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1.
ABSTRACT: BACKGROUND: A simple, specific, and fast stability indicating reverse phase liquid chromatographic method was established for instantaneous determination of moxifloxacin and prednisolone in bulk drugs and pharmaceutical formulations. RESULTS: Optimum chromatographic separations among the moxifloxacin, prednisolone and stressinduced degradation products were achieved within 10 minutes by use of BDS Hypersil C8 column (250 X 4.6 mm, 5 mum) as stationary phase with mobile phase consisted of a mixture of phosphate buffer (18 mM) containing 0.1% (v/v) triethylamine, at pH 2.8 (adjusted with dilute phosphoric acid) and methanol (38:62 v/v) at a flow rate of 1.5 mL min-1. Detection was performed at 254 nm using diode array detector. The method was validated in accordance with ICH guidelines. Response was a linear function of concentrations over the range of 20-80 mug mL-1 for moxifloxacin (r2 [greater than or equal to] 0.998) and 40-160 mug mL-1 for prednisolone (r2 [greater than or equal to] 0.998). The method was resulted in good separation of both the analytes and degradation products with acceptable tailing and resolution. The peak purity index for both the analytes after all types of stress conditions was [greater than or equal to] 0.9999 indicated a complete separation of both the analyte peaks from degradation products. The method can therefore, be regarded as stabilityindicating. CONCLUSIONS: The developed method can be applied successfully for simultaneous determination of moxifloxacin and prednisolone in pharmaceutical formulations and their stability studies.  相似文献   

2.
Second derivative-spectrophotometric and high-performance liquid chromatographic methods for the determination of prednisolone in pharmaceutical formulations have been developed. Determination of prednisolone in tablets was conducted by using a second-order derivative UV spectrophotometric method at 250 nm (n = 5). Standards for the calibration graph ranging from 5.0 to 35.0 microg/ml were prepared from stock solution. The proposed method was accurate, with 98% recovery value, and precise, with a coefficient of variation (CV) of 1.38. These results were compared with those obtained by an exclusively developed isocratic reversed-phase high-performance liquid chromatography (HPLC) method. An isocratic reversed-phase Bondapak C(18) column with acetonitrile-citrophosphate buffer (pH 5; 45:55 v/v) mobile phase was used and UV detector was set to 241 nm using 11 alpha-hydroxyprogesterone as an internal standard. Calibration solutions used in HPLC were in the range from 2 to 300 microg/ml. Results obtained by derivative UV spectrophotometric method were comparable to those obtained by HPLC method, as far as analysis of variance (ANOVA) test, F(calculated), 0.762 and F(theoretical), 3.89, results were concerned.  相似文献   

3.
Sorbitol and glycerol, along with other inactive ingredients such as preservatives and dyes, are commonly used in various pharmaceutical and personal care products. To accurately assess the effectiveness of various formulations containing sorbitol and/or glycerol, their quantitative determination is essential. In the current study, two types of detectors (a Varian evaporative light scattering detector and an Agilent ultraviolet-visible detector) are evaluated for the assay of working sample solutions. The two detection techniques are complimentary, and a comparison of the results obtained using the two detectors is presented here. The current method is shown to be stability-indicating and free from interference from any of the formulation excipients and potential degradation products. The method is reproducible, accurate, sensitive and selective. It provides enhanced detection sensitivity for sorbitol and comparable sensitivity for glycerol versus similar methods reported in the literature that utilize a refractive index detector for the analysis of either of the two polyols.  相似文献   

4.
Simple, sensitive and accurate thin layer procedure was described for a quantitative determination of paracetamol in its bulk powder and in its pharmaceutical dosage forms in the presence of its degradation product. The method consists of dissolving the drug in methanol and then spotting the solution on a thin layer of silica gel G254. Paracetamol was separated on silica gel using the mixture of the mobile phase, ethyl acetate: benzene: acetic acid in a ratio (1:1:0.05 v/v/v).Absorbance measurements (detection of reflectance) of the separated drug were carried out at 250 nm. Calibration curves were established in the concentration range of 5–20 mcg/spot for paracetamol. Quantitation is achieved by comparing the area under the peaks obtained from scanning the thin layer chromatographic plates in a spectrodensitometer. The method has been successfully applied to pharmaceutical preparations (capsules) and the results obtained were statistically compared with those obtained by applying the reference method.  相似文献   

5.
Preservatives are used to protect pharmaceutical formulations from microbial attack during the period of administration to the patient. Because of their biological activity, preservatives have to be identified and assayed according to the same rules as apply to active components. A number of methods for separation of preservatives are reported, to account for the heterogeneity of their chemical structures. A capillary electrophoretic method was devised for simple and simultaneous qualification and quantification of the preservatives most often included in pharmaceuticals, such as benzyl alcohol, parabens, phenol, m-cresol, chlorobutanol, thimerosal. After systematic method development, the electrophoretic conditions were defined as: 50 mM borate buffer pH 9.0 containing 20 mM SDS. Separations were performed at a temperature of 20 degrees C and with detection at 214 nm. Preservatives under examination can be analyzed within a 10 min run. The method was successfully validated and applied to the determination of preservatives in a number of pharmaceuticals. Results from the CE method were compared with those from reference methods.  相似文献   

6.
7.
A micellar electrokinetic chromatography (MEKC) method for the simultaneous determination of the antiviral drugs acyclovir and valacyclovir and their major impurity, guanine, was developed. The influences of several factors (surfactant and buffer concentration, pH, applied voltage, capillary temperature and injection time) were studied. Using tyramine hydrochloride as internal standard, the analytes were all separated in about 4 min. The separation was carried out in reversed polarity mode at 28°C, 25 kV and using hydrodynamic injection (15 s). The separation was effected in a fused‐silica capillary 100 μm × 56 cm and a background electrolyte of 20 mM citric acid–1 M Tris solution (pH 2.75), containing 125 mM sodium dodecyl sulphate and detection at 254 nm. The method was validated with respect to linearity, limit of detection and quantification, accuracy, precision and selectivity. Calibration curves were linear over the range 0.1–1 μg/mL (guanine) and from 0.1 to 120 μg/mL for both valacyclovir and acyclovir. The relative standard deviations of intra‐ and inter‐day migration times and corrected peak areas were less than 5.0%. The proposed method was successfully applied to the determination of the analytes in tablets and creams. From the previous study it is concluded that the stability‐indicating method developed for acyclovir and valacyclovir can be used for analysis of the drug in various stability samples. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

8.
A quick, accurate, reproducible high performance liquid chromatographic (HPLC) method for the determination of clenbuterol in the presence of some common pharmaceutical preservatives (i.e., methyl and propyl paraben) is described. The method is specific enough to separate and determine clenbuterol in the presence of degradation products of the formulation components. Extraction of interfering formulation components provides the necessary clean-up to determine clenbuterol via HPLC.  相似文献   

9.
 A simple and fast analytical procedure is proposed for the simultaneous determination of paracetamol, acetylsalicylic acid and caffeine in pharmaceuticals by means the partial least square treatment of the spectrophotometric absorbance data between 216 and 300 nm, taken at 5 nm intervals. The method involves the use of 8 standard mixtures of the three compounds assayed, considered at two concentration levels, and the measurement of the absorbance of samples in a 20% (v/v) ethanol in water solution previously filtered. In the analysis of real and synthetic samples precise and accurate values were obtained by the aforementioned procedure, providing in all cases variation coefficients and accuracy errors lower than 5% which agree with the tolerance level established by the pharmacopoeia for this kind of samples which is ±10%. Received: 10 May 1996 / Revised: 8 July 1996 / Accepted: 12 July 1996  相似文献   

10.
An HPLC method with DAD detection was developed and validated for the simultaneous determination of zofenopril and hydrochlorothiazide in tablets. The separation was carried out through a gradient elution using an Agilent LiChrospher C18 column (250×4.0 mm id, 5 μm) and a mobile phase consisting of (A) water–TFA (99.9:0.1 v/v) and (B) acetonitrile–TFA (99.1:0.1 v/v) delivered at a flow‐rate of 1.0 mL/min. 8‐Chlorotheophylline was used as internal standard. Calibration curves were found to be linear for the two drugs over the concentration ranges of 5.0–40 and 1.0–20 μg/mL for zofenopril and hydrochlorothiazide, respectively. Linearity, precision, accuracy, specificity and robustness were determined in order to validate the proposed method, which was further applied to the analysis of commercial tablets. The proposed method is simple and rapid, and gives accurate and precise results.  相似文献   

11.
The study describes development and subsequent validation of a stability indicating reverse-phase HPLC method for the simultaneous estimation of atorvastatin (ATV), and amlodipine (AML) from their combination drug product. The proposed RP-HPLC method utilizes a Lichrospher 100 C18, 5 microm, 250 mm x 4.0 mm i.d. column, at ambient temperature, optimum mobile phase consisted of acetonitrile and 50 mM potassium dihydrogen phosphate buffer (60 : 40, v/v), apparent pH adjusted to 3+/-0.1 with 10% phosphoric acid solution, effluent flow rate monitored at 1.0 ml/min, and UV detection at 254 nm. ATV, AML, and their combination drug product were exposed to thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by proposed method. The method was applied for the in vitro dissolution of marketed combination drug products. The described method was linear over the range of 1-90 microg/ml and 1-80 microg/ml for ATV and AML, respectively. The mean recoveries were 99.76 and 98.12% for ATV and AML, respectively. The intermediate precision data obtained under different experimental setup, the calculated value of coefficient of variation (CV, %) was found to be less than critical value. The limit of detection for ATV and AML were found to be 0.4 and 0.6 mug/ml, respectively and the limit of quantification was 1.0 microg/ml for both drugs. The average percentage drug release was found to be more than 70% within 30 min for both drugs. Chromatographic peak purity data of ATV and AML indicated no co-eluting peaks with the main peaks of drugs which demonstrated the specificity of assay method for their estimation in presence of degradation products. The proposed method can be useful in the quality control and in vitro dissolution of combination drug products.  相似文献   

12.
Two sensitive and reproducible methods were developed and validated for the determination of ziprasidone (ZIP) in the presence of its degradation products in pure form and in pharmaceutical formulations. The fi rst method was based on reversed-phase high-performance liquid chromatography (HPLC), on a Lichrosorb RP C(18) column using water:acetonitrile:phosphoric acid (76:24:0.5 v/v/v) as the mobile phase at a fl ow rate of 1.5 mL min(-1) at ambient temperature. Quantification was achieved with UV detection at 229 nm over a concentration range of 10-500 micro g mL(-1) with mean percentage recovery of 99.71 +/- 0.55. The method retained its accuracy in presence of up to 90% of ZIP degradation products. The second method was based on TLC separation of ZIP from its degradation products followed by densitometric measurement of the intact drug spot at 247 nm. The separation was carried out on aluminium sheet of silica gel 60 F(254) using choloroform:methanol:glacial acetic acid (75:5:4.5 v/v/v) as the mobile phase, over a concentration range of 1-10 micro g per spot and mean percentage recovery of 99.26 +/- 0.39. Both methods were applied successfully to laboratory prepared mixtures and pharmaceutical capsules.  相似文献   

13.
14.
Summary A simple, rapid and accurate, routine-HPLC method is described for simultaneous determination of acetaminophen, caffeine and chlorpheniramine maleate in a new tablet formulation Chromatographic separation of the three pharmaceuticals was achieved on a Hypersil CN column (150×5.0 mm, 5 μm) using a mobile phase comprising a mixture of acetonitrile, an ion-pair solution and tetrahydrofuran (13:14:87, v/v,pH4.5). The flow-rate was changed from 1.0 mL min−1 (in 0≈7.5 min) to 1.8 mL min−1 (after 3.5 min). was complete in <10 min. The method was validated for system suitability, linearity, accuracy, precision, limits of detection and quantitation, and robustness. Linearity, accuracy and precision were found to be acceptable over the ranges 31.6≈315.8 μg mL−1 for acetaminophen, 9.5≈94.6 μg mL−1 for caffeine and 1.4≈13.8 μg mL−1 for chlorpheniramine maleate.  相似文献   

15.
16.
A rapid procedure based on a direct extraction and HPLC determination with fluorescence detection of phenylephrine in pharmaceutical sachets that include a large excess of paracetamol (65 + 1, w/w), ascorbic acid (5 + 1, w/w), and other excipients (aspartame and sucrose) was developed and validated. The final optimized chromatographic method for ion-pair chromatography used an XTerra RP18 column, 3 microm particle size, 50 x 3.0 mm id. The mobile phase consisted of a mixture of acetonitrile and buffer (10 mM sodium octane-1-sulfonate, adjusted with H3PO4 to pH 2.2; 200 + 800, v/v), with a constant flow rate of 0.3 mL/min. The separation was carried out at 30 degrees C, and the injection volume was 3 microL. Fluorescence detection was performed at excitation and emission wavelengths of 275 and 310 nm, respectively. The mobile phase parameters, such as the organic solvent fraction (acetonitrile) in mobile phase as an organic modifier, the concentration of sodium octane-1-sulfonate as a counter-ion, temperature, and pH of mobile phase, were studied. As an alternative to ion-pair chromatography, hydrophilic interaction liquid chromatography (HILIC) was investigated using a Luna HILIC column, 3 microm, 100 x 4.6 mm id. The mobile phase consisted of acetonitrile and buffer (5 mM potassium dihydrogen phosphate, adjusted with H3PO4 to pH 2.5; 750 + 250, v/v) at a flow rate of 0.8 mL/min. The separation was carried out at 25 degrees C, and the injection volume was 5 microL. The proposed method has an advantage of a very simple sample pretreatment, and is much faster than the currently utilized HPLC methods using gradient elution and UV detection. Commercial samples of sachets were successfully analyzed by the proposed HPLC method.  相似文献   

17.
Reversed-phase high performance liquid chromatography (LC) method is developed for the assay of sodium montelukast in coated tables and its photodegradation kinetics. An isocratic LC separation is performed on a Zorbax XDB C18 column using a mobile phase of acetonitrile-methanol-water (pH 3.8) (75:10:15, v/v/v) at a flow rate of 0.8 mL/min and detection at 280 nm. The detector response for sodium montelukast is linear over the concentration range from 5-35 μg/mL (r = 0.9999). The specificity of the method is proved using stress conditions. The solutions are exposed to UV radiation (352 nm), alkaline and acid hydrolysis, oxidation, and temperature (80 °C). The intra- and inter-day precision show suitable results (RSD < 0.49%). The accuracy of analytical method is 100.04% (RSD = 0.44%). Detection and quantification limits are 0.10 and 0.32 μg/mL respectively. The robustness of the method is assured after small changes in chromatographic conditions. The kinetic of photodegradation using a LC method is established and it can be described by zero-order kinetics. This developed method show to be viable for the determination of sodium montelukast in pharmaceutical dosage form and satisfactory in the determination of the kinetics of degradation.  相似文献   

18.
The applicability of H-point standard additions method (HPSAM) to the resolving of overlapping spectra corresponding to the sulfamethoxazole and trimethoprim is verified by UV-vis spectrophotometry. The results show that the H-point standard additions method with simultaneous addition of both analytes is suitable for the simultaneous determination of sulfamethoxazole and trimethoprim in aqueous media. The results of applying the H-point standard additions method showed that the two drugs could be determined simultaneously with the concentration ratios of sulfamethoxazole to trimethoprim varying from 1:18 to 16:1 in the mixed samples. Also, the limits of detections were 0.58 and 0.37 μmol L(-1) for sulfamethoxazole and trimethoprim, respectively. In addition the means of the calculated RSD (%) were 1.63 and 2.01 for SMX and TMP, respectively in synthetic mixtures. The proposed method has been successfully applied to the simultaneous determination of sulfamethoxazole and trimethoprim in some synthetic, pharmaceutical formulation and biological fluid samples.  相似文献   

19.
New, simple, cost effective, accurate and reproducible UV-spectrophotometric methods were developed and validated for the estimation of moxifloxacin in bulk and pharmaceutical formulations. Moxifloxacin was estimated at 296 nm in 0.1N hydrochloric acid (pH 1.2) and at 289 nm in phosphate buffer (pH 7.4). Beer's law was obeyed in the concentration range of 1-12 microg ml(-1) (r2=0.9999) in hydrochloric acid and 1-14 microg ml(-1) (r2=0.9998) in the phosphate buffer medium. The apparent molar absorptivity and Sandell's sensitivity coefficient were found to be 4.63 x 10(4) l mol(-1) cm(-1) and 9.5 ng cm(-2)/0.001 A in hydrochloric acid; and 4.08 x 10(4) l mol(-1) cm(-1) and 10.8 ng cm(-2)/0.001 A in phosphate buffer media, respectively indicating the high sensitivity of the proposed methods. These methods were tested and validated for various parameters according to ICH guidelines. The detection and quantitation limits were found to be 0.0402, 0.1217 microg ml(-1) in hydrochloric acid and 0.0384, 0.1163 microg ml(-1) in phosphate buffer medium, respectively. The proposed methods were successfully applied for the determination of moxifloxacin in pharmaceutical formulations (tablets, i.v. infusions, eye drops and polymeric nanoparticles). The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation <2%), while being simple, cheap and less time consuming and hence can be suitably applied for the estimation of moxifloxacin in different dosage forms and dissolution studies.  相似文献   

20.
A new, simple, precise, rapid, and selective high-performance thin-layer chromatographic (HPTLC) method is developed for the simultaneous analysis of amlodipine and benazepril in pharmaceutical formulations. The method uses zolpidem as an internal standard (IS). The stationary phase used is silica gel 60 F254 prewashed with methanol. The mobile phase consists of an ethyl acetate-methanol-ammonia solution (8.5:2.0:1.0, v/v/v). Detection and quantitation are performed densitometrically at lambda = 254 nm. The Rf values of amlodipine, benazepril, and zolpidem (IS) are 0.58, 0.50, and 0.78, respectively. The limits of detection of amlodipine and benazepril are 0.02 and 0.2 microg; linearity ranges are 0.1-0.8 and 0.2-2.0 microg; and the percentage recoveries are 99.79% and 100.25%, respectively.  相似文献   

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