LOQ

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.

The objective of present work was to develop and validate a rapid reverse phase high-performance liquid chromatography (RP-HPLC) method for the quantitative analysis of lenvatinib in bulk and pharmaceutical dosage forms. Chromatographic analyses were performed on an ODC column of 250mm 4.6mm: i.d and 5µ particle size with a mobile phase comprising of 0.5M ammonium acetate and acetonitrile in the ratio 90:10 v/v. The   flow rate maintained at 1 ml/min, detected lenvatinib at RT 1.15 minutes. The lenvatinib was detected and quantitated using a photodiode array detector at a wavelength of 367 nm. The method was shown to be specific and linear in the range of 20-120?g/ml (r2= 0.999). The precision (intra- and inter-day) was demonstrated. The method is robust relative to changes in flow rate, column and temperature. The limits of detection and quantitation were 0.4 and 0.12µg/ml respectively. Validation parameters such as specificity, linearity, precision, accuracy, and robustness, limit of detection (LOD) and limit of quantitation (LOQ) were evaluated for the method according to the International Conference on Harmonization (ICH) Q2 R1 guidelines. The method fulfilled the requirements for reliability and feasibility for application to the quantitative analysis of lenvatinib in bulk and pharmaceutical dosage forms.

A novel, convenient, accurate, precise and reproducible reverse phase high performance liquid chromatography was developed and validated for the estimation of Vilazodone in bulk and pharmaceutical tablet dosage form. Objective was achieved under optimized chromatographic conditions on Shimadzu LC-20AT Prominence Liquid Chromatograph with Welchrom C18 isocratic column, (250 mm × 4.6 mm i.d., particle size 5 μm, maintained at ambient temperature), is used as stationary phase. An isocratic mode with mobile phase consisting of Acetonitrile: Water (50:50 v/v), with apparent pH of 3.3, at a flow rate of 1.0 mL/minutes. The effluent was monitored at 240 nm using Shimadzu SPD-20A prominence UV-Vis detector. The retention time of Vilazodone was found to be 4.103 minutes. The linearity range was found to be 1-5 μg/mL with correlation coefficient (R2) is 0.999. Validation parameters such as specificity, linearity, precision, accuracy, and robustness, limit of detection (LOD) and limit of quantitation (LOQ) were evaluated for the method according to the International Conference on Harmonization ICH Q2 (R1) guidelines. The LOD and the LOQ were found to be 0.044 μg/mL and 0.135 μg/mL respectively. Recovery of Vilazodone was found to be in the range of 99.80 % - 99.92 %. The method was validated statistically using the % RSD and the values are found to be within the limits. Therefore this method was conveniently and easily applied for the quantitative determination of Vilazodone in pharmaceutical dosage forms.

A simple, specific, selective and accurate stability-indicating reversed phase high performance liquid chromatographic method was developed for simultaneous determination of Diclofenac potassium (DIC), Paracetamol (PCM) and Methocarbamol (MET). An isocratic RP-HPLC was achieved on younglin HPLC system using Varian C18 (250 Χ 4.6 mm i.d, 5 μm particle size) column with the mobile phase containing mixture of Methanol:water (80:20,v/v). The flow rate was 0.8 ml/min and the eluent was monitored at 225nm. The retention times of DIC, PCM and MET were found to be 3.51, 6.42 and 9.90 min respectively. The linearity was established for DIC, PCM and MET in the range of 10-60 µg/ml, 65-390µg/ml, 100-600µg/ml respectively. The percentage recoveries of DIC, PCM and MET were found to be in the range of 99.73%±0.109, 99.59%±0.085 and 99.50%±0.16 respectively. The LOD for DIC, PCM and MET were found to be 0.15, 2.40 and 1.82μg/ml respectively, while LOQ were 0.48, 7.29 and 5.53μg/ml respectively. All three drugs were subjected to acid, alkali, oxidation, and dry heat degradation. The degradation studies indicated DIC, PCM and MET showed degradation in acid, alkaline, H2O2, and in dry heat condition. The degradation products of DIC, PCM and MET were resolved well from the pure drug with significant differences in their retention time values. This method was also successfully employed for simultaneous quantitative analysis of DIC, PCM and MET in bulk drugs and formulations. The developed method is stability indicating and separate degradants and can be used to determine the stability of samples.