ICH.

In this review articles, the development, formulation, and manufacture of drugs, analytical method development & validation play a critical role. Methods are developed for ensuring purity, identity, potency, and performance of pharmaceutical products. Methods should be applied to the extent that they are sufficient for their intended purpose. Throughout the life cycle of a drug product and substance, a range of activities are associated with developing and validating methods. An objective of method validation is to prove that the procedure can be used as intended. Once the method is developed, validation is performed. Different national and international committees have defined the parameters for method validation. The International Conference on Harmonization attempted to harmonize pharmaceutical applications. In accordance with the ICH, other organizations define Linearity, Selectivity/Specificity, Range, Accuracy, Precision (repeatability, intermediate precision, and reproducibility), Limit of quantitation, Limit of detection, Ruggedness, and Robustness.

A simple, specific, quick, isocratic Reversed Phase High Performance Liquid Chromatographic method was developed and validated for the analysis of Noscapine. RP-HPLC method was developed on a Symmetry C-8 (4.6 × 150 mm), 3.5 µm particle, reversed-phase column. The mobile phase was 0.1% octane sulphonic acid (pH- 3): acetonitrile, 40:60 (v/v) at a flow rate of 0.8 ml/min. and the eluate was monitored at 260 nm. The retention time of the drug was found to be 2.314 min. The method was linear over the range of 4-8 μg/ml with a regression coefficient of 0.999 and validated with respect to accuracy, precision, linearity, and specificity, limit of detection and limit of quantization as per the guidelines of International Conference for Harmonization (ICH). This method can be used in the industries for determination of Noscapine to analyze the quality of formulation without interference of the excipients.

Clobazam is an antiepileptic drug. There have been very less number of analytical methods developed for estimation of Clobazam in pure bulk form and in dosage form. In the present research a simple, accurate, precise and cost effective High performance liquid chromatographic method for the estimation of Clobazam, in bulk and pharmaceutical dosage form was carried out. HPLC method was developed on a Symmetry C-8 (4.6×150mm), 3.5µm particle, reversed-phase column. The mobile phase was acetonitrile: phosphate buffer (0.05M, pH- 4.5), 60:40 (v/v) at a flow rate of 0.8ml/min. The eluate was monitored at 231 nm. The method was validated reaching satisfactory results for selectivity, precision and accuracy. The retention time of the drug was found to be 3.38min in the mobile phase, acetonitrile: 0.05M potassium dihydrogen orthophosphate buffer (pH-4.5) 40: 60 (v/v). A linear response was observed in the range of 20-60µg/ml with a regression coefficient of 0.999. Validation parameters were carried out as per the guidelines of International Conference for Harmonization (ICH). This method can be used in the industries for determination of Clobazam to analyze the quality of formulation without interference of the excipients.

A simple, accurate and precise HPLC method for the estimation of memantine in bulk and pharmaceutical dosage form has been reported. Chromatography was performed with Shimadzu HPLC equipment comprising an LC-10A VP quaternary pump, a variable-wavelength programmable UV–visible detector, an SPD-10AVP column oven, and an SCL 10AVP system controller. A Rheodyne injector fitted with a 20μL loop was also used and data were recorded and evaluated using Class-VP 5.032 software. The Compound was separated, at ambient temperature (25 ± 2°C), on a  BDS C18, ( 4.6 mm i.d x 250 mm, 5μm reversed phase column with 100% methanol as mobile phase at a flow rate of 1.0mL.min−1. Before use, the mobile phase was filtered through a 0.22-μm Nylon filter. UV detection was performed at 274nm. A linear response was observed in the concentration ranges of 5-25μg/ml with a regression coefficient of 0.9999. The method was then validated for different parameters as per the ICH guidelines. This method can be used for the determination of memantine in quality control of formulation without interference of the excipients.

An accurate, simple, precise and sensitive HPLC method with UV detection was developed and validated to separate and detect ibuprofen in human plasma using Nimesulide as an internal standard. Ibuprofen and Nimesulide were extracted from human plasma using acetonitrile protein precipitation and HPLC analysis was performed using Waters 515 Series pumps combined with a Waters PDA 2998 series photo diode array detector (DAD). The column used was Agilent C18 column (150mm×4.6mm, particle size 5-micron Agilent, USA). Analysis was isocratic at 1.5 ml/min flow rate with ACN: Buffer (0.025M Potassium dihydrogen ortho phosphate) pH 4.5 (55:45, v/v) as mobile phase. The mobile phase was premixed, filtered through a 0.2 µm nylon membrane filter to remove any particulate matter and degassed by sonication before use. The elution was detected at 230 nm. Each solution was injected in triplicate, and the relative standard deviation (R.S.D.) was measured. The retention times of Ibuprofen 2.24 min and for I.S. 1.72 min respectively. The method was validated over the range of 0.5-8.0 μ/ml. The limit of detection was 0.06μg/ml and the limit of quantification was 0.193μg/ml for ibuprofen. Inter-day as well intra-day replicates of Ibuprofen, gave % R.S.D. below 2.07 and 2.001 respectively  The absolute recovery of ibuprofen was greater than 90% were achieved. This method of analysis for Ibuprofen determination using RP-HPLC was applied for determination of Ibuprofen in plasma.