Spectrofluorometric Determination of Lasalocid Sodium in Finished Feeds and Premixes

1974 ◽  
Vol 57 (3) ◽  
pp. 636-641
Author(s):  
Modest Osadca ◽  
Mercedes Araujo
Keyword(s):  
Standard Deviation ◽  
Ethyl Acetate ◽  
Boric Acid ◽  
Chemical Method ◽  
Sodium Concentration ◽  
Acid Complex ◽  
Average Recovery ◽  
Spectrofluorometric Determination ◽  
Coefficients Of Variation

Abstract A simple, rapid, and sensitive chemical method is described for determining lasalocid sodium in finished poultry feeds and premixes. The drug is extracted with ethyl acetate directly from premixes and after a brief treatment with pH 4.7 buffer from finished feeds. Lasalocid sodium concentration is measured spectrofluorometrically and a correction for nonspecific fluorescence is determined after formation of a lasalocid- boric acid complex. Replicate assays of typical poultry mashes and pellets containing about 0.0075% lasalocid sodium yielded coefficients of variation of 2.8 to 5.0%. Average recovery of lasalocid sodium added in the laboratory at 0.0037, 0.0075, and 0.0112% was 90% with a pooled standard deviation of ±1.86%.

Collaborative Study of a Spectrofluorometric Method for Lasalocid Sodium in Feeds

1975 ◽  
Vol 58 (3) ◽  
pp. 507-512
Author(s):  
Modest Osadca ◽  
Mercedes Araujo
Keyword(s):  
Ethyl Acetate ◽  
Boric Acid ◽  
Ethyl Acetate Extract ◽  
Collaborative Study ◽  
Feed Additives ◽  
Brief Treatment ◽  
Acid Complex ◽  
Coefficients Of Variation ◽  
Spectrofluorometric Method ◽  
Feed Samples

Abstract A collaborative study has been completed on a spectrofluorometric method for determining lasalocid sodium in finished poultry feeds. After a brief treatment of feed samples with pH 4.7 buffer, the drug is extracted with ethyl acetate. The ethyl acetate extract is further cleaned up by treatment with HCI and NaOH and quantitatively measured by spectrofluorometry. Nonspecific fluorescence is corrected for via the lasalocid-boric acid complex. The method is rapid, sensitive, and free of interference. A number of other feed additives, including monensin and ethoxyquin, do not interfere. Nine collaborators participated in the study and agreement between laboratories was satisfactory. The average recoveries of lasalocid sodium from the mash feeds added at levels of 0.0064, 0.0080, and 0.0096% were 100, 98, and 99%, respectively, and the corresponding coefficients of variation were 12.8, 8.2, and 8.0% (all results included). The method has been adopted as official first action.

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 the Determination of Dichlorophene in Veterinary Preparations by Ultraviolet Spectrophotometry

1972 ◽  
Vol 55 (1) ◽  
pp. 163-165
Author(s):  
Dalia M Gilvydis
Keyword(s):  
Standard Deviation ◽  
Collaborative Study ◽  
Liquid Extraction ◽  
Synthetic Mixture ◽  
Ultraviolet Spectrophotometry ◽  
Average Recovery ◽  
Liquid Liquid Extraction ◽  
Coefficients Of Variation ◽  
Standard Deviations

Abstract Dichlorophene is determined in veterinary preparations by a liquid-liquid extraction and UV quantitation. Eight collaborators each analyzed 4 commercial preparations and one synthetic mixture. The average recovery for dichlorophene in the synthetic mixture is 100.3% with a standard deviation of 2.13. The standard deviations obtained for the 5 samples range from 0.13 to 3.69 with coefficients of variation from 0.69 to 3.43. It is recommended that the method be adopted as official first action.

scholarly journals A sensitive spectrophotometric determination of tadalafil in pharmaceutical preparations and industrial wastewater samples

2013 ◽  
Vol 10 (3) ◽  
pp. 1005-1013 ◽  
Author(s):  
Baghdad Science Journal
Keyword(s):  
Standard Deviation ◽  
Industrial Wastewater ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Average Recovery ◽  
Relative Standard ◽  
Wastewater Samples ◽  
Sensitive Spectrophotometric Method

A simple, accurate, precise, rapid, economical and a high sensitive spectrophotometric method has been developed for the determination of tadalafil in pharmaceutical preparations and industrial wastewater samples, which shows a maximum absorbance at 204 nm in 1:1 ethanol-water. Beer's law was obeyed in the range of 1-7?g/ mL ,with molar absorptivity and Sandell ? s sensitivity of 0.783x105l/mol.cm and 4.97 ng/cm2respectively, relative standard deviation of the method was less than 1.7%, and accuracy (average recovery %) was 100 ± 0. 13. The limits of detection and quantitation are 0.18 and 0.54 µg .ml-1, respectively. The method was successfully applied to the determination of tadalafil in some pharmaceutical formulations (tablets) and industrial wastewater samples. The proposed method was validated by sensitivity and precision which proves suitability for the routine analysis of tadalafil in true samples.

Chemical Method for the Determination of Vitamin D in Evaporated Milk With Elimination of Cholesterol by Digitonin Precipitation

1969 ◽  
Vol 52 (6) ◽  
pp. 1189-1195 ◽  
Author(s):  
J Eisses ◽  
H Dk Vries
Keyword(s):  
Vitamin D ◽  
Standard Deviation ◽  
Calibration Curve ◽  
Chemical Method ◽  
Colorimetric Method ◽  
Sterol Content ◽  
Alumina Column ◽  
Decomposition Products ◽  
Colorimetric Measurement

Abstract The colorimetric method of Jones et al. for the determination of vitamin D in evaporated milk, based on theUSPXVI method, was modified to obtain a simpler colorimetric measurement and more accurate results. The main modification is the elimination of nearly all cholesterol, according to the procedure of Den Herder for the determination of the sterol content of fats, by precipitation with digitonin in the saponified mass. The Florex column, used in the procedure of Jones et al. for the elimination of decomposition products of vitamin A, was omitted since it gave high blank values; an alumina column was substituted. The resulting method, when applied to samples of evaporated milk to which a known quantity of vitamin D had been added, showed a recovery of 78% with a standard deviation of 6%, using a calibration curve based on crystalline vitamin D. Data from these measurements, as well as data from vitamin D determination on several brands of fortified and unfortified evaporated milk, are presented.

Automated Method for the Determination of Niacin and Niacinamide in Cereal Products: Collaborative Study

1975 ◽  
Vol 58 (4) ◽  
pp. 799-803
Author(s):  
Anthony F Gross
Keyword(s):  
Chemical Method ◽  
Collaborative Study ◽  
Pet Food ◽  
Microbiological Method ◽  
Chemical Methods ◽  
Cereal Products ◽  
Automated Method ◽  
Coefficients Of Variation ◽  
Baked Products

Abstract In a collaborative study, an automated method for the determination of niacin and niacinamide in cereal products was compared with the official final action microbiological (43.121–43.125) and chemical (43.044–43.046) methods. Ten samples of cereal products, including enriched flour, yeast-leavened baked products, fortified breakfast cereals, and baked pet food products, were submitted to 14 laboratories. Nine laboratories reported values by the automated method, 6 reported values by the microbiological method, and 7 reported values by the chemical method. The results from the microbiological method were not subjected to analysis of variance because of the unusually large between-laboratory variation. The between-laboratory coefficients of variation for the automated and chemical methods were 10.90 and 10.18%, on the basis of results from 7 and 4 laboratories, respectively. There was no significant (p>0.05) difference between methods when results from the 4 laboratories who used both methods were compared. The automated chemical method has been adopted as official first action.

Determination of Methyl 2-Benzimidazolecarbamate in Wine by Competitive Inhibition Enzyme Immunoassay

1993 ◽  
Vol 76 (4) ◽  
pp. 851-856 ◽  
Author(s):  
Rodney J Bushway ◽  
Lance R Paradis ◽  
Lewis B Perkins ◽  
Titan S Fan ◽  
Barbara E S Young ◽  
...  
Keyword(s):  
Enzyme Immunoassay ◽  
Competitive Inhibition ◽  
White Wines ◽  
Average Recovery ◽  
Total Analysis Time ◽  
Coefficients Of Variation ◽  
Limit Of Quantitation ◽  
Total Analysis ◽  
Commercial Kit

Abstract A benomyl polyclonal enzyme immunoassay (EIA) commercial kit was used to quantitate methyl 2- benzimidazolecarbamate (MBC), a degradation product of benomyl in wine. Total analysis time, including sample preparation, was 30 min. As many as 8 samples can be analyzed simultaneously with a limit of quantitation of 5 ppb. The assay logarithmic response was linear from 0.4 to 26 ppb MBC. Intra-assay percent coefficients of variation (%CVs) ranged from 2.4 to 13 for standards and from 7.4 to 21 for actual wine samples. Interassay %CVs varied from 2.6 to 15 for the standards and from 6.9 to 23 for the samples. Average recovery from samples spiked at 10–10 000 ppb was 93% for evaporated red and white wines. MBC was determined in 134 different wines by immunoassay and liquid chromatography (LC). Of these samples, 98 were positive for MBC by both methods with a correlation coefficient (r) of 0.986. The other 36 samples had MBC levels that either were not detectable by either procedure or were below the 10 ppb limit of quantitation for LC. Concentrations of MBC in wine ranged from 5 to 1329 ppb, with the majority ranging from 10 to 300 ppb. Also, a mini-study was conducted using the plate EIA format.

Simple Combustion-Vapor Trapping Technique for Determination of Mercury in Fish

1978 ◽  
Vol 61 (1) ◽  
pp. 43-47
Author(s):  
Fuad M Teeny
Keyword(s):  
Standard Deviation ◽  
Nitric Acid ◽  
Mercuric Chloride ◽  
Apparent Effect ◽  
Average Recovery ◽  
Sample Matrix ◽  
Fish Samples ◽  
Mercury In Fish

Abstract A simple combustion train was constructed for analyzing mercury in fish samples. A nitric acid trap was used to capture the mercury vapors which were released later by adding a tin salt. The method is rapid, accurate, and reproducible and permits one person to analyze 40 samples daily. Sample matrix had no apparent effect on the recovery of mercury. Mean recoveries from fish samples spiked with 0.3 and 1.0 μg mercuric chloride/g ranged from 97 to 105% with an average recovery of 101.5% and a standard deviation of 2.74%.

Volumetric Determination of Malathion, Using Dichlorofluorescein as Indicator

1976 ◽  
Vol 59 (1) ◽  
pp. 216-218
Author(s):  
Miguel Siquiroff ◽  
Ricardo Pollero ◽  
Rodolfo Goyena
Keyword(s):  
Standard Deviation ◽  
Petroleum Ether ◽  
Silver Nitrate ◽  
Ethyl Ether ◽  
Colorimetric Method ◽  
Florisil Column ◽  
Average Recovery ◽  
Florisil Column Chromatography ◽  
Volumetric Determination

Abstract A method has been developed which is based on alkali cleavage of malathion and volumetric determination of the resulting dimethylphosphorodithioate with silver nitrate, using dichlorofluorescein as the indicator. Pure malathion standards were analyzed by the proposed method, yielding a standard deviation of 0.27. Four typical malathion formulations containing talc, wheat flour, and anionic and nonionic emulsifiers were analyzed by both the proposed method and the former official first action colorimetric method with comparable results. Potential interferences from surfactants currently employed in liquid formulations are avoided by the use of Florisil column chromatography. Malathion is eluted from the column with petroleum ether-ethyl ether with an average recovery of 92.5%.

A Rapid Multiresidue Screen for Organophosphorus, Organochlorine, and N-Methyl Carbamate Insecticides in Plant and Animal Tissues

1994 ◽  
Vol 77 (5) ◽  
pp. 1263-1274 ◽  
Author(s):  
Dirk M Holstege ◽  
David L Scharberg ◽  
Elizabeth R Tor ◽  
Laura C Hart ◽  
Francis D Galey
Keyword(s):  
Ethyl Acetate ◽  
Solid Phase ◽  
Gel Permeation Chromatography ◽  
Bovine Liver ◽  
Animal Tissues ◽  
Average Recovery ◽  
Carbamate Insecticides ◽  
High Lipid ◽  
Level Method

Abstract A multiresidue screen for the quantitative determination of 43 organ op hosphorus, 17 orga no-chlorine, and 11 N-methyl carbamate insecticides in 10 g of plant or animal tissues is described. The insecticides are extracted with 5% ethanol in ethyl acetate (v/v). Samples with high lipid content are cleaned up by automated gel permeation chromatography with a 30% ethyl acetate in hexane (v/v) eluant and in-line silica gel minicolumns. Highly pigmented samples are cleaned up with class-specific solid-phase extraction columns. The concentrated extracts are analyzed by selective detection with gas chromatography or liquid chromatography. Recovery of 71 insecticides ranged from 77 to 113%. Analysis of fortified bovine liver (n = 5) resulted in an average recovery of 96 ± 4% at the 0.5 to 0.05 μg/g level. Analysis of fortified alfalfa hay (n = 5) resulted in a mean recovery of 94 ± 4% at the 0.06 to 0.5 μg/g level, and analysis of fortified fresh tomatoes (n = 5) resulted in an average recovery of 97 ± 3% at the 0.06 to 0.5 μg/g level. Method detection limits ranged from 0.02 to 0.5 μg/g for the compounds studied with a nominal 10 g sample.

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