Collaborative Study of the Spectrophotometric Determination of Procainamide Hydrochloride

1976 ◽  
Vol 59 (4) ◽  
pp. 807-810
Author(s):  
Jeffrey C Hamm

Abstract The USP analysis for procainamide HCl is titrimetric and relatively nonspecific, capsule and tablet dyes may interfere, and the method is not applicable to coated tablets. In the spectrophotofluorometric method the sample deteriorates when exposed to a xenon source. In the ultraviolet spectrophotometric method reported here, the sample is dispersed in acid medium, possible interferences are extracted in chloroform, base is added, procainamide is extracted in chloroform, the residue is dissolved in sodium hydroxide, and the compound is measured by absorption at 272 nm and comparison with a standard. Recoveries of standards added to capsule, tablet, and injection composites ranged from 99.3 to 102%. Twelve collaborators reported duplicate assay results for all 3 dosage forms with per cent standard deviations for 5 samples ranging from 1.01 to 1.27%. The method has been adopted as official first action.

1988 ◽  
Vol 71 (6) ◽  
pp. 1212-1214
Author(s):  
Anna-Maija K SJÖBERG

Abstract Fifteen official food control laboratories participated in a collaborative study of a spectrophotometric method to determine cyclamate in a soft drink and a dessert at concentrations of 90-311 mg/L and 202-526 mg/kg, respectively, with blind duplicates and a blank. Average recovery from the soft drink was 97.5%, and from the dessert, 98.6%. Reproducibility relative standard deviations were 4.7-6.5% and 6.9-8.5%, respectively. The outlier percentage was 5.5%. This study complements an earlier work by leading Nordic food laboratories and was designed according to the latest recommendations. The results of this study were compared with those of the earlier collaborative study and with general collaborative results obtained by AOAC.


1978 ◽  
Vol 61 (2) ◽  
pp. 296-298
Author(s):  
Mark A Litchman

Abstract The spectrophotometric method for pyrantel tartrate in swine feeds was collaboratively studied. Twenty-seven laboratories assayed feeds containing 0.0103, 0.0965, and 0.7902% pyrantel tartrate. Repeatability (σo) and reproducibility (ax) standard deviations were: σo = 0.00068%, σx = 0.00105% (10% of grand mean) for 0.0103% pyrantel tartrate level; σo = 0.0065%, σx = 0.0090% (10% of grand mean) for 0.0965% pyrantel tartrate level; and σo = 0.0415%, σx = 0.0743% (10% of grand mean) for 0.7902% pyrantel tartrate level. The mean theoretical recovery values for feeds containing 0.0103, 0.0965, and 0.7902% were 100, 97, and 96%, respectively. The method was adopted as official first action for feeds or concentrates containing 0.0106–0.8811% pyrantel tartrate.


2008 ◽  
Vol 27 (2) ◽  
pp. 149 ◽  
Author(s):  
Ivana Savić ◽  
Goran Nikolić ◽  
Vladimir Banković

Simple, accurate and reproducible UV-spectrophotometric method was developed and validated for the estimation of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. Phenylephrine hydrochloride was estimated at 291 nm in 1 mol⋅dm-3 sodium hydroxide (pH 13.5). Beer’s law was obeyed in the concentration range of 10–100 μg⋅cm−3 (r2 = 0.9990) in the sodium hydroxide medium. The apparent molar absorptivity was found to be 1.63×103 dm3⋅mol−1⋅cm−1. The method was tested and validated for various parameters according to the ICH (International Conference on Harmonization) guidelines. The detection and quantitation limits were found to be 0.892 and 2.969 μg⋅cm−3, respectively. The proposed method was successfully applied for the determination of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation < 1 %), while being simple, cheap and less time consuming, and hence can be suitably applied for the estimation of phenylephrine hydrochloride in different dosage forms.


1990 ◽  
Vol 73 (5) ◽  
pp. 721-723
Author(s):  
Robert D Parker

Abstract An atomic absorption spectrophotometric method for determination of polydimethylsiloxane (PDMS) residues In pineapple juice was collaboratively studied by 9 laboratories. PDMS residues are extracted from pineapple Juice with 4- methyl-2-pentanone and the extracted silicone Is measured by atomic absorption spectrophotometry using a nitrous oxide/ acetylene flame. Collaborators analyzed 5 samples Including 1 blind duplicate. Reproducibility relative standard deviations (RSDR) were 13.1% at 31 ppm, 6.9% at 18 ppm, 14.8% at 7.9 ppm, and 16.1 % at 4.9 ppm PDMS. The method has been approved Interim official first action by AOAC.


1987 ◽  
Vol 70 (3) ◽  
pp. 588-590
Author(s):  
Anna-Maija K Sjoberg ◽  
Timo A Alanko

Abstract A spectrophotometric method for the determination of cyclamate was collaboratively studied in 9 laboratories. Ethyl acetate is added to extract cyclamate from acidic aqueous solution into water, and the cyclamate is then quantitatively converted to /V,./V-dichlorocyclohexylamine by adding excess hypochlorite. A',A'-Dichlorocyclohexylamine is determined by measuring its UV absorption at 314 nm. Six samples, 3 soft drinks with cyclamate levels of 0.36-0.47 g/kg and 3 jams with levels of 1.23-1.50 g/kg, were included in the study. Average recoveries of cyclamate were 99.7% in the soft drinks and 103.8% in the jams. Reproducibility coefficients of variation were 6.7% for the soft drinks and 4.4% for the jams.


2018 ◽  
Vol 33 (2) ◽  
pp. 41
Author(s):  
Chand Pasha ◽  
Badiadka Narayana

A simple spectrophotometric method for the determination of cefotaxime, ceftriaxone, cefadroxil and cephalexin with variamine blue is presented. The determination is based on the hydrolysis of β-lactam ring of cephalosporins with sodium hydroxide which subsequently reacts with iodate to liberate iodine in acidic medium. The liberated iodine oxidizes variamine blue to violet colored species of maximum absorption at 556 nm. The absorbance is measured within the pH range of 4.0-4.2. Beer’s law is obeyed in the range of 0.5-5.8 μg mL–1, 0.2-7.0 μg mL–1, 0.2-5.0 μg mL–1 and 0.5-8.5 μg mL–1 for cefotaxime, ceftriaxone, cefadroxil and cephalexin respectively. The analytical parameters were optimized and the method is successfully applied for the determination of cefotaxime, ceftriaxone, cefadroxil and cephalexin in pharmaceuticals.


2015 ◽  
Vol 12 (2) ◽  
pp. 317-323
Author(s):  
Baghdad Science Journal

A simple, and rapid spectrophotometric method for the estimation of paracetamol has been developed. The methods is based on diazotisation of 2,4-dichloroaniline followed by a coupling reaction with paracetamol in sodium hydroxide medium. All variables affecting the reaction conditions were carefully studied. Beer's law is obeyed in the concentration range of 4-350 ?gml?1 at 490 nm .The method is successfully employed for the determination of paracetamol in pharmaceutical preparations. No interferes observed in the proposed method. Analytical parameters such as accuracy and precision have been established for the method and evaluated statistically to assess the application of the method.


1977 ◽  
Vol 60 (6) ◽  
pp. 1350-1354
Author(s):  
Daniel J Sullivan

Abstract A spectrophotometric method for determining Fe2+, Fe3+, and total Fe in drugs has been developed, using α, α′-dipyridyl as the colorimetric reagent. The method is applicable to tablets, elixirs, injectables, and bulk powders. Eight collaborators analyzed a synthetic iron preparation and 7 commercial samples. For the synthetic iron preparation, the average recovery was 100.3% and the coefficient of variation was 1.02%. For 7 commercial samples, the average coefficient of variation was 1.44%. The method has been adopted as official first action.


1990 ◽  
Vol 73 (4) ◽  
pp. 616-619 ◽  
Author(s):  
Karen S Harlin ◽  
P Frank Ross

Abstract Ten collaborating laboratories assayed 4 blind duplicate pairs of whole bovine blood for cholinesterase activity. The 4 sample pairs ranged from normal (100 %) to severely organophosphorus- lnhiblted (&lt;10%) activity. Collaborators also received commercially available human lyophllized serum as an external control and a chromate solution to evaluate spectrophotometer performance. The Ellman kinetic assay was performed on a 1:1000 dilution of the whole blood In pH 8.0 phosphate buffer. The method monitors the increase in absorbance at 412 nm caused by formation of 5-thio-2- nltrobenzolc acid (yellow reaction product). Repeatability standard deviations (RSDr) ranged from 4.30 to 14.2%; reproducibility standard deviations (RSDR) ranged from 6.99 to 19.3 %. The lower limit of detection was estimated to be 0.10 μmole/mL/min. The method has been approved interim official first action by AOAC.


1973 ◽  
Vol 56 (3) ◽  
pp. 681-683
Author(s):  
Marshall C Stricklin

Abstract A collaborative study was conducted on simulated tablet and injection preparations at 2 concentration levels each and a 20 tablet composite of a tablet simulating presently marketed dosage forms of benztropine mesylate. Analysis involves the extraction of benztropine from 0.2N H2SO4 with bromophenol blue in CHCl3. Absorbance of the dye complex formed is measured at about 410 nm. Average recoveries and standard deviations submitted were: 98.9±2.54 and 99.2±2.58, 100.1±2.78 and 100.0±2.19, and 100.1±2.23%, respectively. The method has been adopted as official first action.


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