analysis

In the pharmaceutical industry today, there are some examples of the use of quality risk management but, they do not represent the full contributions that risk management has to offer. Quality risk assessment is a process of identification of hazards, analysis and evaluation of the risks associated with exposure to those hazards. Risk assessment is a main part of quality risk management process. The evaluation of the risk to quality is based on scientific knowledge, experience with the process and ultimately links to the safety of the patient. For any pharmaceutical organization, quality risk management should aim at raising the level of protection for the patient, by reduction of the risk to which that patient is exposed at the time he/she receives a drug product. In the present seminar report all the aspects regarding quality, quality risk assessment and risk management are covered in great detail.

A rapid, sensitive, precise, and accurate HPLC method coupled with a photodiode array detector was developed, optimized, and validated for the estimation of everolimus in bulk and tablet dosage forms. The chromatographic separation was achieved using a kromosil C8 column (200 mm × 4.6 mm i.d., 5 μm particle size) at 30°C temperature. The isocratic mobile phase consisted of 0.1M dipotassium hydrogen phosphate and methanol (60:40, v/v). The mobile phase was delivered at 1.0 ml/min and the analyte was monitored at 277 nm. The method was successfully validated in accordance to International Conference on Harmonization. The retention time of everolimus was found to be 3.496 min, and the calibration curve was linear in the concentration range of 50-150 μg/ml (R2 = 0.9992). The limit of detection and the limit of quantitation were found to be 0.109 μg/ml and 0.364 μg/ml, respectively.  The proposed method is accurate (percent recoveries were in the range of 99.56-100.09%) and precise (percent relative standard deviation - 0.047 %). No chromatographic interferences from the tablet excipients and components of mobile phase were found. The proposed method was found to be suitable for the quantitative determination of everolimus in tablet dosage forms.

A simple, new, precise, accurate and reproducible RP-HPLC method for simultaneous estimation of mefenamic acid, ethamsylate and tranexamic acid in bulk and pharmaceutical formulations. Separation of mefenamic acid, ethamsylate and tranexamic acid was successfully achieved on a Kromasil C8 (250 mm x 4.6mm x 5µ ) in an isocratic mode utilizing Ammonium acetate buffer and methanol (60:40 v/v) at a flow rate of 1.0 mL/min. The method was validated according to ICH guidelines for linearity, sensitivity, accuracy, precision, specificity and robustness. The response was found to be linear in the drug concentration range of 25-75 mg/mL for mefenamic acid ,25-75 mg/mL for ethamsylate 50-150 mg/mL for tranexamic acid. The correlation coefficient was found to be 0.9997 for both the drugs. The limit of detection (LOD) was 0.158,0.2183 and 0.321 for  mefenamic acid, ethamsylate and tranexamic acid respectively. The limit of quantification (LOQ) was 0.527,0.7278 and 1.071 for mefenamic acid, ethamsylate and tranexamic acid respectively. The relative standard deviation (RSD) of six replicates is less than 2%. This HPLC method is applied successfully to the simultaneous quantitative analysis of mefenamic acid, ethamsylate and tranexamic acid in commercial tablets.

A novel, simple, precise, accurate and reproducible RP-HPLC method was developed and validated for simultaneous estimation of paracetamol, tramadol and dicyclomine in bulk and pharmaceutical formulations. Separation of paracetamol, tramadol and dicyclomine was successfully achieved on a Inertsil ODS C18 (250mm x 4.6mm x 5 µm). The mobile consisted of ammonium acetate buffer (pH 4.5): methanol (80:20 v/v) at a flow rate of 1.0 mL/min. The detection was performed at 271 nm. The method was validated according to ICH guidelines for linearity, sensitivity, accuracy, precision and robustness. The response was found to be linear in the concentration range of 500 µg/mL to1500 µg/mL for paracetamol; 50µg/mL to150 µg/mL for tramadol; 10 µg/mL to 30 µg/mL for dicyclomine. The LOD and LOQ for paracetamol were found to be 2.712 µg/mL and 9.042 µg/mL, respectively. The LOD and LOQ for tramadol was 0.9009 µg/mL and 3.003 µg/mL, respectively and for dicyclomine it was 0.380 µg/mL and 1.265 µg/mL, respectively.  The percentage recovery for paracetamol, tramadol, and dicyclomine were found to be 99.00%, 100.00% and 99.00%, respectively. The excellent percentage recovery values indicate the high accuracy of the proposed method. The method specifically determines the analytes in the sample without interference from excipients of tablet dosage forms. The method was extensively validated according to ICH guidelines for Linearity, Range, Accuracy, Precision, Specificity and Robustness.

  This study was conducted for qualitative estimation of serum proteins separated by SDS-PAGE in order to describe the definition of potential serum proteins that may act as diagnostic marker in oral cancer. Serum samples of 25 biopsy confirmed cases of oral cancer and normal controls of similar age group were subjected to SDS-PAGE on a 12% resolving gel, followed by staining with Coomassie Brilliant Blue R-250. Protein fractions were analyzed using computer software program “Gene Genius Gel Documentation and Analysis System”. Major protein fractions ranging in molecular weights from 1.46-159 kDa were observed. Raw volumes of most of the protein fractions seem to be increased in majority of oral cancer cases as compared to normal control. Protein fractions 56-58 kDa were undetected in normal controls under 80 years of age but appeared in 54% of Oral cancer patient. Further advancement of this work could yield better resolution of protein fraction 56-58 kDa that could serve as marker for oral cancer.

Determination of duloxetine by various methods from various matrices is reviewed in this paper. The methods used consist of spectrofluorimetry, ultraviolet (UV) spectroscopy, thin layer chromatography (TLC), and high-performance liquid chromatography (HPLC). These methods were used to determine the amount of duloxetine in bulk drugs, pharmaceutical dosage forms and biological matrix. HPLC with UV detector as well as mass spectrometric (MS) detector was used for evaluation of pharmacokinetics of duloxetine. It is concluded that HPLC-UV is the most reliable and applicable method for estimation in bulk drugs and formulations while LC-MS is widely employed in bioanalysis.   Keywords: duloxetine, analysis, estimation