A new, simple, sensitive, precise and accurate High-performance thin-layer chromatographic method for simultaneous determination of Ritonavir and Atazanavir in their combined tablet dosage form has been developed, validated and used for determination of the compounds in commercial pharmaceutical products. Chromatographic separation was achieved on Eclipse C18column (100 mm × 4.6 mm, 3.5 μm particle size) as the stationary phase and Acetonitrile and acetate buffer in the ratio of 60:40. With mean recoveries of 98.20 to 100.03% for atazanavir and 99.73 to 99.98% for ritonavir respectively. Limit of detection for ritonavir and atazanavir were found to be 1.717µg/ml and 0.646µg/ml respectively.
Alagar Raja. M*, Bhavana, Rao. K N V, David Banji, Selva Kumar. D.
Scleropyrum pentandrum(Dennst.)Mabb, Synonym: Scleropyrum wallichianum Arn belongs to the family Santalaceae growing along the margin of evergreen to semi-evergreen forests between 600 and 1600 m. It will flowering in January to March, fruiting in August to October. They are small trees growing up to 7m tall; branches ascending or horizontally to the main trunk.Literatures revealed that, a proper investigation was not done with this plant. It is used by semalai people for its contraceptive activity. The roots are boiled and the decoction is taken as a contraceptive. It is believed that women will become barren after consuming the decoction. Paste of stem bark and leaf is applied externally to treat skin diseases. Screened antibacterial activity of methanol extract of leaves and found inhibitory efficacy was dose dependent. Anticariogenic and cytotoxic activity of methanol extract of S. pentandrum leaves were carried out. The extract was found to be having anticariogenic activity. Hence in this current review a list of activities present in the plant Scleropyrum pentandrum were screened. It is a beneficial work for researchers to provide many details about the plant Scleropyrum pentandrum plant.
A simple, fast, accurate and precise UV-spectroscopic method and RP-HPLC method were developed and validated for the estimation of per ICH guidelines. The λ max of Dasatinib was found to be 315nm RP-HPLC method was developed by using Triethyl amine buffer solution PH 6.5 ±0.05 and solvent mixture (Methanol, Acetonitrile) in (50:50v/v) was used as the solvent and flow rate was set on 1.1 ml/min at 315 nm, retention time for Dasatinib was found to be 12 min. The method was developed in Cosmicsil BDS C18 column (100 mm × 4.6 mm, 3.5μm particle size). In RP-HPLC method was found to be linear in the range of is Dasatinib 50-150μg/ml and with a correlation coefficient value of 0.999. The accuracy studies of RP-HPLC method was performed at five different levels, i.e. 50%, 75%, 100%, 125% and 150% and recovery was found to be in the range of 101 to 101.5% for Dasatinib respectively. This method was Rugged and Robust in different testing criteria, The Limit of Detection (LOD) and Limit of Quantification (LOQ) were found to be LOD value was 2.83 and LOQ value was 9.41 for RP-HPLC method. The % RSD is <2% which indicates the precision of the method. Results of all validation parameter were within the limit as per ICH guideline. So this method can be used for the determination of Bulk Drug as well as Tablet Dosage form easily and the method was precise, economical and accurate to perform in future.
Alagar Raja. M*, Swapna. M, Shirisha. V, David Banji, Rao. K N V, Selva Kumar. D.
A simple, accurate, precise, sensitive, rapid UPLC method has been developed and validated for determination of Glimepride and Ezetimibe in its pharmaceutical dosage form. Chromatographic separation was achieved on a inspire C18 column (2.1×50mm,18), by a mobile phase consisted of buffer (PH 2.5,maintained with ortho phosphoric acid) and Acetonitrile in 60:40(V/V) ratio with a flow rate of 0.25 ml/min. The detection wavelength was set at 242 nm. Glimepride and ezetimibe was subjected to different stress conditions. The degradation products, when any, were well resolved from the pure drug with significantly different retention time values. The method was linear (r2=0.999).The intra and inter day precisions were satisfactory the relative standard deviations did not exceed 2%. The accuracy of the method was proved the mean recovery of Glimepride and ezetimibe was 100.27-101.72%. The proposed method has high throughput as the analysis involved short run-time (2mins). The method met the ICH/FDA regulatory requirements. The proposed method was successfully applied for the determination of Glimepride and ezetimibe with acceptable accuracy and precisions the results demonstrated that the methodcan be applied successfully for routine use in quality control industry laboratories.
Alagar raja. M*, Namratha. CH, David banji, Rao. K.N.V, Selva Kumar. D.
A new simple specific, sensitive, precise reverse phase high performance liquid chromatography method has been developed for simultaneous estimation of lovastatin and niacin. The determination was carried out by using Symmetry C8 (4.6 x 250mm, 5µm) column with the mobile phase containing acetonitrile: phosphate buffer (Ph4.±0.5) in the ratio of 65:35 v/v. The optimized flow rate was 0.7ml/min and the UV detection was carried out at 240 nm. The retention time of lovastatin and niacin were found to be 3.093 min and 6.196 min respectively. The method was found to be linear in the concentration range 2.0-10µg/ml for lovastatin and niacin respectively. The method was validated as per ICH guidelines. The proposed method was successfully applied for the estimation of lovastatin and niacin in pharmaceutical dosage forms.
R. Vasanthi*, J. Prasad, M. Alagar Raja, V. Prashanthi, V. Shrisha, David Banji, D. Selva Kumar.
A simple and precise RP-HPLC method was developed and validation for the determination of Sumatriptan and Naproxen in pharmaceutical dosage forms. Chromatography was carried out on a C8 (4.6x150mm.3.5µm) using a mixture of Buffer: acetonitrile (50:50) as the mobile phase at 0.7 ml/min flow rate. The analytes were monitored using UV detector at 285nm. The retention times of the drugs are 5.87 and 2.24min for Sumatriptan and Naproxen respectively. The proposed method is found to be having linearity in the concentration range of 60-100 mg/ml with correlation coefficient of r =0.999. The developed method has been statistically validated and found simple and accurate. The accuracy studies of RP-HPLC method was performed at three different levels, i.e., 50%, 100%, 150% and recovery was found to be in range 99.0-101.0 %. Sumatriptan and Naproxen respectively. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 3.36µg/ml and 3.206µg/ml for sumatriptan and 9.906µg/ml and 9.86µg/ml for naproxen. The % R.S.Dreported was found to be < 2 %. Due to its simplicity, rapidness, high precision and accuracy of the proposed method it may be used for determining Sumatriptan and Naproxen in bulk and dosage forms.
R. Vasanthi*, B. Sumathi, M. Alagar Raja, V. Shirisha, David Banji, D. Selva Kumar.
Isotretinoinis a topical keratolytic agent which is used in the treatment of skin diseases including acne vulgaris. This paper deals with a simple, feasible and sensitive reverse-phase high performance liquid chromatographic method and ultraviolet spectrophotometric method for quantitative determination of Isotretinoin in pharmaceutical dosage form. The chromatography and spectrum was carried out by using HPLC system and UV spectrophotometry. The mobile phase consisting of Bufferand Methanol in the ratio 80, 20. The detection made at 232 nm and the mobile phase flowed 1.2 ml/min. Validation parameters included system suitability, specificity, linearity, accuracy precision, robustness, ruggedness were determined according to the ICH guidelines. The method could be successfully applied for routine analysis of Isotretinoin in pharmaceutical dosage forms.
R. Vasanthi*, N. Rajitha, M. Alagar Raja, V. Shrisha, David Banji, D. Selva Kumar.
Infectious and parasitic diseases are responsible for 23% of percentage of worldwide deaths and the second ranking cause of death according to the World Health Organization. The other issue related to infectious diseases is their emerging resistance to the used antimicrobial agents. The aim of the study was to synthesize, and identification of novel anti-microbial agents that can potently target microbes.
Talal H. Zeglam*, Omran N. R. Fhid, Suaad M. Abuskhuna, Asma. Gebril, Mohamed. A. Edweshia, Fouad. A. Abonaja, Ramy. Y. Krsift, Moad. M. Dardor.
Two simple and selective visible spectrophotometric methods were developed for assay of Zafirlukast (ZAF) in pure drug and in its pharmaceutical formulation. Studies were carried out to use the charge-transfer reactions of Zafirlukast (ZAF), extracted from neutralized Zafirlukast, as n-electron donor with the π-acceptor, dinitrophenol (DNP) for method A and σ-acceptor, and iodine (I2) For method B, resulting in the formation of colored complex. The colored reaction products were quantities spectrophotometrically at 502 nm and 417 nm for ZAF-CAA and ZAF –I2 complexes, respectively. Beer’s law is obeyed over the concentration ranges of 2.0–40.0 and 5.0–60.0 μg mL-1 for DNP and I2, respectively, with correlation coefficients (r) of 0.9991 and 0.9985, and molar absorptive 0.2409 × 104 and 0.2631 × 104 L mol−1 cm−1 for method A and method B, respectively The analytical parameters such as apparent limits of detection (LOD) and quantification (LOQ) are also reported for two methods. The described methods were successfully applied to the determination of ZAF in tablets. No interference was observed from the common excipients present in tablets. The reaction stoichiometry in two methods was evaluated by Job’s method of continuous variations and was found to be 1: 1 (donor: acceptor).
The simple, sensitive, rapid, direct chiral method for the quantitative determination of chiral purity in S-Amlodipine by HPLC-PDA. The stationary phase was Lux-2 chiral column and mobile phase was Acetonitrile: Triethylamine: Acetic acid (100: 0.1: 0.2 % v/v/v) and measurement was carried out in PDA at a flow rate of 1.0 ml min-1. This method was validated as per the ICH guideline and the method was accurate, precise, specify, linear and sensitive. In enantiomeric separation of the chromatographic run time were less than 7.0 min and R- form eluted at 5.87 and S- form eluted at 6.79 min respectively. The calibration plots were linear over the concentration ranges 1.0-5.0 µg ml-1 for both S and R-Amlodipine. The proposed method was successfully applied to separate (S)-enantiomers from (±)-Amlodipine and was proven to be reproducible and accurate for the quantitative estimation of (S)-enantiomers in bulk drugs and pharmaceutical formulation. The proposed method can be applied to identify and quantitative estimation chiral purity of both recemic amlodipine and S-amlodipine.
R. Sathiyasundar*, K. Selvakumar, K. Valliappan, R. Suresh, P. Venkatesan, M. Swamivelmanickam.