RP-HPLC Method for Quantitative Analysis of Linagliptin in Bulk and Dosage Forms

Dhaka University Journal of Pharmaceutical Sciences ◽

10.3329/dujps.v17i2.39173 ◽

2018 ◽

Vol 17 (2) ◽

pp. 175-182

Author(s):

Joy Chandra Rajbangshi ◽

Md Mahbubul Alam ◽

Md Shahadat Hossain ◽

Md Samiul Islam ◽

Abu Shara Shamsur Rouf

Keyword(s):

Limit Of Detection ◽

Dosage Forms ◽

Hplc Method ◽

Pharmaceutical Dosage Forms ◽

Rp Hplc ◽

System Suitability ◽

Relative Standard ◽

Limit Of Quantitation ◽

Precision Limit ◽

Development And Validation

This research was aimed to establish a versatile, sensitive, rapid and validated RP-HPLC method to analyze linagliptin in bulk as well as in pharmaceutical dosage forms. Liquid chromatography was performed on HPLC system and 20μl of samples were injected into a C18 column (150 x 4.6 mm i.d., 5μm particle size) and the eluents were monitored through a PDA detector at 239 nm. An isocratic method with a flow rate of 1 ml/min was used to elute the compounds with a mobile phase comprised of 70:30 v/v mixture of phosphate buffer (pH 6.8±0.2) and acetonitrile. The retention time of the compound was found to be 2.8 minutes. According to the ICH Q2(R1) guidelines, the method was validated by establishing several analytical parameters such as system suitability, specificity, linearity, accuracy, precision, limit of detection (LOD), limit of quantitation (LOQ), ruggedness and robustness to assay linagliptin. The method showed good linearity (R2 = 0.9981) over the concentration ranges of 40 – 60 μg/ml with a recovery between 99.48% ± 0.38% RSD to 100.22% ± 0.011% RSD, whereas the LOD and LOQ values were 0.05 μg/ml and 0.15 μg/ml, respectively. The relative standard deviation (% RSD) for inter-day and intra-day precision was not more than 2.0%. Hence, the proposed method can be applied accurately for research and routine analysis of linagliptin in bulk as well as different pharmaceutical dosage forms. Dhaka Univ. J. Pharm. Sci. 17(2): 175-182, 2018 (December)

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