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1.
A simple, selective, rapid, precise and accurate reverse phase high pressure liquid chromatographic method has been developed for the simultaneous estimation of diclofenac sodium and rabeprazole sodium from pharmaceutical formulations. The method was developed using a HiQ SiL C18 (250 mm × 4.6 mm i.d.) column with a mobile phase consisting of methanol:water, (80:20 v/v), at a flow rate of 1.25 mL min−1. Detection was carried out at 284 nm. Indapamide was used as an internal standard. The developed method was validated for linearity, accuracy, precision, limit of detection and limit of quantitation. The proposed method can be used for the estimation of these drugs in combined dosage forms. 相似文献
2.
A liquid chromatographic method for the simultaneous determination of dextromethorphan hydrobromide, pyrilamine maleate and sodium benzoate in cough cold syrup has been developed. The method was based on replacing heptane sulfonate by sodium chloride as ion pairing agent. The addition of sodium chloride to the mobile phase has changed the retention behaviour of the basic drugs. The separation of these compounds was achieved in less than 8 min with an isocratic mobile phase consisting of acetonitrile/0.1 M dihydrogenphosphate buffer containing 0.1 M sodium chloride (29:71 v/v) at pH 2.5 and using a Kromasil C18 column. The analysis was performed at a flow rate of 1 mL min ?1 and at a detection wavelength of 220 nm. The selectivity, linearity of calibration, accuracy, within and between days precision, limit of detection and quantification, recovery were examined as parts of the method validation. Calibration curves were linear in the range 1–140 μg mL ?1 with a regression coefficient ( R 2) better than 0.999. The results of the method repeatability (intra-day) and reproducibility (inter-day) were all less than 2% ( n = 6). The lowest detectable concentration of dextromethorphan hydrobromide and pyrilamine maleate varied between 0.10 and 0.12 μg mL ?1. The proposed liquid chromatographic method was satisfactorily applied for the routine quality control of dextromethorphan hydrobromide, pyrilamine maleate and sodium benzoate in cough cold syrup formulations. 相似文献
3.
A new and accurate chiral liquid chromatographic method has been developed for determination of the enantiomeric purity of montelukast sodium ( R enantiomer) in bulk drugs and dosage forms. Normal phase chromatographic separation was performed on an immobilized amylose-based chiral stationary phase with n-hexane–ethanol–1,4-dioxane–trifluoroacetic acid–diethylamine 65:25:10:0.3:0.05 ( v/v) as mobile phase at a flow rate of 1.0 mL min ?1. The elution time was approximately 15 min. The resolution ( R S) between the enantiomers was >3. The mobile phase additives trifluoroacetic acid and diethylamine played a key role in achieving chromatographic resolution between the enantiomers and also in enhancing chromatographic efficiency. Limits of detection and quantification for the S enantiomer were 0.07 and 0.2 μg, respectively, for a test concentration of montelukast sodium of 1,000 μg mL ?1 and 10 μL injection volume. The linearity of the method for the S enantiomer was excellent ( R 2 > 0.999) over the range from the LOQ to 0.3%. Recovery of the S enantiomer from bulk drug samples and dosage forms ranged from 97.0 to 103.0%, indicative of the high accuracy of the method. Robustness studies were also conducted. The sample solution stability of montelukast sodium was determined and the compound was found to be stable for a study period of 48 h. 相似文献
4.
A simple, sensitive, precise and accurate reversed phase liquid chromatographic method has been developed for the simultaneous estimation of atorvastatin (AT) calcium, ramipril (RA) and aspirin (AS) from capsule dosage form. The method was developed using a Phenomenex Luna C 18 (250 mm, 4.6 mm i.d., 5 µm) column with a mobile phase consisting of 0.1%, orthophosphoric acid buffer:acetonitrile:methanol (45:50:5 v/ v/ v), pH 3.3, at a flow rate of 1 mL min ?1. Detection was carried out with ultra-violet detection at 210 nm. The retention times were about 12.19, 2.35, and 3.95 min for AT calcium, RA and AS, respectively. The developed method was validated for linearity, accuracy, precision, limit of detection, limit of quantitation and robustness. The linearity ranges were 1–6 µg mL ?1 for AT calcium, 0.5–3 µg mL ?1 for RA and 7.5–45 µg mL ?1 for AS with mean recoveries of 100.59 ± 0.68, 100.62 ± 0.83 and 100.49 ± 0.73% for AT calcium, RA and AS, respectively. Limit of detection obtained were 29.85 ng mL ?1 for AT calcium, 4.71 ng mL ?1 for RA and 85.13 ng mL ?1 for AS. Impurity of salicylic acid was found in capsule dosage form at the retention time of about 4.84 min. The proposed method can be used for the estimation of these drugs in combined dosage forms. 相似文献
5.
A new stability-indicating reversed-phase LC method has been developed and validated for the assay and identification of betamethasone dipropionate and its related compounds in a dermatological pharmaceutical drug product, namely Diprolene Ointment. Separation of all the peaks of interest was achieved on a Symmetry Shield RP18 (100 mm × 4.6 mm, 3.5 µm) column using a gradient elution at a flow rate of 1.5 mL min ?1 with mobile phase A (10 mM monobasic sodium phosphate at pH 2.5) and mobile phase B (acetonitrile) and UV detection at 250 nm. The limit of detection (LOD) and limit of quantitation (LOQ) of this method was 0.00004 and 0.0001 mg mL ?1, respectively. The method was successfully validated in accordance with ICH guidelines and was accurate, linear, precise, reproducible, specific, and robust. A simple, reproducible and accurate single step sample extraction procedure using tetrahydrofuran, water, and methanol (40:30:30, v/ v/ v) was developed to extract betamethasone dipropionate and its related compounds from the ointment. The sample extraction procedure and the LC conditions presented in this report can be used for routine analysis of Diprolene Ointment in quality control laboratories. This method may also be applied to other dermatological pharmaceutical drug products “as-is” or with minor modification. 相似文献
6.
Spectrophotometric and LC methods have been developed and validated for the analysis of alendronate sodium in tablet dosage forms. Methods were based on reaction of the primary amino group of alendronate with ninhydrin reagent in methanolic solution of sodium bicarbonate. The condensed product exhibited UV absorption maximum at 569 nm whereas neither the reagents nor the analyte had any UV absorption. A Box-Behnken statistical design was employed to study the effect of independent variables, ninhydrin ( X 1 ), NaHCO 3 ( X 2 ) and drug concentration ( X 3 ) on dependent variable, absorption via spectrophotometer. From the point prediction tool of design software, it was observed that ninhydrin (0.26%) and NaHCO 3 (0.048 mol L ?1) produced maximum absorption. These optimized parameters were then selected for method validation. The methods obeyed Beer’s law over a selected concentration range with good correlation co-efficient (>0.99). The limit of detection and limit of quantification were 4.5 and 13.75 μg mL ?1 by spectroscopy, and 87 and 263 ng mL ?1 by LC, respectively. Accuracy, precision and % recovery were satisfactory for the proposed method. The method was highly feasible and reproducible for determination of alendronate sodium in bulk powder and pharmaceutical dosage form. 相似文献
7.
Abstract A reliable and sensitive RP-HPLC method was developed and validated for the quantitative estimation of ceftriaxone sodium (CFTZ) in pure drug and pharmaceutical dosage forms. The separation of ceftriaxone sodium was achieved on a Waters XTerra RP-18 (5 µm, 250 × 4.6 mm i.d.) column using photodiode array detector at 240 nm. The mobile phase consisted of 0.1 M triethylammoniumacetate–acetonitrile (60:40 v/v) mixture delivered at a flow rate of 1.0 ml/min. Accuracy, evaluated by means of the spike recovery method, was excellent, with percent recovery in the range 99.5–102% with precision in the range 0.3–1.2%. 相似文献
8.
A simple, sensitive and specific liquid chromatographic method with UV detection (228 nm) was developed for the simultaneous estimation of rosiglitazone and glimepride in human plasma. Rosiglitazone and glimepride were extracted from plasma using liquid–liquid extraction. Separation was achieved with an RP C 18 Column using a mixture of phosphate buffer (50 mM) with octane sulfonic acid (10 mM), methanol and acetonitrile as a mobile phase (55:10:35, v/v). pH was adjusted to 7.0. Amlodipine was used as an internal standard (IS). LOD of the method was found to be 20 ng mL ?1 for both drugs. Results were linear over the studied range 40.994–2007.556 ng mL ?1 for rosiglitazone ( r 2 ≥ 0.99) and 41.066–2094.84 ng mL ?1 for glimepride( r 2 ≥ 0.99). The method was found to be simple, selective, precise and reproducible for the estimation of both drugs from spiked human plasma. 相似文献
9.
An accurate, simple, and sensitive reversed-phase high-performance liquid chromatographic method, with loratadine as internal standard (IS) and UV detection at 286 nm, has been developed for deterination of cystine in human urine. The major innovations of the method include use of acrylonitrile to protect cysteine from oxidization to cystine, separation of cysteine, as the dansyl derivative, from cystine, and use of isocratic elution instead of gradient elution to reduce the time and cost of serial analysis. The mobile phase was 0.05 M sodium acetate–methanol, 35:65 ( v/ v), adjusted to pH 3.5 with 2.5 M citric acid, at a flow rate of 1.0 mL min ?1. The retention times of cystine and the IS were 16.6 and 19.9 min, respectively. The limit of detection for cystine was 0.3 mg L ?1. Extraction recovery of cystine was >85.6%. Intra-day and inter-day precision (RSD) for cystine were below 4.3 and 8.5%, respectively. There was no chromatographic interference from other α-amino acids present in mammalian proteins, or from other urine components. The calibration plot for the cystine derivative was linear in the range 1–500 mg L ?1 and the correlation coefficient was 0.9992. The method was validated appropriately and successfully used for determination of cystine in human urine. 相似文献
10.
We present a simple and reliable method for simultaneous determination of voriconazole and its main metabolite resulting from N-oxidation (UK-121,265), in human plasma. The work-up procedure used acetonitrile and potassium salts to precipitate plasma proteins. No internal standard was used. The chromatographic system used a LiChroCART ® 250-4 cartridge packed with LiChrospher ® 100 RP-8 (diameter particules, 5 μm). The UV monochromatic detector was set on 260 nm. The mobile phase consisted of a 60/40 ( v/ v) mixture of acetonitrile and water. The flow rate was 1 mL min ?1. The retention times for voriconazole and its metabolite were 8.98 and 4.02 min respectively, and total run time was 12 min. The linearity of the method was investigated from 0.31 to 10.0 mg L ?1; the lowest limit of quantification was 0.30 mg L ?1. Precision ranged from 2.41% to 6.32% for voriconazole and 0.80% to 11.6% for the N-oxide voriconazole metabolite. Accuracy was between 93.0% and 101% for voriconazole and 90.0% and 101% for the N-oxide voriconazole metabolite. This rapid and accurate method could be interesting to investigate metabolite/voriconazole ratio with respect to CYP2C19 genetic status and CYP3A4 activity changes. 相似文献
11.
A new and accurate chiral liquid chromatographic method has been developed for the determination of enantiomeric purity of darifenacin [( S)-enantiomer] in bulk drugs and extended release tablets. Normal phase chromatographic separation was performed on an immobilized cellulose based chiral stationary phase (Chiralpak-IC) with n-hexane:ethanol:diethylamine (50:50:0.3, v/v/v) as mobile phase at a flow rate of 1.0 mL min ?1. The elution time was ~15 min. The resolution ( R s ) between the enantiomers was greater than four and interestingly the ( R)-enantiomer was eluted prior to darifenacin in the developed method. The limit of detection (LOD) and limit of quantification (LOQ) for the ( R)-enantiomer were 0.02 μg and 0.07 μg, respectively, for a 10 μL injection volume. The method was extensively validated in terms of linearity, precision and accuracy and satisfactory results were obtained. Robustness studies were also conducted. The sample solution stability of darifenacin was determined and the compound was found to be stable for a study period of 48 h. 相似文献
12.
A simple, selective and sensitive HPLC–UV method for quantification of propranolol hydrochloride and sodium benzoate in oral liquid preparations was developed and fully validated. Separation was performed by Supelco Discovery® C18 (25 cm × 4.6 mm, particles 5 μm) column. UV/VIS absorbance detector was set at wavelength 230 nm. Column oven was conditioned to 25 °C. Mobile phase was prepared by dissolving 1.6 g of sodium dodecyl sulphate and 0.31 g of tetrabutylammonium dihydrogen phosphate in 450 mL of ultrapure water; 1 mL of sulphuric acid (95–97 %) and 550 mL of acetonitrile were added. Sodium hydroxide solution (2.1 M) was used for adjusting pH to value 3.3 (±0.05). Retention times of sodium benzoate, propranolol hydrochloride and butylparaben (internal standard) were 2.2, 3.3 and 4.1 min, respectively. Newly developed method is suitable for simultaneous determination of propranolol hydrochloride and sodium benzoate in oral liquid preparations which are used for therapy of haemangiomas in paediatric patients. Method has been applied for stability testing of extemporaneous paediatric oral formulations containing propranolol hydrochloride. 相似文献
13.
A simple, rapid and sensitive reverse phase liquid chromatography-diode array detector method has been developed and validated for the determination of isoliquiritigenin in rat plasma using acetanilide as an internal standard. The plasma was deproteinized with acetonitrile and separated from the aqueous layer by adding sodium chloride. The mobile phase was acetonitrile, 0.05 M potassium dihydrogen phosphate and triethylamine (50:50:0.5, v/v/v) (pH 2.00). Detection wavelength was set at 242 nm during 0–5 min and 362 nm during 5–9 min. The limit of quantification was 0.019 μg mL ?1. The mean accuracy was 96.851–98.140%. Extract recoveries at concentration of 0.038, 0.625, 1.250, 5.000 and 20.000 μg mL ?1 were 82.740, 80.814, 80.920, 80.978 and 81.103%, respectively. The validated method was successfully applied to the pharmacokinetic study of ISL in rat plasma after intravenous administration. 相似文献
14.
A new, simple, rapid, sensitive and specific isocratic RP–LC–UV method was developed and validated for the determination of ondansetron in pharmaceutical dosage forms of orally disintegrating tablets, oral solution and injection. The LC separation was achieved on a Hypersil C4 column (250 × 4.6 mm, 5 μm) using a mobile phase of 50 mM potassium dihydrogen phosphate anhydrous adjusted to pH 3.5 with orthophosphoric acid and acetonitrile (30:70, v/v) at a flow rate of 1.0 mL min ?1 and UV detection at 310 nm. The method was validated for specificity, linearity, precision, accuracy, limit of quantification, limit of detection, robustness and solution stability. The calibration curve was linear over a concentration range of 100–1,000 ng mL ?1 ( r 2 = 0.9996) with limit of detection and limit of quantification 50 and 100 ng mL ?1, respectively. The intra-day and inter-day precision and accuracy were between 0.79 and 2.37% and ?0.64 and 1.65%, respectively. The method was successfully applied for analysis of ondansetron in the presence of excipients in commercially available pharmaceutical dosage forms. 相似文献
15.
A stability-indicating LC method was developed for the simultaneous determination of ibuprofen and diphenhydramine citrate in pharmaceutical dosage forms. The chromatographic separation was achieved on an Inertsil ODS 3V, 150 × 4.6 mm, 5 μm, column. The mobile phase contained a mixture of 50 mM potassium dihydrogen phosphate buffer:acetonitrile:triethylamine:glacial acetic acid (55:45:0.2:0.2, v/ v/ v/ v) . This method allowed the determination of 2.85–9.14 mg mL ?1 of ibuprofen and 0.54–1.73 mg mL ?1 of diphenhydramine citrate, in a diluent consisting of pH 7.2, 50 mM potassium dihydrogen phosphate buffer:acetonitrile (40:60, v/ v). The flow rate was 1.2 mL min ?1 and the detection wavelength was 260 nm. The limit of detection for ibuprofen and diphenhydramine citrate was 1.72 and 0.54 μg mL ?1 and the limit of quantification was 5.73 and 1.64 μg mL ?1, respectively. This method was validated for accuracy, precision and linearity. The method was also found to be stability indicating. 相似文献
16.
A sensitive and specific liquid chromatography–electrospray ionization–tandem mass spectrometry method has been developed and validated for the quantification of huperzine A in human plasma. After the addition of trimetazidine, the internal standard (IS) and sodium hydroxide, plasma samples were extracted using 5 mL ethyl acetate. The compounds were separated on an Agilent Zorbax SB C 18 column (100 mm × 2.1 mm ID, dp 3.5 μm) using an elution system of 10 mM ammonium acetate solution–methanol–formic acid (18:82:0.1, v/ v) as the mobile phase. The quantification of target compounds was obtained by using multiple reaction monitoring (MRM) transitions: m/ z 243.1, 210.1 and 267.2, 166.0 were measured in positive mode for huperzine A and IS. Linearity was established for the range of concentrations 0.01–4.0 ng mL ?1 with a coefficient of correlation ( r) of 0.9991. The lower limit of quantification (LLOQ) was identifiable and reproducible at 0.01 ng mL ?1. The method has been successfully applied to study the pharmacokinetics of huperzine A in healthy male Chinese volunteers. 相似文献
17.
A simple, sensitive, selective, rapid, rugged, reproducible and specific liquid chromatography?Ctandem mass spectrometry (LC?CMS/MS) method was used for quantitative estimation of rizatriptan (RZ) in human plasma using rizatriptan- d 6 (RZD6) as internal standard (IS). Chromatographic separation was performed on Ascentis Express RP Amide C18, 50 × 4.6 mm, 2.7 ??m column with isocratic mobile phase composed of 10 mM ammonium formate:acetonitrile (20:80 v/v) at flow rate of 0.5 mL min ?1. RZ and RZD6 were detected with proton adducts at m/ z (amu) 270.2 ?? 201.2 and 276.1 ?? 207.1, respectively, in multiple reaction monitoring (MRM) positive mode. Liquid?Cliquid extraction was used and validated over a linear concentration range of 0.1?C100.0 ng mL ?1 with correlation coefficient r 2 ?? 0.9981. The limit of quantification (LOQ) and limit of detection (LOD) were found to be 0.1 ng mL ?1 and 12.5 fg, respectively. Intra- and inter-day precision were within 1.7?C3.1% and 2.8?C3.7%, and accuracy within 96.0?C101.7% and 99.7?C101.4% for RZ. Drug was found to be stable throughout three freeze?Cthaw cycles. The method was successfully employed for analysis of plasma samples following oral administration of RZ (10 mg) in 25 healthy Indian male human volunteers under fasting conditions. 相似文献
18.
A rapid, selective and sensitive reversed-phase liquid chromatographic (LC) method was developed for the determination of piribedil in human serum, urine and pharmaceutical dosage form. LC analysis was carried out using reversed-phase isocratic elution with a C 18 column and a mobile phase of 0.01 M phosphate buffer-acetonitrile (50:50, v/ v). The chromatograms showed good resolution and sensitivity with no interference of human serum and urine. Piribedil concentrations were determined using diode array detection at 240 nm. Sildenafil citrate was used as internal standard. The limit of quantification (LOQ) and limit of detection (LOD) concentrations were 107.2 and 321.6 pg mL ?1, 96.6 and 290.4 pg mL ?1, 161.7 and 53.9 pg mL ?1 for urine, serum and pharmaceutical dosage forms, respectively. The method was validated for its linearity, precision and accuracy and applied to the tablets, urine and human serum. In addition, the results were compared to those obtained from UV-spectrophotometry. 相似文献
19.
A simple, rapid, specific and sensitive thin layer chromatographic (TLC) method has been developed for the quantitative estimation of mevalonic acid (MVA) in leaves of medicinal plants; Artemisia annua, Psorelia corylifolia, Vinca rosea, Withania somnifera and Barleria proinites. The assay procedure involved conversion of MVA to its lactone, mevalonolactone (MVAL). Mevalonic acid was extracted from the leaf tissues of plants. Separation of MVAL was carried out on silica gel 60 F 254 TLC plates using benzene:acetone (3:2) as the mobile phase. The densitometric determination of MVAL was performed at 600 nm after derivatization with anisaldehyde reagent in absorption–reflectance mode. The method was validated over the linearity range of 100–500 ng spot ?1 and correlation coefficient for the calibration curve was >0.99. The average recovery of MVAL, used as internal standard, was higher than 98%. The lower limit of detection was found to be 50 ng spot ?1. 相似文献
20.
An accurate LC method was developed and validated for simultaneous determination of irinotecan (CPT-11) and its active metabolite SN-38 in rat plasma. Plasma samples were pretreated with 0.4 g mL ?1 sodium dodecyl sulfate to inactive the carboxylesterase and avoid the conversion of CPT-11 to SN-38. Chromatographic separation was achieved on a Diamaonsil C 18 column using acetonitrile–50 mM phosphate buffered solution (30:70, v/v) at pH 4.0 as the mobile phase with the flow rate of 1 mL min ?1. The linear quantitation ranges for CPT-11 and SN-38 were 5.05–3,030 and 3.15–315 ng mL ?1 with r 2 > 0.99, respectively. The lower limit of quantification (LLOQ) was 2.33 ng mL ?1 for CPT-11 and 0.26 ng mL ?1 for SN-38 with intra- and inter-day relative standard deviation of <12% and the accuracy values of >90%. The method was proved to be accurate and sensitive enough and was successfully applied to a pharmacokinetic study of CPT-11 in rats. 相似文献
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