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1.
A liquid chromatographic (LC) method for the determination of colchicine in pharmaceutical dosage forms and the bulk drug was evaluated in an interlaboratory study which included 13 participating laboratories. The method involves extraction (or dissolution) of the active ingredient with methanol-water (1 + 1), followed by filtration of the extract and reverse phase LC using an octylsilane bonded phase column and UV detection at 254 nm. The mobile phase consists of a methanol-phosphate buffer mixture (pH = 5.5). Three commercial tablet formulations (0.5-0.6 mg colchicine/tablet), 1 synthetic injectable preparation (0.510 mg colchicine/mL), and 1 bulk drug sample were assayed in duplicate by the proposed method. The reproducibility and repeatability standard deviations based on nonpooled results for each sample ranged from 0.0062 mg/mL to 0.0147 mg/tablet and from 0.0037 mg/mL to 0.0127 mg/tablet, respectively; the corresponding coefficients of variation ranged from 1.21 to 2.54% and from 0.73 to 2.19%, respectively. The mean recovery from the synthetic injectable formulation was 100.0%. The method has been adopted official first action.  相似文献   

2.
Reserpine-rescinnamine group alkaloids are extracted from Rauwolfia serpentina preparations into a dimethylsulfoxide (DMSO)-methanol mixture and diluted with 0.5N H2SO4. The chloroform extract of this solution is passed through a 0.1N NaOH-Celite column and then through a silica gel column. The weakly basic alkaloids trapped on the latter column are eluted with a methanol mixture; a portion of the eluate is treated with nitrous acid and the reserpine-rescinnamine content is determined by measuring the intensity of fluorescence of the oxidation product. The following means and standard deviations (11 collaborators) were obtained for the determination of reserpine-rescinnamine group alkaloids in 4 samples of Rauwolfia serpentina (NF reference powder, 100 mg and 50 mg commercial tablets, and a 45 mg synthetic tablet formulation) : 0.174% +/- 0.0112, 0.131% +/- 0.0047, 0.160% +/- 0.0100, and 0.153% +/- 0.0083, respectively.  相似文献   

3.
A liquid chromatographic (LC) method for the determination of pentaerythritol tetranitrate (PETN) in pharmaceutical formulations and the bulk drug triturate was evaluated in an interlaboratory study that included 12 participating laboratories. The procedure involves extraction of the active ingredient with mobile phase, followed by filtration of the extract and reverse-phase liquid chromatography using an octadecylsiliane bonded phase column and UV detection at 230 nm. The mobile phase composition is 35% water in acetonitrile (v/v). Three bulk drug samples (20, 20, and 35% PETN), 2 commercial tablet formulations (20 and 80 mg PETN/tablet), and 1 commercial capsule formulation (45 mg PETN/capsule) were analyzed in duplicate by the proposed method. Repeatability (sr, RSDr) and reproducibility (SR, RSDR) based on peak height measurement for these samples ranged from 0.0066 to 0.1806 (0.53-3.36%) and 0.0165 to 0.2075 (0.76-3.86%), respectively. Results for peak area measurements ranged from 0.0145 to 0.2011 (0.93-3.74%) and 0.0231 to 0.2091 (1.28-3.89%), respectively. The method has been approved interim official first action by AOAC.  相似文献   

4.
A normal phase liquid chromatographic (LC) method for the determination of prednisolone in tablets and bulk drugs was studied by 7 analysts. An LC system, consisting of a methanol-water-ethylene dichloride-acetic acid mobile phase and a silica column, was used to analyze bulk drugs, individual tablets, and composite samples. Analysts were supplied with 16 samples, including simulated formulations, composites of commercial tablets, intact tablets, and bulk drug substances. Results agreed with those obtained by the author. The coefficients of variation of the analysts' results ranged from 1.34% for bulk drugs to 2.14% for tablet composites. The LC method is suggested as an alternative to the official AOAC and USP XX blue tetrazolium colorimetric methods.  相似文献   

5.
A nuclear magnetic resonance (NMR) procedure is described for the quantitative analysis of chlorpromazine. HCl in bulk chemical as well as in final dosage forms--tablets, spansules, and injectables. The method is based on measurement of a characteristic signal of chlorpromazine relative to an internal standard. Three different internal standards are specified: Cyclohexane was selected because of the convenience and rapidity with which samples could be prepared for assay. Piperonal was used to verify the method and to show that precision and accuracy were not affected by the volatility of the cyclohexane. Tetramethylammonium bromide was used as an internal standard for Thorazine injectable. No interferences were found from stearates and other tablet excipients. The NMR procedure provides a simple, direct, and specific assay with a precision of +/- 1-2%.  相似文献   

6.
A stability-indicating liquid chromatographic method is presented for determining sulfamethoxazole in tablets. The method uses a 10 micron silica column, an isooctane-methylene chloride-2-propanol-acetonitrile-glacial acetic acid (70 + 25 + 5 + 5 + 0.5) mobile phase, and photometric detection at 254 nm. Seven laboratories collaboratively studied this method on powdered composite samples prepared from commercial 500 and 1000 mg tablets and on an authentic tablet mixture containing 83.32% added sulfamethoxazole. Mean assay results for the 500 and 1000 mg tablets were 102.2 and 97.9% of declared, respectively (n = 4). The mean recovery value for the synthetic sample was 99.4% (n = 4). The pooled reproducibility standard deviation (SD) (coefficient of variation (CV)) and pooled repeatability SD (CV) were +/- 1.01 (1.01%) and +/- 0.96 (0.96%), respectively. These results were in good agreement with those obtained by the Associate Referee for the titration method of USP XX. The proposed method can also be used for monitoring the presence of sulfanilamide in sulfamethoxazole by increasing the proportions of both acetonitrile and 2-propanol in the mobile phase. The method has been adopted official first action.  相似文献   

7.
A UV spectrophotometric method for the determination of hydralazine hydrochloride in tablets was collaboratively studied by 5 laboratories. The method is based on conversion of hydralazine to a tetrazolo [5,1-alpha]phthalazine derivative which shows an absorption maximum at about 274 nm. Each collaborator received blind duplicate samples of 2 commercial powdered composites from 10 and 100 mg tablets, and 1 synthetic tablet formulation. Each collaborator also received a set of 10 tablets for determination of content uniformity. The pooled mean recovery of hydralazine hydrochloride from the synthetic formulation was 101.2 +/- 0.94%. The mean assay values for 10 and 100 mg tablets were 95.6 +/- 0.98 and 101.0 +/- 0.73% of the declared amounts, respectively, with corresponding CV values of 1.02 and 0.73%. The pooled mean for individual tablet assay was 99.8 +/- 3.26% of the declared value, with a CV of 3.29%. The method has been adopted official first action.  相似文献   

8.
A liquid chromatographic method has been developed that determines the amount of sulfasalazine in tablets and bulk powder in the presence of residual synthesis by-products and excipients. The method was tested on crude product containing large amounts of impurities. A C-18 reverse phase column with water-acetonitrile-acetic acid mobile phase was found to effectively separate the drug on the column. Six different commercial samples of 500 mg tablets were assayed. The results varied from 92.6 to 101.8% of the declared amount. Spectrophotometric determinations, which do not discriminate between the drug and impurities, gave 95.4-101.8% of declared. One commercial sample of bulk powder was assayed.  相似文献   

9.
A simple gas chromatographic method is described for the determination of histapyrrodine HCl in marketed formulations. Chlorpheniramine maleate is used as the internal standard. The amount of histapyrrodine HCl found by the proposed method averaged 19.91 mg/tablet, compared with the label claim of 20 mg/tablet. The method was statistically evaluated for accuracy and precision.  相似文献   

10.
A liquid chromatographic method for the determination of coumarin anticoagulants in tablets was collaboratively studied by 7 laboratories. The method uses an octadecylsilane-bonded microparticulate column, tetrahydrofuran-methanol-water-acetic acid mobile phase, and photometric detection at 311 nm. Each collaborator received samples of warfarin sodium, phenprocoumon, and dicumarol as a synthetic composite and as commercial individual and composited tablets. Pooled average assay values for synthetic and commercial tablet samples of warfarin sodium were 101.6 and 99.5%, respectively, with a combined reproducibility SD of 2.38% (CV = 2.37%) and combined repeatability SD of 1.49% (CV = 1.49%). Pooled average (SD) assay values for dicumarol and phenprocoumon commercial samples were 98.0 (2.27) and 101.3% (4.00), respectively. The content uniformity determinations of 2 mg warfarin sodium and 25 mg dicumarol tablets indicated average tablet contents (range) of 99.5% (91.0-116.0) and 98.0% (89.8-108.8), respectively. The method has been approved interim official first action.  相似文献   

11.
A rapid, accurate method for separating and determining the enantiomeric composition of amphetamine bulk drug and commercial preparations was developed and subjected to collaborative study. Amide derivatives of the amphetamine enantiomers are formed by using achiral 2-naphthoyl chloride. The resulting enantiomeric amides are then chromatographed on a commercially available chiral stationary phase with hexane-isopropyl alcohol-acetonitrile (97 + 3 + 0.5) mobile phase, with detection at 254 nm. Seven collaborators received bulk drug and commercial samples of amphetamine. The collaborators and authors determined the mean percent l- and d-amphetamine from 2 injections of each sample. The method can detect the presence of as little as 0.5% of the l-enantiomer in d-amphetamine, with reproducibility between laboratories of +/- 71.3%. The method has been adopted official first action for determination of the enantiomeric composition of amphetamine bulk drug and preparations.  相似文献   

12.
A liquid chromatographic method for the determination of penicillin V potassium in tablets was collaboratively studied by 7 laboratories. The method uses an octadecyl silane reverse-phase column, a mobile phase of acetonitrile-methanol-0.01 M potassium phosphate monobasic (21 + 4 + 75 v/v/v), photometric detection at 225 nm, and sulfadimethoxine as an internal standard. Each collaborator received 6 samples: powdered composites of 2 commercial tablet preparations and 1 synthetic tablet powder mixture, each with blind duplicates. The mean repeatability and reproducibility relative standard deviations for commercial samples were, respectively, 1.10 and 1.46% (250 mg dosage), and 0.84 and 2.82% (500 mg dosage). The average standard recovery from the synthetic formulation was 99.1%, with repeatability and reproducibility relative standard deviations of 1.30 and 3.66%, respectively. The method has been adopted official first action.  相似文献   

13.
A normal phase liquid chromatographic method for the determination of dexamethasone in bulk drugs and elixirs was collaboratively studied by 6 laboratories. The method uses a silica column, water-modified acetic acid-methanol-methylene chloride mobile phase, cortisone internal standard, and photometric detection at 254 nm. Collaborators were supplied blind duplicate samples of 3 bulk drugs, 2 commercial elixirs, and 1 authentic elixir. Dexamethasone elixir dosage level is 0.5 mg/5 mL. Mean recovery of dexamethasone from the authentic elixir formulated to contain 0.471 mg/5 mL was 94.5%. (Authentic elixirs were found to stabilize about 6% below the theoretical concentration.) Mean recovery for the bulk drugs was between 97.1 and 100.1%. Mean coefficients of variation for bulk drug and elixir samples were less than 0.8% and 3.6%, respectively. Identification tests for dexamethasone by thin-layer chromatography, infrared spectroscopy, and relative LC retention times, as well as the gas chromatographic determination of alcohol in the elixirs were also collaboratively studied. Mean recovery of alcohol from the synthetic elixir was 98.6%. The mean coefficient of variation for alcohol for all samples analyzed was less than 1.4%. The LC method for dexamethasone in drug substance and elixirs, the identification tests, and the GC method for alcohol in dexamethasone elixirs have been adopted official first action.  相似文献   

14.
A reverse phase liquid chromatographic method previously reported for the determination of acetaminophen in tablets was collaboratively studied by 5 laboratories. Each collaborator received duplicate samples of a synthetic tablet formulation and 3 powdered commercial tablet composites. The composites represented single-component and multi-component proprietary products and a single-component generic product. The pooled repeatability (CVDo) and reproducibility (CVDx) values for the proprietary tablets were 0.89 and 1.34%, respectively. For the generic tablets, these values were 0.66 and 0.74%, respectively. The pooled recovery value for acetaminophen added to the synthetic formulation was 98.9 +/- 0.7% (n = 10) with a CV of 0.75%, CVDo of 0.37%, and CVDx of 0.78%. The overall repeatability of the method was 0.64%, and the overall reproducibility was 0.95%. The method has been adopted official first action.  相似文献   

15.
Based on the structural differences between quinidine and dihydroquinidine, a 1H-nuclear magnetic resonance spectroscopic method previously reported for quinidine drug substance was modified and shown to be applicable to the quantitative determination of both compounds in quinidine sulfate tablets. Deuterated chloroform was used as the solvent and hexamethylcyclotrisiloxane served as an internal standard. The average recovery and standard deviation of quinidine sulfate (calculated as the sum of quinidine sulfate plus dihydroquinidine sulfate) from synthetic formulations was 98.94 +/- 0.43% (n = 10). Five lots of 200 mg tablets of quinidine sulfate from one commercial source were found to contain from 92.9 to 95.8% quinidine sulfate, and from 1.1 to 7.0% dihydroquinidine sulfate.  相似文献   

16.
A liquid chromatographic method for the determination of flucytosine in capsules was collaboratively studied by 7 laboratories. The method uses a C18 reverse phase column, water-methanol-acetic acid mobile phase containing 1-octanesulfonic acid sodium salt, p-aminobenzoic acid as internal standard, and photometric detection at 285 nm. The mean recovery value (+/- SD) of flucytosine from a synthetic formulation representing capsules was 99.2 +/- 1.72% (CV = 1.73%). Composited samples of 250 and 500 mg commercial capsules gave assay values of (mean +/- SD) 103.17 +/- 2.21 and 99.29 +/- 1.29% of declared, respectively. CV values were 2.15 and 1.30%. Reproducibility and repeatability CVs were 2.19 and 1.50%, respectively, for the 250 mg capsules, and 1.34 and 0.63%, respectively, for the 500 mg capsules. The method has been adopted official first action.  相似文献   

17.
Tiaprofenic acid (Surgam) has been determined directly by using differential pulse polarography (DPP) and pH 5.5 acetate buffer as a supporting electrolyte. The differential pulse polarogram was obtained under constant amplitude pulses of 50 mV superimposed on a linearly increasing dc ramp. Peak current was measured at the peak potential of -0.990 V vs Ag/AgCl reference electrode. Under the experimental conditions used, a linear relationship between peak current and concentration was established over the range 0.5-5.0 micrograms/mL. Mean percentage recoveries for tiaprofenic acid in authentic and tablet forms were 100.27 +/- 2.25 and 99.45 +/- 1.44, respectively. The results obtained by the DPP method were compared with those of the spectrophotometric method used by the manufacturer for the analysis of tiaprofenic acid and its tablet form.  相似文献   

18.
A liquid chromatography technique coupled with tandem mass spectrometry (LC-MS/MS) electrospray ionization was used to measure (-)-epigallocatechin-3-gallate (EGCG) in rat plasma. This method was applied to investigate the pharmacokinetics of EGCG in a conscious and freely moving rat by an automated blood sampling device. Multiple reaction monitoring (MRM) was used to monitor the transition of the deprotonated molecule m/z of 457 [M - H]- to the product ion 169 for EGCG and the m/z of 187 to 164 for the internal standard. The limit of quantification (LOQ) of EGCG in rat plasma was determined to be 5 ng/mL, and the linear range was 5-5000 ng/mL. The protein binding of EGCG in rat plasma was 92.4 +/- 2.5%. The brain distribution result indicated that EGCG may potentially penetrate through the blood-brain barrier at a lower rate. The disposition of EGCG in the rat blood was fitted well by the two-compartmental model after intravenous administration (10 mg/kg, iv). The elimination half-life of EGCG was 62 +/- 11 and 48 +/- 13 min for intravenous (10 mg/kg) and oral (100 mg/kg) administration, respectively. The pharmacokinetic data indicate that the oral bioavailability of EGCG in a conscious and freely moving rat was about 4.95%.  相似文献   

19.
A liquid chromatographic (LC) procedure is described for the assay of morphine sulfate in bulk drug material and injection solutions. The bulk drug and injection samples are prepared by direct dilution with LC mobile solvent. The average bulk drug purity (5 manufacturers) determined by the LC method was 99.9% with a difference of 0.1% from the average purity (anhydrous) found by the official USP XX procedure. The average LC recovery (19 studies) of morphine sulfate added to injection samples was 99.4% with a coefficient of variation (CV) of 1.14%. Morphine sulfate content was determined in triplicate for 53 injection samples (1-15 mg morphine sulfate/mL) formulated by 6 manufacturers, using the proposed LC procedure. Individual sample CV (n = 3) averaged 1.14%. The LC method is simple and specific for morphine sulfate. Major degradation products, preservatives, and some contaminants and related compounds are separated during LC.  相似文献   

20.
A reverse phase liquid chromatographic method was developed for determining methocarbamol in injection and tablet dosage forms. The injections require dilution only; the tablets require a filtration step before introduction into the chromatograph. Response for methocarbamol was linear over the range 0-18 micrograms, using an ultraviolet detector at 274 nm. Recoveries by the author ranged from 96.1 to 101.9% for authentic injection formulations and 98.0 to 101.0% for authentic tablet formulations. A collaborative study of the method by 6 laboratories resulted in standard deviations of 1.70 and 2.22 for injection and tablet dosage forms, respectively. The method has been adopted official first action.  相似文献   

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