Chromatographic conditions LC system equipped

Chromatographic conditions LC system equipped http://www.selleckchem.com/products/Lenalidomide.html with an injection valve (quaternary), 217 UV detector, and Chemstation software was used. A reversed-phase Jupiter C18 column (4.6 mm ID �� 250 mm L, porosity 300 ?, particle size 5 ��m) with a guard column (reversed-phase C18 column of 4.6 mm ID �� 12.5 mm L, porosity 300 ?, particle size 5 ��m) was used for separation. To get the optimum results, the mobile phase with a flow rate of 1.0 mL/min was used and the column temperature was maintained at 30��C. The isocratic programme for the mobile phase was optimized for 12 min. Validation of chromatographic methods During validation, an analytical method is confirmed for reliability, accuracy, and precision of the intended purpose of that method.

[8] The International Conference on Harmonisation (ICH) of Technical Requirements for Registration of Pharmaceuticals for Human Use[9] recognizes accuracy, precision, repeatability, intermediate precision, specificity, limit of quantitation and detection, linearity, and the range of a method as important validation parameters. The guidance for the methodology and statistical tests and associated limits for the validation procedure is provided in the ICH Q2B.[10] The optimized chromatographic methods were validated according to the procedures described in ICH guidelines Q2 (R1).[11] The USP[12] states that the validation of an analytical method is a process that establishes the performance characteristics of a developed analytical method and ensures that it meets its intended purpose and analytical application.

Method validation includes an assessment of the adequacy of the analytical procedure by means of statistical testing, including linear regression analysis, and relative standard deviation (RSD) determination in order to demonstrate the validity of the method.[13] RESULTS AND DISCUSSION Method development To obtain the best chromatographic conditions, the mobile phase composition, column temperature, and flow rate were adequately selected. The flow rate was varied from 0.8 mL/min to 1.2 mL/min. The column temperature was varied between 22��C and 30��C, and the analysis at 30��C was preferred to improve the peak symmetry and resolution. The % of the mobile phase was varied from 58% to 62%. Isocratic chromatographic conditions were optimized for determination of m-cresol in a PTH pharmaceutical product.

The chromatographic separation was achieved by applying Brefeldin_A chromatographic conditions described in ��Chromatographic condition�� section. The applied chromatographic conditions permitted a good separation of m-cresol and PTH at different concentrations of m-cresol. No interference of other excipients was observed as shown in Figure 2 a and b. Figure 2 (a) Sample chromatogram of the principal peak of PTH API buffer, m-cresol standard and mobile phase.

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