Determination of Procaine and Related Local Anesthetics. II. Collaborative Study

1975 ◽  
Vol 58 (1) ◽  
pp. 93-94
Author(s):  
Joseph B Proctor ◽  
Thomas D Doyle
Keyword(s):  
Spectrophotometric Determination ◽  
Local Anesthetics ◽  
Active Component ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Ion Pairing ◽  
The Other ◽  
Three Solutions ◽  
Average Recovery

Abstract The ion-pairing chromatographic method reported previously for the isolation and spectrophotometric determination of the local anesthetics, alone and in combination, was studied collaboratively. Three solutions were assayed. One containing procaine as the single active component gave an average recovery of 99.8± 1.7%. A mixture of procaine and tetracaine gave results of 99.3±1.6 and 98.9±8.82%, respectively. A third solution containing procaine and propoxycaine assayed 100.0±1.5 and 99.1±1.9%, respectively. It was shown that low results for tetracaine were due to loss during the final evaporative step. The method for samples containing tetracaine should be studied further. The other methods have been adopted as official first action.

Spectrophotometric Determination of Cyclamate in Soft Drinks and Desserts: Complementary Collaborative Study

1988 ◽  
Vol 71 (6) ◽  
pp. 1212-1214
Author(s):  
Anna-Maija K SJÖBERG
Keyword(s):  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Soft Drink ◽  
Collaborative Study ◽  
Soft Drinks ◽  
Food Control ◽  
Average Recovery ◽  
Relative Standard ◽  
Standard Deviations

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.

Gas Chromatographic Determination of Phenolic Compounds in Drug Preparations: Collaborative Study

1972 ◽  
Vol 55 (3) ◽  
pp. 610-612 ◽  
Author(s):  
Carol C Douglas
Keyword(s):  
Phenolic Compounds ◽  
Methyl Salicylate ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
The Other ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method for the determination of phenol, methyl salicylate, menthol , and camphor in drug preparations was studied collaboratively by 9 laboratories. Mean recoveries were: phenol 98.2, 106.0, a n d 103.6%; methyl salicylate 103.9, 102.0, and 101.9%; menthol 102.9 and 100.9%; and camphor 101.9 and 100.9%. The method has been adopted as official first action for camphor-containing drugs. Additional study will be done to improve recoveries for the other 3 compounds.

Collaborative Study of the Determination of Sorbic Acid in Wine

1975 ◽  
Vol 58 (1) ◽  
pp. 133-135
Author(s):  
Arthur Caputi ◽  
Karen Slinkard
Keyword(s):  
Sorbic Acid ◽  
Collaborative Study ◽  
Thiobarbituric Acid ◽  
The Other ◽  
Ultraviolet Spectrophotometry ◽  
Acid Complex ◽  
Average Recovery ◽  
Colorimetric Measurement ◽  
Coefficients Of Variation

Abstract Eleven collaborators participated in a study of 2 methods for determining sorbic acid in wine. One method utilizes ultraviolet spectrophotometry and the other depends on the colorimetric measurement of a thiobarbituric acid complex. Three different wine types were each spiked with 200, 300, and 400 mg sorbic acid/ L. Average recovery ranged from 97.3 to 107.5% with the thiobarbituric acid method with coefficients of variation from 4.4 to 8.7%. The ultraviolet method gave recoveries from 97 to 103.5% with coefficients of variation ranging from 2.0 to 6.4%. Comments on both methods from collaborators were favorable. Both methods have been adopted as official first action.

Collaborative Study of Spectrophotometric Determination of Hexachlorocyclopentadiene in Technical Chlordane

1966 ◽  
Vol 49 (2) ◽  
pp. 254-257
Author(s):  
Marshall Malina
Keyword(s):  
Spectrophotometric Determination ◽  
Collaborative Study ◽  
Quantitative Measure ◽  
Ultraviolet Absorption ◽  
The Other ◽  
Positive Bias ◽  
Alternative Procedures ◽  
Small Absorption

Abstract Hexachlorocyclopentadiene exhibits strong ultraviolet absorption at 324 mμ, while technical chlordane exhibits only small absorption at this wavelength. The intensity of this absorption is a quantitative measure of the hexachlorocyclopentadiene content. Eight laboratories cooperated in a collaborative study of two alternative procedures on six samples. Results show that one procedure exhibits a positive bias and that the other procedure does not. The precision of both procedures is excellent. The methods are recommended for adoption as official, first action.

Collaborative Study of a Spectrophotometric Determination of Ferric, Ferrous, and Total Iron in Drugs by Reaction with α,α′-Dipyridyl

1977 ◽  
Vol 60 (6) ◽  
pp. 1350-1354
Author(s):  
Daniel J Sullivan
Keyword(s):  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Coefficient Of Variation ◽  
Collaborative Study ◽  
Total Iron ◽  
Average Recovery ◽  
Average Coefficient ◽  
Iron Preparation ◽  
Colorimetric Reagent

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.

Collaborative Study of a Chromatographic Method for Sodium Diphenylhydantoin in Capsules

1972 ◽  
Vol 55 (1) ◽  
pp. 170-172
Author(s):  
C G Cunningham ◽  
Charlotte A Brunner ◽  
Joseph Levine
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Synthetic Mixture ◽  
Commercial Preparation ◽  
Average Recovery ◽  
Average Value ◽  
Column Chromatographic

Abstract A column chromatographic method is described for the determination of sodium diphenylhydantoin in capsules. A collaborative study was performed, using a synthetic mixture and a composite of a commercial preparation as samples. The average recovery for the synthetic mixture was 100.2 ±1.6%, and the average value for the commercial preparation was 96.2±1.6% of the labeled content. It is recommended that this method be adopted as official first action.

Collaborative Study of a Column Chromatographic Method for Chlorothiazide, Methyclothiazide, and Polythiazide

1973 ◽  
Vol 56 (3) ◽  
pp. 677-680
Author(s):  
F Raymond Fazzari
Keyword(s):  
Acetic Acid ◽  
Spectrophotometric Determination ◽  
Organic Phase ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Standard Deviations ◽  
Column Chromatographic

Abstract Chlorothiazide is eluted from a K2HPO4 column with acetic acid-ether solvent and extracted from the organic phase into HCl for the Spectrophotometric determination. Methyclothiazide and polythiazide are eluted from a NaHCO3 column with CHCl3 and measured directly. The method was collaboratively studied by 10 analysts. The average per cent recovered and standard deviations for preparations of chlorothiazide and methyclothiazide were 100.2±0.67 and 99.8±1.64, respectively. The method for chlorothiazide and methyclothiazide has been adopted as official first action.

Collaborative Study of the Spectrophotometric Determination of Procainamide Hydrochloride

1976 ◽  
Vol 59 (4) ◽  
pp. 807-810
Author(s):  
Jeffrey C Hamm
Keyword(s):  
Sodium Hydroxide ◽  
Acid Medium ◽  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Collaborative Study ◽  
Dosage Forms ◽  
Standard Deviations

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.

Spectrophotometric Determination of Phosphine Residues in Rice

1985 ◽  
Vol 68 (2) ◽  
pp. 205-208 ◽  
Author(s):  
Jois R Rangaswamy ◽  
Mysore Muthu
Keyword(s):  
Spectrophotometric Determination ◽  
Closed System ◽  
The Other ◽  
Parboiled Rice ◽  
Polished Rice ◽  
Rice Samples ◽  
Phosphine Residues

Abstract Phosphine residues were determined in 2 types of rice samples, raw polished and parboiled. The yellow chromophore due to phosphine from raw polished rice had 2 absorption maxima, a strong one at 370- 380 nm and a weaker one at 400-410 nm. The chromophore from parboiled rice also had 2, one at 390-400 nm and the other at 410-420 nm. A closed system containing rice and a phosphine tablet or powder yielded 93-99% recovery of fortified phosphine. At any given dose of phosphine, parboiled rice retained a higher amount of residue after aeration than did raw polished rice.

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