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A new and stability-indicating High performance liquid chromatographymethod was developed and validated for simultaneous determination of clofarabine impurities in Injectionformulation.The Chromatographic system consisted of a Shimadzu Class VP Binary pump LC-10ATvp, SIL-10ADvp Auto sampler, CTO-10Avp Column Temperature Oven, SPD-10Avp UV-Visible Detector.The method was validated as per the ICH guidelines Apart from these Chromatographic parameters likeresolution, capacity factor, separation factor, column efficiency and peakasymmetry should also be the ideal for estimation.
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Current work discloses the sensitive LC-MS/MS method development for the trace level determination of genotoxicimpurity 2-Methyl-6-nitro aniline in Telmisartan. 2-Methyl-6-nitro aniline was determined by LC-MS/MS methodin selected ion monitoring mode using LiChrospher RP-18 (100 × 4.6 mm) 5.0 µm column. Gradient technique wasapplied for the elution of analytes using acetonitrile (mobile phase A) and 0.01 M ammonium acetate buffer (mobilephase B) in different ratios. The gradient program (T/%B) was set as 0/5, 2.50/15, 5.00/30, 10.00/50, 15.00/95, and20.00/95. Developed method was validated as per International Conference on Harmonization guidelines. The limit ofdetection and limit of quantitation values found for 2-Methyl-6-nitro aniline were 0.05 and 0.1 µg/ml. The developedmethod serves as an upright tool in quality control for quantitation of 2-Methyl-6-nitro aniline impurity at trace levelsin Telmisartan.
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The present work takes into account the development of Reverse Phase High Performance Liquid Chromatography(HPLC) for simultaneous method estimation and validation of pyrimethamine and sulfamethoxypyrazine inpharmaceutical formulation. The chromatographic separation was accomplished on C8 column by using acetonitrileand potassium dihydrogen phosphate as the mobile phase (60:40 v/v) having a flow rate of 0.8 ml/minute. Theeluent was detected at 254 nm, simultaneously for both the drugs. The retention time for pyrimethamine andsulfamethoxypyrazine was found to be 3.33 and 4.21 minutes, respectively. According to the International Conferenceon Harmonisation guidelines, the develop method was validated in terms of accuracy, precision, linearity, limit ofdetection, limit of quantitation, robustness, and stress degradation studies. This validated method can be suggested forthe routine simultaneous laboratory analysis of pyrimethamine and sulfamethoxypyrazine.
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The liquid chromatography mass spectrometry (LC-MS) compatible, stability-indicating, specific, linear, accurate, sensitive with less run-time related impurities reversed phase high-performance liquid chromatography (RP-HPLC) related impurities method has been developed for olmesartan medoxomil (OLM), chlorthalidone (CHLR), and cilnidipine (CIL) drug combinations, and the method has been validated according to ICH and US-FDA guidelines. The chromatographic separation was performed by using Hypersil-BDS Thermo-Scientific, C18 (12.5 cm, 4.6 mm, 5 microns particle size) column. Mobile phase-A was prepared by mixing 3.85 gm ammonium acetate in HPLC water and adjust pH 5.0 by using diluted acetic acid. Acetonitrile was taken as mobile phase-B. Initial mobile phase ratio (55:45 v/v) was adjusted for mobile phase-A: mobile phase-B followed by gradient program. Other chromatographic conditions such as column temperature 25 degrees, flow rate 1.0 mL/minutes with the detection wavelength at 260 nm. The retention time for CHLR impurity A, olmesartan (OL), OLM impurity A, were found about 2.7, 3.3, and 7.2 minutes respectively, with a total run time of 18.0 minutes. The linearity calibration plot was performed and found linear relationship over the concentration range of 1.25 limit of quantitation (LoQ)–18.75 μg/mL, 3.6 LoQ–60.0 μg/mL, 3.6 LoQ– 60.0 μg/mL respectively for CHLR impurity A, OL and OLM impurity A respectively. The limit of detection (LoD) and LoQ were found 0.4 ppm (μg/mL) and 1.2 ppm (μg/mL), 1.2 ppm (μg/mL) and 3.5 ppm (μg/mL), 1.1 ppm (μg/mL) and 3.3 ppm (μg/mL) for CHLR impurity A, OL and OLM impurity A respectively. The accuracy was determined by recovery studies and was found between 90.0–110.0%. The developed analytical method has been validated for LoD-LoQ, specificity, linearity, accuracy, precision, robustness, and ruggedness, which were well within the acceptance limit as per ICH guidelines. All the degradation products generated by stress conditions were found to be well separated from one another (all drug components and impurities). The developed method with shorter runtime was successfully implemented for routine quality control and stability analysis to check the quality of OLM, CHLR, and CIL drug combinations.
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Objective: The current work is intended towards the development of a novel, simple and precise high-performance thin layer chromatographic (HPTLC) method coupled with a densitometer for the estimation of teriflunomide (TEF) present in the marketed formulation. Methods: The chromatographic development was performed on aluminum plates coated with silica gel 60 F254 using toluene: ethyl acetate: glacial acetic acid (7.5:2: 0.5 v/v/v) as the mobile phase. Densitometric scanning was achieved at the absorbance maxima, UV 284 nm. Results: Well separated band was observed with Rf value 0.46. The calibration curve plotted in the concentration range 100-700ng/band exhibited an excellent linear relationship with the r2 value of 0.9928. The method was found to comply with all the validation parameters as per the ICH guidelines. Conclusion: The method ensures minimal use of mobile phase with minimal run time compared to other reported analytical methods. This validated method can be used by quality control laboratories for the routine quantitative analysis of tablets consisting of Teriflunomide.
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Abstract: Simple, specific, accurate and cost economic UV spectrophotometric methods weredeveloped and validated for determination of Donepezil Hydrochloride. Instead of usingorganic solvents, mixture of Acetonitrile and water was used during method development andvalidation. Donepezil hydrochloride standard solution was scanned in the UV range (400-200nm) in a 1cm quartz cell in a double beam UV spectrophotometer. The standard solution ofDonepezil Hydrochloride showed maximum absorption at wavelength 231 nm. The methodobeys Beer’s law in the concentration range from 4-20µg/ml. The correlation coefficient wasfound to be 0.9983and regression of the curve was found Y=0.0376x+0.0185 with excellentrecovery 99.66-100.83%. Limit of detection and limit of quantification were found to be0.197µg/ml and 0.6µg/ml respectively. The ruggedness and robustness were performed. Themethod was validated for several parameters like accuracy, precision as per ICH guidelines.Statistical analysis proved that the methods are repeatable and specific for determination ofthe drug. These methods can be adopted in the routine assay analysis of DonepezilHydrochloride in API and pharmaceutical dosage form.
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Lidocaine (LDC) and prilocaine (PLC) are estimated in a topical local anesthetic cream using a direct, eco-friendly,stability-indicating gas chromatographic technique with flame ionization detector. The mixture of LDC and PLCwas separated using Zebron DB drug column. The column temperature and flow rate were 230°C and 14 ml/minute,respectively. The retention time was found to be 5.1 minutes for PLC and 5.4 minutes for LDC. Linearity was observedin the concentration range of 20–100 μg/ml and 10–50 μg/ml for LDC and PLC, respectively. The method was validatedand values of linearity, limit of detection, limit of quantification, precision, and accuracy were found to be in goodaccordance with the International Conference on Harmonization guideline. A direct, stability-indicating method wasdeveloped for the determination of LDC and PLC in topical dosage forms in the presence of its degradation products.The proposed method can be useful in the quality control of LDC and PLC in their topical formulation.
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Lidocaine (LDC) and prilocaine (PLC) are estimated in a topical local anesthetic cream using a direct, eco-friendly,stability-indicating gas chromatographic technique with flame ionization detector. The mixture of LDC and PLCwas separated using Zebron DB drug column. The column temperature and flow rate were 230°C and 14 ml/minute,respectively. The retention time was found to be 5.1 minutes for PLC and 5.4 minutes for LDC. Linearity was observedin the concentration range of 20–100 μg/ml and 10–50 μg/ml for LDC and PLC, respectively. The method was validatedand values of linearity, limit of detection, limit of quantification, precision, and accuracy were found to be in goodaccordance with the International Conference on Harmonization guideline. A direct, stability-indicating method wasdeveloped for the determination of LDC and PLC in topical dosage forms in the presence of its degradation products.The proposed method can be useful in the quality control of LDC and PLC in their topical formulation.
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An accurate RP-HPLC method developed for the estimation of Neratinib in bulk and tablet dosage form. The method is and validated for parameters linearity, accuracy, suitability, specificity, precession, LOD, LOQ and robustness. An Altima column (150 mm × 4.6 mm × 5µ) used for chromatographic separation within a runtime of 6 min. The mobile phase buffer (monopotassium phosphate) and acetonitrile (60:40 v/v) with 0.1% formic acid is used. The flow rate maintained at 1.0 ml/min with the effluents monitored at 215 nm. The Neratinib analyzed at retention time of 4.001. The concentration linear over 30-180µg/ml with regression equation y = 6065.6x + 795.43 and regression co-efficient 0.999.
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Objective: The aim of the present work was to develop and validate a simple UV spectroscopic method for the determination of duloxetine, which is a thiophene derivative and a selective neurotransmitter reuptake inhibitor for serotonin, norepinephrine, and to lesser degree dopamine. Methods: The UV Spectrophotometric analysis was performed using Shimadzu UV-1800 and Shimadzu UV-1700 spectrophotometer by using solvent system acetonitrile and water in the ratio of 8:2. Detection was performed at a wavelength of 290 nm. Method validation was carried out according to ICH Q2R1 guidelines by taking the parameters linearity, accuracy, precision, ruggedness, and robustness, LOD and LOQ. Results: The UV Spectrophotometric method was found linear in the range of 10-50 μg/ml. The method was rugged and robust with % relative standard deviation less than 2. The extraction recoveries were found to be higher than 99% in all experimental conditions. Conclusion: Based upon the performance characteristics, the proposed method was found accurate, precise and rapid and suitable for the determination of Duloxetine for routine analysis.
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Objective: To develop an innovative, rapid, simple, cost-effective, stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for simultaneous estimation of ledipasvir (LP) and sofosbuvir (SB) in combination pill dosage form. Methods: The method was developed using C8 column, 250 mm x 4.6 mm, 5 mm using mobile section comprising of 0.1% (v/v) orthophosphoric acid buffer at pH 2.2 and acetonitrile in the ratio of 45:55 that was pumped through the column at a flow rate of 0.8 ml/min. Temperature was maintained at 30 °C, the effluents were monitored at 260 nm with the help of usage of PDA detector. Results: The retention time of LP and SB were found to be 2.246 min and 3.502 min. The approach was found to be linear with the variety of 9-36 µg/ml and 40-240 μg/ml for LP and SB respectively, the assay of estimated compounds were found to be 99.65% and 99.73% w/v for LP and SB respectively. Conclusion: The pressured samples changed into analyzed and this proposed a technique turned into determined to be particular and stability indicating as no interfering peaks of decay compound and excipients were observed. Hence, the approach was easy and economical that may be efficiently applied for simultaneous estimation of both LP and SB in bulk and combination tablet system.
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Objective: The present work was undertaken with an aim to develop and validate a rapid reverse-phase high-performance liquid chromatography (RP-HPLC) method for the estimation of curcumin and cyclosporine in the capsule dosage form. Methods: The RP-HPLC method for the simultaneous estimation of curcumin and cyclosporine was developed using Agilent (Infinity 1260) HPLC system and Eclipse XDB-C18 (4.6 x 150 mm i.d., 5µ) stationary phase. The optimized mobile phase comprised of acetonitrile: water: methanol (50: 10: 40 v/v/v) pumped at a flow rate of 0.5 ml/min. Separation of drugs was achieved in an isocratic mode and elution was monitored using PDA detector at 214 nm. The method was validated as per ICH-Q2R1 guidelines. Results: Retention time of the curcumin and cyclosporine were found to be 3.073 min and 6.373 min with the correlation coefficient (R2) of 0.9993 and 0.998 respectively. The response of curcumin and cyclosporine was found linear in the concentration range of 8-48 μg/ml and 4-24 μg/ml respectively. The percent recovery values were found in the range of 97-103% indicating satisfactory accuracy of the method. The percent relative standard deviation (% RSD) values for the precision study was less than 2 which suggest that the method is precise. Conclusion: The proposed method was found accurate, precise and specific for the determination of curcumin and cyclosporine in bulk as well as in capsule dosage form. Thus, the present method can be used for routine analysis and quality control of curcumin and cyclosporine in bulk and capsule dosage form.
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A stability indicating simple, selective, accurate high Performance Liquid Chromatographic (HPLC) method was developed and validated for the combined tablet formulation of pyrimethamine & sulphadoxine. Chromatographic separation was optimized by gradient HPLC on a C18 column [Inertsil Silica, 250 x 4.6 mm, 5μ] utilizing a mobile phase of potassium dihydrogen phosphate and acetonitrile taken in the ratio 70:30 at a flow rate of 1.0 ml/min with UV detection at 221nm. The retention time of pyrimethamine and sulphadoxine was 2.77 and 6.57 min respectively. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantitation, robustness and stress degradation studies. Validation of the method was done in accordance with ICH guidelines for the assay of active ingredients. Thus validated method can be recommended for the routine laboratory analysis.
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A simple, specific, accurate and precise new high performance liquid chromatographic method was developed for the estimation of irbesartan in bulk and its developed dosage form. The mobile phase containing acetonitrile: Phosphate buffer pH 3.5 in proportion of 50:50 v/v was employed with flow rate of1.0 ml/min and eluting medium was monitored at 240 nm. The method was validated for linearity, accuracy, precision, limit of detection, limit of quantification and robustness for irbesartan. A linear response was observed in the range of 5- 40µg/ml. Linear regression of absorbance on concentration gave equation y = 101.9x + 195.3 with a regression co-efficient r2 =0.993. The method was validated for different parameters as per the ICH guidelines. The degradation studies were carried out by using the developed method. Thus the method was found to be useful for the determination of irbesartan in bulk as well as for dosage forms.
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A Fourier transform infrared (FTIR) spectrophotometric method was developed for rapid and direct measurement of efavirenz in pharmaceutical formulations. The method involves extraction of efavirenz from tablets with chloroform by sonication and the direct measurement of the absorbance in liquid phase using a reduced path length cell. In general, the spectrum was measured in transmission mode. The equipment was configured to collect a spectrum at 8 cm-1 resolution and 45 scans per sec .The spectra were collected between 4000 cm-1 and 450cm-1, the band obtained at 1750cm-1 (carbonyl group) showed intense, clear peak in the liquid phase for quantitation. The method was validated as per ICH guidelines. The method fulfilled most validation requirements in the linearity range 200-1000μg/mL. The coefficient of determination, limit of detection and quantification was found to be 0.993, 49.12μg/mL and 148.84μg/mL respectively. Results of developed FTIR method were compared with the results obtained with the existing UV method statistically by using t-test, which indicated that there is no significant difference between the methods at P=0.05. The proposed FTIR method reduces the solvent consumption and also eliminates the use of reagents. Thus the developed method offers a good alternative for the quantitative estimation of efavirenz in bulk and pharmaceutical dosage forms and also to quantify efavirenz when combined with other API in the same dosage form.
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A new simple, sensitive and specific procedure has been developed for determination of tenofovir disoproxil fumarate in bulk and pharmaceutical dosage forms using MBTH reagent. The purpose of this analytical validation procedure is to validate it by laboratory experiments to prove that the method meets the minimum standards for laboratory use. 3-methyl-2-bezothiazoline hydrazone reacts with the secondary amine group of tenofovir in the presence of oxidizing agent, ferric chloride. The resulting apple green coloured chromogen when measured spectrophotometrically in visible region (i.e., 400-800nm) shows a maximum absorbance at 626.5nm. This method can be successfully applied for the determination of drug content in pharmaceutical formulations. The results of analysis have been validated statistically.
ABSTRACT
A Fourier transform infrared (FTIR) spectrophotometric method was developed for rapid and direct measurement of efavirenz in pharmaceutical formulations. The method involves extraction of efavirenz from tablets with chloroform by sonication and the direct measurement of the absorbance in liquid phase using a reduced path length cell. In general, the spectrum was measured in transmission mode. The equipment was configured to collect a spectrum at 8 cm-1 resolution and 45 scans per sec .The spectra were collected between 4000 cm-1 and 450cm-1, the band obtained at 1750cm-1 (carbonyl group) showed intense, clear peak in the liquid phase for quantitation. The method was validated as per ICH guidelines. The method fulfilled most validation requirements in the linearity range 200-1000μg/mL. The coefficient of determination, limit of detection and quantification was found to be 0.993, 49.12μg/mL and 148.84μg/mL respectively. Results of developed FTIR method were compared with the results obtained with the existing UV method statistically by using t-test, which indicated that there is no significant difference between the methods at P=0.05. The proposed FTIR method reduces the solvent consumption and also eliminates the use of reagents. Thus the developed method offers a good alternative for the quantitative estimation of efavirenz in bulk and pharmaceutical dosage forms and also to quantify efavirenz when combined with other API in the same dosage form.
ABSTRACT
A new simple, sensitive and specific procedure has been developed for determination of tenofovir disoproxil fumarate in bulk and pharmaceutical dosage forms using MBTH reagent. The purpose of this analytical validation procedure is to validate it by laboratory experiments to prove that the method meets the minimum standards for laboratory use. 3-methyl-2-bezothiazoline hydrazone reacts with the secondary amine group of tenofovir in the presence of oxidizing agent, ferric chloride. The resulting apple green coloured chromogen when measured spectrophotometrically in visible region (i.e., 400-800nm) shows a maximum absorbance at 626.5nm. This method can be successfully applied for the determination of drug content in pharmaceutical formulations. The results of analysis have been validated statistically.
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A simple, rapid, precise, and economical spectrophotometric method has been developed for quantitative analysis of Raltegravir Potassium (RALP) in tablet formulations. The stock solution of RALP was prepared in water. The standard solution of RALP in water showed absorption maxima at 331.6 nm. The drug obeyed Beer–Lambert’s law in the concentration range of 1–100 μg/mL with coefficient of correlation (R2) was 0.9999. It showed coefficient of variation below 2 % in intra-run and inter-run precision. The recovery was obtained with values close to the 100 % of theoretical at three different concentrations. The results of analysis have been validated as per ICH guidelines. The method can be adopted in routine analysis of RALP in bulk and tablet dosage form and it involves water as a solvent and no complex extraction techniques.
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Objective: To develop and validate a simple, accurate HPTLC method for the analysis of 8-gingerol and to determine the quantity of 8-gingerol in Zingiber officinale extract and ginger-containing dietary supplements, teas and commercial creams. Methods:The analysis was performed on 10×20 cm aluminium-backed plates coated with 0.2 mm layers of silica gel 60 F254 (E-Merck, Germany) with n-hexane: ethyl acetate 60: 40 (v/v) as mobile phase. Camag TLC Scanner III was used for the UV densitometric scanning at 569. Results:This system was found to give a compact spot of 8-gingerol at retention factor (Rf) value of (0.39±0.04) and linearity was found in the ranges 50-500 ng/spot (r2=0.9987). Limit of detection (12.76 ng/spot), limit of quantification (26.32 ng/spot), accuracy (less than 2 %) and recovery (ranging from 98.22-99.20) were found satisfactory. Conclusions:The HPTLC method developed for quantification of 8-gingerol was found to be simple, accurate, reproducible, sensitive and is applicable to the analysis of 8-gingerol in Zingiber officinale extract and ginger-containing dietary supplements, teas and commercial creams.