ICH

A new simple, rapid, precise and accurate assay method was developed for simultaneous estimation of Bilastine and Montelukast in pure form and tablet form. The analytes were separated by RP HPLC on a RP-Purosnosphere C18 column (5 µm, 4.6mm* 250 mm).The mobile phase was Acetonitrile: water: methanol (30:25:45 v/v) at 1.1 ml/min flow rate satisfactorily resolve the tertiary mixture. The UV detector was operated at 214 nm for the determination of all the drugs. Linearity, accuracy and precision were found to be acceptable over the concentration ranges of 10-50 µg/ml for Bilastine and 5-25 µg/ml for Montelukast with a R2 0.9960 and 0.9974 values respectively. The optimized methods proved to be specific, robust and accurate for the quality control of drugs in bulk drug and pharmaceutical formulations.

In the pharmaceutical industry an impurity is considered, defined the any other organic material besides the drug substance or pharmaceutical ingredients.  The impurity may be formed during the formulation or upon aging of two APIs in medicines. Stability testing is an integral part of pharmaceutical development. The primary purpose of stability testing is to provide supporting evidence on stability behavior of pharmaceutical drug products. Stability is the capacity of a drug product to remain within specifications established to ensure its identity, strength, quality and purity.

A simple, selective and rapid reverse phase high performance liquid chromatographic (RP-HPLC) method for the analysis of Gliclazide in bulk and in tablet dosage form has been developed and validated. Sample was analysed on a Enable C18 (250mm X 4.6 mm i.d, particle size 5μm) column. The mobile phase consist of Methanol: Water (pH 3.5) in the ratio of 85:15v/v which was sonicated to degased and delivered at a flow rate of 1ml/min at ambient temperature. The retention time of Gliclazidewas 3.7+0.02 minutes. Studies were performed using an HPLC system equipped with a UV detector; the response was monitored at 230 nm.The calibration curve was linear over the concentration range of 20-70 μg/ml (r2=0.999). The limit of detection for Gliclazide was found to be 0.2438 μg/ml and the limit of quantification limit was about 0.7388 μg/ml. The accuracy of the method was established based on the recovery studies. The proposed method can be applied to the routine analysis of Gliclazide in bulk and in tablet dosage form.

The present work was defined to develop area under curve method for antipsychotic drug by UV spectrophotometric analysis which was economical, precise and an accurate method for estimation of Quetiapine fumarate. This method was based on area under curve of UV spectrum between 287 to 297 nm and validated as per ICH guideline Q2 (R1). The linearity in the range was found to be 4-14 μg/ml. The result of correlation coefficient was 0.999. The results of percent relative standard deviation for the intra-day and inter-day precision indicated that method is precise. The values of the recovery studies (99.65 % to 101.04 %) showed good accuracy of the method. LOD and LOQ were calculated as 0.3806 and 1.153μg/ml, respectively. The developed method can be applied for routine estimation of Quetiapine fumarate in bulk and tablet dosage forms.

A novel, simple, rapid and stability-indicating reversed-phase ultra performance liquid chromatographic and mass spectrometric method was developed and subsequently validated for quantitation of Efavirenz (EFV) from drug substance matrix. The separation was achieved in 2.5 minutes on Waters ACQUITY UPLC BEH C18 (50 x 2.1) mm, 1.7µm column in isocratic mode with flow rate 0.4 mL/min. Mobile phase used was 0.01 M ammonium acetate buffer pH 7.5 and acetonitrile in ratio 50:50 v/v. Detection was carried out at the maximum wavelength of 247 nm using a photodiode array detector. The retention time of Efavirenz was found 1.8 minutes. Specificity of the method was established on drug substance by hydrolytic and oxidative stress conditions. Validation of analytical method was carried out as per the current ICH guidelines for linearity, recovery, precision, limit of detection, limit of quantification and robustness parameters.

A simple, accurate, precise, specific, sensitive, reproducible and Reliable RP- HPLC Method was developed for Quantitative Estimation of Metaxalone and Diclofenac potassium in Pharmaceutical Dosage Form. The developed RP- HPLC method with the mobile phase Methanol: Water (80: 20) and Qualisilgold-C18 (250Χ4.6mm, 5μm particle size) as stationary phase with a flow rate of 1.0 mL/minute by using λmax 275nm and PDA detector. Proposed method was found to be linear in the concentration range of 8.0 to 80.0 μg/mL for Metaxalone and 1.0 to 10.0 μg/mL for Diclofenac potassium respectively, and the correlation coefficient was found to be 0.9991 for both the drugs. Precision study showed that the % RSD was within the range of acceptable limits (< 2), and the % Recovery was found to be in the range of 99.29%-101.28% for Metaxalone and 99.98%-102.45% for Diclofenac potassium. The proposed method has been validated as per ICH guidelines.

A novel, simple, rapid and stability-indicating reversed-phase ultra performance liquid chromatographic method was developed and subsequently validated for quantitation of Emtricitabine (ECB) from drug substance matrix. The separation was achieved in less than 2.0 minutes on Waters ACQUITY UPLC BEH C18 (50 x 2.1) mm, 1.7µm column in isocratic mode with flow rate 0.25 mL/min. Mobile phase used was 0.015 M potassium dihydrogen phosphate buffer pH 2.2 and acetonitrile in ratio 75:25 v/v. Detection was carried out at the maximum wavelength of 284 nm using a photodiode array detector. The retention time of emtricitabine was 1.2 minutes. A forced degradation study was performed. Specificity of the method was established on drug substance by hydrolytic and oxidative stress conditions. Validation of analytical method was carried out as per the current ICH guidelines for linearity, recovery, precision, limit of detection, limit of quantification and robustness parameters.

  An accurate, precise and reproducible Reverse Phase High Performance Liquid Chromatographic (RP-HPLC) method was developed and validated for the estimation of Metformin Hydrochloride, Glimepiride and Atorvastatin in Pharmaceutical dosage forms. In this method Qualisil gold C18 column (250mmx4.6mm I.D., 5µm particle size) with mobile phase containing 0.1% TFA in Water (pH adjusted to 2.92 with ammonia) and Methanol in the ratio of 28: 72v/v was used. The flow rate was 1ml/min. and the detection wavelength was 235nm1-2. The linearity was observed in the range of 50 - 225µg/ml, 0.2 - 0.9µg/ml and 1 – 4.5 µg/ml for Metformin Hydrochloride, Glimepiride and Atorvastatin with correlation coefficient of 0.9992, 0.9992, and 0.9997 respectively. Retention times were 3.1min, 7.8min, and 10.1min for Metformin Hydrochloride, Atorvastatin and Glimepiride respectively. The proposed method was validated for Linearity, accuracy, precision and Robustness. The proposed method was validated as per ICH guidelines and can be applied for routine quality control analysis of pharmaceutical dosage forms used for Multidrug therapy containing Metformin Hydrochloride, Glimepiride and Atorvastatin. Key words: RP-HPLC, OPA, Multidrug therapy, ICH, Validation.

An accurate, precise and economic reversed phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for the estimation of lamivudine, zidovudine and nevirapine in pharmaceutical dosage forms. In this method Qualisil BDS C8 column (250mmx4.6mm i.d., 5µm particle size) with mobile phase containing water and acetonitrile in the ratio of 70: 30 v/v with pH adjusted to 5 with ortho phosphoric acid (OPA). The flow rate was 1mL/min and the detection wavelength was 250nm. The linearity was observed in the range of 1-15µg/mL for lamivudine, 3-24 µg/mL for zidovudine and 2.5-20 µg/mL for nevirapine. Retention times were 3.1min, 4.4min, and 7.0min for lamivudine, zidovudine and nevirapine respectively. The proposed method was validated as per ICH guidelines for linearity, accuracy, precision and robustness and can be applied for routine quality control analysis of pharmaceutical dosage forms used for multidrug therapy containing lamivudine, zidovudine and nevirapine.

Development and validation of an analytical UV derivatives spectrophotometric method to quantify carbimazole as a single active principle in pharmaceutical formulation were done. Based on the spectrophotometric characteristics of carbimazole, a signal of first (314 nm), second (300 nm), third (289 nm), fourth (320 nm) order derivative spectrum was found to be adequate for quantification. The method obeyed Beer's law in the concentration range of (2-18 µg/ml) with square correlation coefficient (r2 = 0.999). The mean percentage recovery was found to be 99.56 ± 0.7179. As per ICH guidelines the results of the analysis were validated in terms of linearity, precision, accuracy, limit of detection and limit of quantification, and were found to be satisfactory. Key Words: Carbimazole, Derivative spectrophotometry, ICH, Validation.