Spectrophotometric Determination of Cyclamate in Foods: NMKL Collaborative Study

1987 ◽  
Vol 70 (3) ◽  
pp. 588-590
Author(s):  
Anna-Maija K Sjoberg ◽  
Timo A Alanko
Keyword(s):  
Aqueous Solution ◽  
Ethyl Acetate ◽  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Collaborative Study ◽  
Soft Drinks ◽  
Uv Absorption ◽  
Acidic Aqueous Solution ◽  
Coefficients Of Variation

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.

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.

Spectrophotometric Determination of Caffeine in Coffee Products: Collaborative Study

1979 ◽  
Vol 62 (4) ◽  
pp. 705-708
Author(s):  
John M Newton
Keyword(s):  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Collaborative Study ◽  
Caffeine Content ◽  
Coefficients Of Variation ◽  
Decaffeinated Coffee

Abstract An ultraviolet (UV) spectrophotometric method for determining caffeine in regular and decaffeinated coffee products has been studied collaboratively. Nine laboratories participated in this study which compares the proposed UV method with the official AOAC micro Bailey-Andrew method. Caffeine content was determined on as-is basis on 8 samples of green, roasted, and soluble coffees. The coefficients of variation for the proposed method ranged from 2.02 to 6.98% for the 8 samples studied. The results agreed well with those from the Bailey-Andrew method. The method was 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.

Semiautomated Method for the Analysis of Chlorpheniramine Maleate Tablets: Collaborative Study

1979 ◽  
Vol 62 (6) ◽  
pp. 1197-1201
Author(s):  
Ross D Kirchhoefer ◽  
◽  
R L Brown ◽  
J P Gleason ◽  
S Hauser ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Excellent Agreement ◽  
Active Ingredient ◽  
Close Agreement ◽  
Collaborative Study ◽  
Chlorpheniramine Maleate ◽  
Acidic Aqueous Solution ◽  
Coefficients Of Variation ◽  
Semiautomated Method

Abstract A semiautomated method for the analysis of chlorpheniramine maleate tablets, which is based on the USP XIX general assay for salts of organic nitrogenous bases, was collaboratively studied by 6 laboratories. Collaborators were supplied with 4 composites from 4 manufacturers. In the method, the active ingredient is dissolved in dilute HC1, sampled, made basic with dilute NaOH, and extracted with isooctane. The isooctane phase is resampled and the drug is re-extracted into dilute HCL. The absorbance of the acidic aqueous solution is measured at 265 nm. The Associate Referee assayed the collaborative samples to compare the semiautomated and USP XIX methods, and found close agreement in the results from the 2 methods. In the collaborative study of the semiautomated method, there was excellent agreement of the results obtained by the collaborators. The coefficients of variation ranged from 0.46 to 2.24%. The method has been adopted as official first action.

scholarly journals Development of Method for Extractive Spectrophotometric Determination of Fe(III) with 2-Hydroxy-1-Naphthalene Carboxaldehyde Phenyl Hydrazone as an Analytical Reagent

2013 ◽  
Vol 14 ◽  
pp. 7-12
Author(s):  
Ratnamala P. Sonawane ◽  
R.S. Lokhande ◽  
Utkarsha M. Chavan
Keyword(s):  
Ethyl Acetate ◽  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Molar Absorptivity ◽  
Beer's Law ◽  
Beer’S Law ◽  
Coloured Complex ◽  
Analytical Reagent

A spectrophotometric method has been developed for the determination of Fe(III) using 2-Hydroxy-1-Naphthalene carboxaldehyde phenyl hydrazone as an extractive reagent. The reagent forms a coloured complex, which has been quantitatively extracted into ethyl acetate at pH 6. The method obeys Beer’s law over arrange from 1 to 7 ppm. The Molar absorptivity and Sandell’s sensitivity were 0.31 × 104 L mol-1cm-1 and 0.13 μg cm-2 respectively. The proposed method is very sensitive and selective. The method has been successfully applied to synthetic and commercial samples.

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 Spectrophotometric Method for Determining Maleic Hydrazide Residues in Tobacco and Vegetables

1975 ◽  
Vol 58 (6) ◽  
pp. 1235-1243
Author(s):  
Milan Ihnat ◽  
Brian Thompson
Keyword(s):  
Standard Deviation ◽  
Spectrophotometric Method ◽  
Strong Evidence ◽  
Maleic Hydrazide ◽  
Collaborative Study ◽  
Green Bean ◽  
F Test ◽  
Coefficients Of Variation ◽  
Better Than

Abstract A distillation-spectrophotometric method for the determination of maleic hydrazide residues in tobacco and vegetables reported previously was studied collaboratively. Ten laboratories submitted analytical results on 10 samples containing residues resulting either from field treatment or laboratory fortification. The samples were estimated to contain from 0.99 to 16.36 μg maleic hydrazide/0.5 g sample analyzed. The coefficients of variation based on precision standard deviation ranged from 57.7% for the lowest residue content to 32.4% for the highest. The corresponding coefficients of variation based on overall standard deviations were estimated to be at least one-fifth larger. Strong evidence of systematic laboratory differences was found (F-test, significant at 0.1%). Apparent recoveries of 10.0 fifl maleic hydrazide added to 0.5 g fluecured tobacco and potato were 97.3 and 89.7%, respectively. Apparent recoveries of 16.0 and 16.5 μg added to 0.5 g green bean were 87.4 and 85.5%, respectively. The precision of the method studied was no better than that of the current official final action method, 29.121–29.127, and its adoption is not recommended.

High Performance Liquid Chromatographic Method for Determination of Temephos in Technical and Formulated Products: Collaborative Study

1982 ◽  
Vol 65 (3) ◽  
pp. 580-583
Author(s):  
James W Miles ◽  
Dwight L Mount
Keyword(s):  
Ethyl Acetate ◽  
High Performance ◽  
Collaborative Study ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Water Dispersible ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic

Abstract An HPLC method for the determination of temephos in temephos technical and formulated products has been subjected to an international collaborative study with 14 laboratories participating. Samples were extracted with ethyl acetate and eluted on a silica gel column with ethyl acetate-hexane (1 + 9); p-nitrophenyl p-nitrobenzoate served as the internal standard. Collaborators were furnished samples of technical, 20 and 50% emulsifiable concentrates, 50% water-dispersible powder, and 1% sand granules. The coefficients of variation of the values obtained on the 5 samples were 1.21,2.02,1.26,1.89, and 9.90%, respectively. The method has been adopted official first action.

Spectrophotometric Determination of Pyrantel Tartrate in Swine Feeds by Method of Standard Additions: Collaborative Study

1978 ◽  
Vol 61 (2) ◽  
pp. 296-298
Author(s):  
Mark A Litchman
Keyword(s):  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Collaborative Study ◽  
Standard Additions ◽  
The Mean ◽  
Standard Deviations ◽  
Pyrantel Tartrate

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.

Gas-Liquid Chromatographic Quantitation of Cocaine.HC1 in Powders and Tablets: Collaborative Study

1978 ◽  
Vol 61 (3) ◽  
pp. 683-686
Author(s):  
Charles C Clark
Keyword(s):  
Aqueous Solution ◽  
Collaborative Study ◽  
Internal Standard ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic

Abstract Eight laboratories collaboratively studied a method for the quantitative gas-liquid chromatographic (GLC) determination of cocaine. HC1 in solid forms. The cocaine.HQ and other water solubles are dissolved in dilute HC1. The aqueous solution is made weakly basic with K2HPO4, and the organic solubles are extracted into CHC13 for the GLC determination of cocaine. Tetracosane (n-C24) is incorporated in the extracting CHC13 as an internal standard. Five samples of known cocaine.HC1 concentration and one sample of commercial ground tablets were collaboratively studied. The cocaine. HC1 content ranged from 6 to 100%. Recoveries ranged from 98.7 to 103%; coefficients of variation ranged from 0.89 to 3.16. The method was adopted as official first action.

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