Drug analysis plays an important role in the development of drugs their manufacture and therapeutic use pharmaceutical industries rely upon quantitative chemical analysis to ensure that the raw material used and the final product obtained meets the required specifications 3 . Because of therapeutic importance of AML, it is highly abundant drug; many methods have been developed for its determination of pharmaceutical dosage forms. 10 The aim of the present study is the stabilityindicatingRP-HPLC method development and validation with less retention time, highly economic & with high sensitivity 5
Purpose: To Develop A simple, rapid and accurate and stabilityindicatingRP-HPLC Method for the determination of Gemfibrozil in pure and tablet form. Method: StabilityindicatingRP-HPLC method. Result: The method showed a linear response for concentrations in the range of 10-50μg/ml using Methanol: Water solution in the ratio (90:10) as the mobile phase with detection at 274 nm and a flow rate of 0.7 ml/min and retention time 2.287min. The value of correlation coefficient, slope and intercept were, 0.999, 12.389and-3.839, respectively. The method was validated for precision, recovery, ruggedness and robustness. The drug undergoes degradation under acidic, basic, peroxide and thermal degradation conditions. All the peaks of degraded product were resolved from the active
Gingerol is an analgesic, hypoglycemic, hepatoprotective, immune-stimulant, anti-inflammatory agents. In traditional medicine, gingerol has been proven plenty of pharmacological properties such as bactericidal, microbicidal, potent antioxidant, antifertility, tuberculostatic and anticancer. The key objective of this work was to develop, validate and estimate gingerol by RP-HPLC method. According to the ICH guidelines, a stability- indicatingRP-HPLC method was developed and validated. In this method, reverse phase enable Cosmosil C 18 column (250 × 4.6 mm, 5μm) was used
However, few UV (Patel et al., 2012, Anantha et al., 2009) HPLC methods (Teja deepthi et al., 2013) for simultaneous estimation of these drugs have been reported. Detailed study revealed that none of the method revealed all possible impurities nor attempted for identification of degradants. An extensive review of literature did not revealed any stabilityindicatingRP- HPLC method for the simultaneous analysis of DIC and TRA. Hence there is a need to develop stabilityindicating assay method for simultaneous analysis of DIC and TRA and to demonstrate and identify possible degradation products which are likely to form in long term storage conditions of their products. The tablet dosage form containing DIC (75 mg and TRA 50 mg) was approved in November 2011 by Central Drugs Standards Control Organization (CDSCO), Government of India. The formulation is approved as bilayer tablet in which DIC incorporated in sustained release layer and TRA incorporated immediate release layer. It is under development stage for the symptomatic treatment of moderate to severe pain in adults. However, few UV (Patel et al., 2012, Anantha et al., 2009) HPLC methods (Teja deepthi et al., 2013) for simultaneous estimation of these drugs have been reported. To date, no stabilityIndicatingHPLC method has been reported, so there is a need to develop stabilityindicating assay method for simultaneous analysis of DIC and TRA.
A simple stabilityindicatingRP-HPLC assay method has been developed and validated for the determination of Deferasirox from tablet dosage form. Drugs were determined on a Hypresil BDS 150 × 4.6mm column packed with 5µ m particles. The optimized mobile phase was a 50: 50 (v/v) Buffer (1ml OPA in 2lit Milli Q Water) and Acetonitrile, pumped at a flow rate of 1 ml/min. UV detection was performed at 245 nm. The method was validated in the concentration ranges of 50 to 150 ppm where it demonstrated good linearity with r 2 = 0.998. The method was found to be robust, resisting to small deliberate changes in flow rate, column temperature and composition of the mobile phase. Degradation was observed for Deferasirox in the conditions of acid, base and peroxide. The drugs were found to be stable during photo-degradation. The degradation products were well resolved from main peak. The applicability of the method was demonstrated by determining the drug content of commercial pharmaceutical formulations, where it exhibited good performance.
Based on literature review, although some HPLC-UV methods have been developed to detect AZM in pharmaceutical dosage form such as tablets and capsules (Pravallika et al., 2014; Waghule et al., 2013; Senthil Raja et al., 2010; Shaikh et al., 2008; Kulikov and Verushkin 2004), few methods were performed under stabilityindicating conditions (Subbareddy and Divakar, 2015; Ramesh et al., 2012; El-Gindy et al., 2011; Al-Rimawi and Kharoaf, 2010). Despite the fact that HPLC-UV techniques were used to quantify AZM in some nano-formulations, but the validation of these methods was not mentioned (Meng Zhong et al., 2014; Pouretedal, 2014; Yan Liu et al., 2009). To the best of our knowledge, this is the first work reporting azithromycin HPLC-UV analysis in bulk and AZM-SEDDs formulation, along with their degradation profiles. The purpose of this work was to develop a simple, specific and reproducible stability-indicatingHPLC–UV method for the determination of AZM in pure, and AZM-SEDDs. The method was developed and validated as per the recommendations of the International Conference on Harmonization ICH guideline (ICH, 2005).
Chromatography was performed on a WATERS 2695 HPLC column (waters corporation, Mildord, USA) with an autosampler and equipped with a 2996 series of PDA detector with a spectral bandpass of 1.2nm. Components were detected using UV and that processing was achieved by Empower 2 software. A hot air oven was used for thermal degradation of the samples and a UV crossinker, with series of 23400 model UV chamber, equipped with a UV fluorescence lamp with the wavelength range between 200 & 300nm was selected for photolytic degradation. Ultrasonic bath (Toshcon by Toshniwal), digital P H meter(Adwa – AD 1020),
KMCH College of Pharmacy 32 Dept. of Pharmaceutical Analysis Jun Chen 75 et al developed a simple, rapid and sensitive high-performance liquid chromatographic (HPLC) method to quantify ZMT in plasma using an isocratic system with fluorescence detection. The method included a single-step liquid–liquid extraction with methyl tertiary butyl ether. HPLC separation was carried out by reversed phase chromatography with a mobile phase composed of 0.05% (v/v) triethylamine in water (adjusting to pH 2.75 with 85% phosphoric acid) and acetonitrile (92:8, v/v). Fluorescence detection was performed at 225 nm (excitation) and 360 nm (emission). The calibration curve for ZMT was linear from 0.2 to 40 ng/ml. The values of the limit of detection (LOD) and limit of quantification (LOQ) were 20 and 40 pg respectively. The method described in this report is able to determine low levels of ZMT in human plasma. The detection limit of this method for ZMT is 20 pg, which is enough to detect terminal phase concentrations of ZMT after oral administration of 5 mg dose of ZMT to healthy volunteers. The validation method yielded good results regarding linearity, precision, accuracy, specificity and recoveries. In addition, this method has a short chromatographic run (<7 min), so the method is more suitable for high-through quantitative analysis such as human pharmacokinetic studies. The method was sensitive, simple and repeatable enough to be used in pharmacokinetic studies.
The LOD and LOQ concentrations were found to be 10 and 20 IU/ml, respectively. The stability of the drug solution of concentration 100 IU/ml up to 24 hours was estimated by using the established HPLC method. Vitamin D 3 was found to be stable in the MeOH. No peaks corresponding to degradation products were observed. The robustness of the projected method was estimated by altering mobile phase composition from Acetonitrile: Methanol 48:52– 52:48 v/v, varying the injection volume from 19.5 to 20.5 ml and changing the flow rate from 0.9 to 1.1 ml/minutes. Acceptable %RSD values were obtained after making small deliberate changes in the ratio of mobile phase, injection volume, and flow rate. This indicates that the method is robust for the envisioned purpose. The ruggedness of the analytical method by different analysts and different instrument confirms the reliability of the analytical method for ruggedness in the chromatographic conditions.
An additional peak was observed for acid degradation at retention time 2.9 minutes indicating degradation of 7.6% for simultaneous analysis of PYR and SLP (Fig. 4). Additionally, basic degradation studies also revealed the presence of an extra peak at 2.9 minutes (Fig. 5). This specifies formation of degradation products with a degradation of 7.46% for simultaneous study of PYR and SLP. In case of oxidative and photolytic studies, no additional peaks were observed as well as there is no variation in drug peak area, representing degradation was not found for the drugs under oxidative (Fig. 6) and photolytic conditions (Fig. 7).
To develop a suitable and robust LC method for the determination of Entecavir in different mobile phases were employed to achieve the best separation and resolution. The method development was started with Symmetry C18; 250 mmx4.6 mm I.D; particle size 5 μm with the flow rate of 1.0ml/min. Mobile phase was Buffer and Acetronitrile in the ratio of 60:40%, Column temperature was Ambient and the wavelength was 210nm. The retention time of Entecavir is 2.6 minutes and the peak shape was broad. For better peak shape the mobile phase pH and Composition was changed, the trial- 5 shown a sharp peak with good resolution on replacing the column with C 18 Develosil ODS HG-5 RP 150mm x
Pure sample of RSV was gifted by DR’ILS, Hyderabad Central University (HCU), Gachibowli, Hyderabad. All Chemicals used were HPLC grade. Acetonitrile, Formic acid, Analytical grade Hydrochloric acid, Sodium hydroxide and 30% Hydrogen Peroxide solution (v/v) were obtained from Merck limited, Mumbai, India. Rosuvas 10 was obtained from a local pharmacy which is manufactured by Ranbaxy laboratories. High purity De ionised water was obtained form a Milli-Q (Millipore, Milford, MA, USA) purification system.
98.68–100.86%, which indicated good accuracy of the method. Precision studies were carried out at 3 different concentration levels (0.6, 4, 10 g/ml) and the results of the intra-day and inter-day studies are reported in terms of RSD (Table 2). In specificity study a single peak was obtained for NEB with recoveries in the range of 98.32-100.79%, which indicate that there was no interference from the excipient used. The LOD value was found to be 0.06 g/ml which is the concentration that yields signal to noise (S/N) ratio 3:1. The LOQ was 0.2 g/ml with S/N ratio of 10:1. The RSD value of the assay of NEB during solution stability studies were with in 2%. The data proves that the sample solutions were stable up to 24 h at room temperature.
A simple stability-indicating high-performance liquid chromatographic method was developed and validated for the determination of Osimertinib Mesylate in tablet dosage forms. Reversed-phase chromatography was performed on Shimadzu Model CBM-20A/20 Alite, using a mixture of 0.1% T.E.A and methanol (50:50, v/v) as mobile phase with a flow rate of 1.0 mL/min. Detection was carried at 211nm. Linearity was observed over the concentration range of 10–400 μg/mL (R 2 = 0.9992) with regression equation y = 125927x + 192648 Osimertinib
A novel RP-HPLC method was developed and validated for quantitative determination of Naloxegol in pharmaceutical dosage forms. An isocratic RP-HPLC method was developed with Inertsil-C18 ODS column (250 mm × 4.6 mm, 5 μm) and the mobile phase composed of 90 volumes of methanol and 10 volumes of Acetonitrile mixture. The flow rate of the mobile phase was 1 ml min −1 . Detection wavelength was 250 nm and temperature was 25 °C. The method was validated with regard to linearity, accuracy, precision, selectivity and robustness. Linearity was evaluated in the concentration range 40– 120 mg L −1 . The coefficient of correlation was found to be 0.9999. The intra-day and inter-day precision values of measured concentration of naloxegol was calculated and the %RSD for intra-day and inter-day were found to be 0.05 and 0.02, respectively, demonstrating that the method was precise. Good recoveries were obtained for each concentration, confirming that the method was accurate. The limit of detection and limit of quantification for Naloxegol was found to be 2.4 ug/mL and 7.3ug/mL, respectively. The method was applied successfully for the determination of Naloxegol during kinetic studies and routine quality control analysis.
Sample & Standard Preparation for the Analysis 10 mg of Tebivudine standard was transferred into 10 ml volumetric flask, dissolved & make up to volume with mobile phase. Further dilution was done by transferring 0.5 ml of the above solution into a 10ml volumetric flask and make up to volume with mobile phase. The sample was analysed by HPLC by using the above method and a very nicely resolved peak has been obtained at a Retention Time of about 3.52 min. The respective chromatogram is attached in the following page.
It was processed by placing the standard drug at 40°C in an incubator. Samples were collected at deﬁnite time intervals. The weighed amount of sample was added to 5 ml of HPLC-grade methanol and vortexed for 5 min. Final volume was made to get 1000μg/ml. From that serial dilutions were made to get 60μg/ml with diluent. It was vortexed and ﬁltered with a 0.22μm ﬁlter, and 20μL of sample was infused into LC-system.
3. Thakkar AM. Chhalotiya, UK. Parekh, N. Desai, JV. Dalwadi, HB. and Shah, DA. Quantification of Brexpiprazole in Bulk and Its Pharmaceutical Dosage Form by UV - Visible Spectroscopic and SIAM RP-LC Method. Austin Chromatogr, 2018; 5: 1050-1058. 4. Nehal. PB, Ashok, BP, Mohana Rao, S, Amit, JV, Nilesh, KP, and
Approximately 10 mg of pure drug was taken in a clean & dry Petri dish. It was kept in a UV cabinet at 254 nm wavelength for 24 hours without interruption. Accurately weighed 1 mg. of the UV exposed drug was transferred to a clean & dry 10 ml. volumetric flask. First the UV exposed drug was dissolved in methanol & make up to the mark and then injected into the HPLC system against a blank of mobile phase (after all optimized conditions) results shown in table No: 06
Lamotrigine were obtained as pure sample from Alembic Pharmaceuticals Ltd., Baroda (India), as gift samples along with their analytical reports. HPLC grade methanol and acetonitrile was obtained from Merck (India) limited. All other chemical used were of analytical grade. Triple distilled water was used for whole experiment was generated in house. Tablet Lamepil 25mg IPCA Laboratories Pvt. Ltd, India was purchased from local market.