Current Issue : October - December Volume : 2014 Issue Number : 4 Articles : 13 Articles
A specific, accurate and precise stability indicating high-performance thin layer chromatographic method for estimation of flupirtine maleate in pharmaceutical formulation was developed and validated. The method employed TLC aluminium plates precoated with silica gel 60F254 as the stationary phase. The solvent system consisted of ethyl acetate: chloroform: ammonia (25%); (9.0:1.0:0.2 v/v/v) which gave compact and dense spots for flupirtine maleate (Rf: 0.67±0.02). Densitometric analysis of drug was carried out in the reflectance-absorbance mode at 320 nm. The linear regression analysis data for the calibration plots showed a good linear relationship with R2 = 0.9976 in the concentration range 100-500 ng/spot for flupirtine maleate. The method was validated with respect to linearity, specificity, accuracy, precision, limit of detection and limit of quantitation. The drug was subjected to acidic, alkaline, water hydrolysis, oxidation, thermal stress and photo degradation studies. The method could effectively separate the drug in presence of its degradation products and can be applied for analysis of pharmaceutical formulation of flupirtine....
A simple, accurate, precise, sensitive, specific and rapid HPTLC method was developed for simultaneous estimation of ethinyl estradiol and levonorgestrel in pharmaceutical dosage form. The developed method with mobile phase CHCl3: toluene: methanol (8:1:0.5 v/v/v), precoated silica gel on aluminum plate 60F254, (10 cm × 10 cm), used as stationary phase, chamber saturation time is 20 minutes. Detection was carried out at 230 nm UV detector. Rf value was found to be 0.4±0.004 and 0.6±0.007 for ethinyl estradiol and levonorgestrel respectively. The calibration curve of Ethinyl estradiol and Levonorgestrel was found to be linear in the range of 300-1800 ng/band and 1500-9000 ng/band respectively. The proposed method has been validated for precision, accuracy, robustness. Accuracy was performed by recovery studies at 80%, 100%, 120%. % recovery for ethinyl estradiol was found to be 99.03% - 99.96% and for levonorgestrel, it was 99.66% - 100.2%. LOD and LOQ values for ethinyl estradiol was 40.71 ng/band and 123.10 ng/band respectively and for levonorgestrel 397.03 ng/band and 1203.11 ng/band respectively. Precision of the method was assessed by performing repeatability, intra-day and inter-day precision studies. Thus, the developed method was found to be accurate, precise and relatively simple for the simultaneous estimation of ethinyl estradiol and levonorgestrel in pure form as well as in marketed formulation....
Lawsonia inermis L. (Lawsone) is an analgesic, hypoglycemic, hepatoprotective, immunostimulant, anti-inflammatory, antibacterial plant drug which have a unique pharmacological action. A stability-indicating RP-HPLC method was developed and validated for the determination of lawsone by using enable C18 column (150 × 4.6 mm, 5 μm) in isocratic mode. The mobile phase consisted of acetonitrile: methanol: water (34:66, v/v) with a flow rate of 1.0 ml/min (UV detection- 269 nm). The retention time was found to be 7.4 min. Linearity was observed between the concentration range of 40 μg/ml to 90 μg/ml and the correlation coefficient R2 value was found to be 0.999±00.13. The method is accurate and recovery was found to be in the range of 100-101.9%. The limit of detection of lawsone was found to be 6.28 μg/ml and limit of quantitation was found to be 19.05 μg/ml. Lawsone was subjected to stress conditions including acidic, alkaline, neutral, oxidation and dry heat degradation. Lawsone is more sensitive to acidic and oxidative degradation. The method was validated according to ICH guidelines....
The aim of present work was to develop an accurate, simple and cost effective UV spectrophotometric method for estimation of lumefantrine. This method was based on area under curve of UV spectrum between 290 to 310 nm and validated as per ICH guideline Q2 (R1). The method has followed linearity in the range of 10-40 μg/ml. The value of correlation coefficient was 0.9992. Satisfactory values of percent relative standard deviation for the intra-day and inter-day precision indicated that method is precise. Results of the recovery studies (99.09% to 99.40%) shows accuracy of the method. LOD and LOQ were calculated as 0.77 μg/ml and 2.34 μg/ml, respectively. The developed method can be used for routine estimation of lumefantrine in bulk and various dosage forms....
HPTLC (high performance thin layer chromatography) is playing an important role in today analytical world, not in competition to HPLC but as a complementary method. This study presents the first report of sensitive, selective, precise and robust HPTLC method, which has been developed and validated for quantification of the rubiadin using the solvent system of toluene: acetonitrile: ethyl acetate: formic acid (10: 1: 2.5: 2 v/v/v/v). The method employed HPTLC aluminium plates precoated with silica gel 60 F254 as a stationary phase as the stationary phase. Densitometric analysis of rubiadin was carried out in the absorbance mode at 280 nm by using camag TLC scanner-3. This system was found to give compact spot of rubiadin at R f value of 0.70 with good linear relationship i.e. r2 = 0.9984. The method was validated using ICH guidelines in terms of specificity, precision, robustness, stability and repeatability. The repeatability of the method was found to be 1.25 RSD and recovery values from 98.40 to 100.28% for rubiadin. Statistical analysis proves that the method is repeatable and selective for the estimation of the said drug. Since the proposed mobile phase effectively resolves the rubiadin, this HPTLC method can be applied for identification and quantitation of these phytochemical in herbal extracts and pharmaceutical dosage form....
A simple, sensitive, precise and stability indicating high performance thin layer chromatographic method of analysis of lacidipine in bulk as well as formulation was developed and validated. The method employed TLC aluminium plates precoated with silica gel 60F-254 as the stationary phase using mobile phase toluene: ethylacetate: glacial acetic acid (6.5:2.5:1 v/v/v). It gives compact spots for lacidipine (Rf value 0.43). The drug was subjected to stress degradation conditions like acid, alkaline, oxidative, photo and thermal degradation. Densitometric analysis of lacidipine was carried out in the absorbance mode at 281 nm. The method was validated for specificity, linearity, precision, accuracy, robustness and solution stability. Method was found to be linear with correlation coefficient 0.998 and also found to be robust as % RSD values are less than 2%. Stress degradation study shows that lacidipine undergoes degradation in acid, base and oxidation (13.41%, 11.29% and 8.49% respectively)....
Rheumatoid arthritis is a progressive chronic inflammatory disease characterized by the activation of synovial tissue lining the joint capsule, which results in the invasion of the cartilage and bone leading to the progressive joint dysfunction. Hence the herbal formulation containing guggul, haridra has been developed. Guggul and haridra which are reported to have string anti-arthritic and anti-inflammatory activity. Guggulsterone E and Z are the active principles present in the guggul extracts and responsible of the anti-arthritic activity. Haridra is also reported to have anti-inflammatory activity and curcumin is the compound provides that’s said potential to haridra. The development of a stable polyherbal formulation is a challenging task because of the large number of varied chemical compounds present in the different medicinal plants. Hence, in the present study the attempt has been made to evaluate the quality of the formulation by using high performance thin layer chromatography. In the present research we have developed the HPTLC method which is capable to identify and determine the amount of guggulesterone E, Z and curcumin....
Analysis of menthol obtained from the extraction of menthol from the formulation was done by the proposed method. Identification and determination were performed by BP-1 Column (30.0 m × 0.32 mm ID) using nitrogen at a flow rate of 3.0 ml/min using FID detector. The developed conditions for GC were column oven temperature (75°C-15 min-@40°C/min-170°C-3 min), total run time (20 min), injection temperature (220°C), detector temperature (260°C) and sample volume for injection was 1 μl. The retention time for menthol was found to be 13.64 min. The linearity range was found to be 1250-6250 µg/ml for menthol. The LOD and LOQ value for menthol was found to be 105.87 µg/ml and 320.83 µg/ml. The method was validated for linearity, accuracy, precision and specificity....
Analysis of Menthol obtained from extraction from the formulation was done by the proposed method. Separation of drug was achieved employing toluene: ethyl acetate (93:7) as the mobile phase on a pre-coated silica gel aluminium plate 60F254 using vanillin-sulphuric acid as colouring reagent. Quantitation was carried out in absorbance mode at 460 nm. The method showed good linearity in the range of 5-25 μg/band, method was found being precise on intra-day and inter day basis as the average % CV value for the determination of menthol was found to be 0.223 – 0.356 and 0.313 - 0.463 respectively. The method showed % mean recovery of 98.74±0.43% and 98.62±0.49 for cold rub vaporizing ointment and menthosil nasal inhaler respectively. The LOD and LOQ for estimation of menthol were found to be 0.33 and 1.00 μg/band respectively. The method was validated for linearity, accuracy, precision and specificity....
The impurities in pharmaceuticals are unwanted chemicals that remain with the active pharmaceutical ingredients (APIs) or develop during formulation or upon aging of both API and formulation. The presence of these unwanted chemicals even in trace amount may influence the efficacy and safety of pharmaceutical product. The current practice of characterization and control of impurities in pharmaceutical substances and products are reviewed with emphasis on issues specific to the active pharmaceutical ingredient and pharmaceutical formulations. The international conference on harmonization (ICH) has formulated a workable guideline regarding the control of impurities in pharmaceutical drug substance as well as formulations. Thus enlightening the need of impurity profiling in pharmaceutical research this review focuses on various tools available for optimization and characterization of impurities present in the pharmaceuticals....
A simple, rapid, accurate and precise vierordt’s method was developed for the simultaneous estimation of domperidone and ilaprazole in pure and capsule dosage form. Domperidone and ilaprazole exhibited absorbance maximum (λmax) at 286.4nm and 302.4nm in methanol. Based on their λmax, both the drugs were analysed by simultaneous equation method or vierordt’s method using precise formula. The developed method was validated for linearity, range, accuracy, precision, robustness and specificity, limit of detection and limit of quantitation as per ICH guidelines. Linearity of domperidone and ilaprazole were found to be 9 -27 µg/ml and 3-9 µg/ml respectively with significantly high value of correlation coefficient (R2). The limit of detection and limit of quantification for domperidone and ilaprazole were found to be 118.66 ng/ml, 359.59 ng/ml and 66.53 ng/ml, 201.61 ng/ml respectively. The proposed vierordt’s method was found to be efficient, precise, accurate, specific and useful for the regular analysis of domperidone and ilaprazole in pure and pharmaceutical dosage form....
Two sensitive spectrophotometric methods; using first derivative 1D spectrophotometry (method I) and dual wavelength spectrophotometry (method II), were developed and validated for the simultaneous determination of dexketoprofen trometamol and tramadol HCl in binary mixtures and synthetic mixture. Method I was based on measuring 1D at 242 nm for determination of dexketoprofen trometamol and 1D at 232 nm for determination of tramadol HCl. Method II was based on measuring the absorbance difference between 259 nm and 281.6 nm for determination of dexketoprofen trometamol and between 225 nm and 281 nm for determination of tramadol HCl. Linearity range for dexketoprofen trometamol using methods I and II was found to be 4.00–30.00 µg.ml-1. For tramadol HCl the linearity range was found to be 20.00–100.00 µg.ml-1 for both methods. The developed methods were successfully applied for the determination of dexketoprofen trometamol and tramadol HCl in synthetic mixture containing all possible excipients present in tablet dosage form. The mean percentage recovery values were found to be 98.68±0.34 and 99.34±0.48 for method I and 101.05±0.41, 101.13±0.54 for method II for dexketoprofen trometamol and tramadol HCl, respectively....
The present work describes development and validation of a specific, sensitive, precise and stability-indicating high-performance liquid chromatographic method of analysis of levocetirizine hydrochloride, as a bulk drug. The separation was achieved by using a mobile phase of acetonitrile: potassium dihydrogen phosphate buffer 0.1 M pH 3.5 (35:65, v/v) and Thermo BDS-hypersil column (250 mm X 4.6 mm, 5 μm) at flow rate of 1.0 ml/min. The detection was done at 230 nm. The retention time of levocetirizine hydrochloride was 7.3±0.01 min. This method has been successively applied to pharmaceutical dosage form. No chromatographic interference from the tablet excipient was found. Levocetirizine hydrochloride was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. The degraded products were well resolved from the pure drug with significantly different retention time values. Linearity was found to be in the range of 0.5–20 μg/ml with significantly high value of correlation coefficient. The method was validated for precision, robustness and recovery. The limit of detection and quantization were 0.129 μg/ml and 0.39 μg/ml. The acid degraded product of levocetirizine hydrochloride was subjected to LC-MS analysis. From the mass spectral data of degraded product, possible degradation pathway was outlined....
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