Determination of Amino Acids in Feeds: Collaborative Study

1994 ◽  
Vol 77 (6) ◽  
pp. 1362-1402 ◽  
Author(s):  
Cynthia R Llames ◽  
Johannes Fontaine
Keyword(s):  
Amino Acids ◽  
Acid Hydrolysis ◽  
Hydrobromic Acid ◽  
Collaborative Study ◽  
Performic Acid ◽  
Acid Oxidation ◽  
Sodium Metabisulfite ◽  
Hydrolysis Method ◽  
Relative Standard

Abstract A total of 28 laboratories (including authors’ laboratories) participated in a collaborative study for determination of amino acids in feeds using 3 complementary procedures. Each collaborator analyzed 5 blind duplicate samples of feed and ingredients used in the poultry industry. The amount of amino acids in these materials ranged from 0.10 to 8.50%. Twenty-three laboratories conducted analyses using performic acid oxidation with acid hydrolysis—sodium metabisulfite method, 16 laboratories performed analyses using performic acid oxidation with acid hydrolysis—hydrobromic acid method, and 15 laboratories used acid hydrolysis method. The repeatability relative standard deviation values for all amino acids for all 3 procedures ranged from 1.1 to 5.6% for broiler finisher feed, 1.1 to 4.73% for starter feed, 1.3 to 9.6% for corn, 0.8 to 3.96% for fishmeal, and 0.8 to 12.7% for poultry meal. The reproducibility relative standard deviation values for all amino acids ranged from 3.71 to 19.80% for broiler finisher feed, 4.1 to 16.93% for starter feed, 4.4 to 28.2% for corn, 3.46 to 18.96% for fishmeal, and 3.73 to 24.1% for poultry meal. The performic acid oxidation with acid hydrolysis—sodium metabisulfite and hydrobromic acid methods, and acid hydrolysis method for determination of amino acids in feeds have been adopted first action by AOAC INTERNATIONAL.

Quantitative Analysis of Cystine, Methionine, Lysine, and Nine Other Amino Acids by a Single Oxidation-4 Hour Hydrolysis Method

1987 ◽  
Vol 70 (1) ◽  
pp. 171-174 ◽  
Author(s):  
Charles W Gehrke ◽  
Paul R Rexroad ◽  
Robert M Schisla ◽  
Joseph S Absheer ◽  
Robert W Zumwalt
Keyword(s):  
Amino Acids ◽  
Amino Acid ◽  
Amino Acid Content ◽  
Performic Acid ◽  
Acid Oxidation ◽  
Hydrolysis Method ◽  
Methionine Sulfone ◽  
Limiting Amino Acid ◽  
Hydrolysis Of

Abstract The sulfur-containing amino acids cystine and methionine play important roles in animal, especially avian, nutrition. Because these ndror-containing amino acids are destroyed to varying extents by 6N HC1 hydrolysis, oxidation and hydrolysis of cystine to cysteic add and methionine to methionine sulfone have been widely used for determination of cystine and methionine. Lysine is considered the next limiting amino acid after the sulfur amino acids in poultry •ntrition; therefore, determination of the amino acid content of rations focuses first on these 3 amino acids. The objective of this investigation was to establish whether lysine and other amino acids could be accurately determined in proteinaceous materials which had mdergone performic acid oxidation. To perform this evaluation, lysine was determined in a variety of protein-containing materials both with and without performic acid oxidation. Performic acid oxidation followed by 6N HC1 hydrolysis at 145°C for 4 h allows accurate measurement of 3 amino acids especially important to poultry nutrition, cystine, methionine, and lysine, in a single preoxidized hydralysate; this method can be extended to another 9 protein amino adds.

Determination of Sulfur Amino Acids and Tryptophan in Foods and Food and Feed Ingredients: Collaborative Study

1988 ◽  
Vol 71 (3) ◽  
pp. 603-606
Author(s):  
Maryann C Allred ◽  
John L Macdonald
Keyword(s):  
Amino Acids ◽  
Amino Acid ◽  
Collaborative Study ◽  
Performic Acid ◽  
Cysteic Acid ◽  
Protein Hydrolysis ◽  
Sulfur Amino Acids ◽  
Feed Ingredients ◽  
Food And Feed

Abstract Samples of 4 foods, 1 animal feed, isolated soy protein, and 0-lao toglobulin were analyzed by 9 laboratories to determine concentrations of cysteine as cysteic acid, methionine as methionine sulfone, and tryptophan. Sulfur amino acids were determined by AOAC method 43.A08-43.A13 for food and feed ingredients, in which samples are oxidized with performic acid before protein hydrolysis with 6N HC1. Tryptophan was determined after protein hydrolysis with 4.2N NaOH. In both methods, free amino acids were separated by ionexchange or reverse-phase chromatography. Each laboratory was provided with detailed methods and with sealed vials containing solutions of standards. Samples were analyzed in duplicate, and variation between laboratories was determined. Coefficients of variation between laboratories for the 6 samples ranged from 5.50 to 11.8% for methionine as methionine sulfoxide, 8.59 to 17.3% for cysteine as cysteic acid, and 3.87 to 16.1% for tryptophan. Amino acid recoveries were determined by analysis of β-lactoglobulin and were based on expected levels of each amino acid obtained from amino acid sequence data. The mean recovery of cysteine was 97% with a range of 88-119%. For methionine, mean recovery was 98% (range 89-115%) and for tryptophan, 85% (range 59-102%). Method 43.A08- 43.A13 for food and feed ingredients has been adopted official first action for determination of cysteine and methionine in processed foods. The alkaline hydrolysis method has been adopted official first action for determination of tryptophan in foods and food and feed ingredients

Precolumn Phenylisothiocyanate Derivatization and Liquid Chromatography of Amino Acids in Food

1989 ◽  
Vol 72 (6) ◽  
pp. 912-916 ◽  
Author(s):  
Steven R Hagen ◽  
Beverly Frost ◽  
Jorg Augustin
Keyword(s):  
Amino Acids ◽  
Liquid Chromatography ◽  
Food Item ◽  
Food Samples ◽  
Protein Hydrolysates ◽  
Performic Acid ◽  
Acid Oxidation ◽  
Coefficients Of Variation

Abstract A precolumn phenylisothiocyanate derivatization method is described for the determination of amino acids in protein hydrolysates from a wide variety of complex food matrixes, with and without performic acid oxidation pretreatment. Analysis of samples that were not pretreated with performic acid was necessary since this pretreatment destroyed an average of 25% of the histidine and 87% of the tyrosine present in the food samples. This method is rapid and reproducible; coefficients of variation between duplicate analyses of the same food item were less than 5% for a majority of the amino acids. Occasionally, variation between duplicate analyses for histidine and tyrosine was greater than 10%. Recoveries of amino acids added to samples were in the 100% range.

scholarly journals Liquid Chromatographic Determination of Lysine, Methionine, and Threonine in Pure Amino Acids (Feed Grade) and Premixes: Collaborative Study

2000 ◽  
Vol 83 (4) ◽  
pp. 771-783 ◽  
Author(s):  
Johannes Fontaine ◽  
Marcelle Eudaimon ◽  
J Bargholz ◽  
M W Empie ◽  
S Eriksson ◽  
...  
Keyword(s):  
Amino Acids ◽  
Amino Acid ◽  
Collaborative Study ◽  
Cation Exchange Resin ◽  
Chromatographic Determination ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract A total of 17 laboratories (including one author's laboratory) participated in a collaborative study for determination of lysine, methionine, and threonine in trade products or concentrated amino acid premixes. Thirteen samples, 4 pure amino acids and 6 premixes, including 3 Youden matched pairs, were analyzed. The applied liquid chromatographic (LC) method using cation-exchange resin and post-column derivatization with ninhydrin or o-phthaldialdehyde was shown to be accurate and specific for the analytes. Titration procedures, normally used for the assay of pure amino acids, are unspecific and the accuracy of the results can be affected by impurities. Repeatability relative standard deviations, RSDr, ranged from 0.84 to 1.17% for pure amino acids and from 0.50 to 1.68% for premixes; reproducibility relative standard deviations RSDR, ranged from 1.52 to 2.31% for pure amino acids and from 1.48 to 2.59% for premixes. Recoveries were between 97.5 and 102.8% of the expected amino acid assays. The method has been adopted Official First Action status by AOAC INTERNATIONAL.

Collaborative Study of the Determination of Fat in Intermediate Moisture Pet Foods

1976 ◽  
Vol 59 (6) ◽  
pp. 1218-1223
Author(s):  
Gustav O Kuhn
Keyword(s):  
Petroleum Ether ◽  
Acid Hydrolysis ◽  
Cross Section ◽  
Collaborative Study ◽  
Pet Food ◽  
Petroleum Ether Extraction ◽  
Hydrolysis Method ◽  
Ether Extraction ◽  
Aoac Method

Abstract Four different semimoist pet food formulations representing a cross section of commercial products were studied collaboratively for fat content by 2 methods. Ten laboratories participated in the study. Direct petroleum ether extraction by AOAC method 7.045 yielded low and variable fat recovery. AOAC acid hydrolysis method 7.047 for fat in baked dog foods was satisfactory for semimoist pet foods. The method, with some editorial changes, was adopted as official first action for this type of pet food.

Colorimetric Determination of Hydroxyproline as Measure of Collagen Content in Meat and Meat Products: NMKL Collaborative Study

1990 ◽  
Vol 73 (1) ◽  
pp. 54-57 ◽  
Author(s):  
Kurt Kolar
Keyword(s):  
Collaborative Study ◽  
Colorimetric Method ◽  
Meat Products ◽  
Acid Oxidation ◽  
Colorimetric Determination ◽  
Mean Values ◽  
Collaborative Studies ◽  
Freeze Dried ◽  
Analytical Result

Abstract A colorimetric method for the determination of hydroxyproline as a measure of collagen in meat and meat products has been collaboratively studied in 18 laboratories. The method includes hydrolysis with sulfuric acid, oxidation with chloramine- T, and formation of a reddish purple complex with 4- dimethylaminobenzaldehyde. Five frozen and 3 freeze-dried samples were tested, ranging in content from 0.11 to 0.88% and from 0.39 to 4.0% hydroxyproline, respectively. The mean values of 2 identical samples were 0.245 and 0.251 %. The average recovery from a spiked sample was 96.1 %. The hydroxyproline content of a known sample (a mixture of 2 samples in the ratio 5:2) was calculated to 1.42%, which agrees well with the analytical result, 1.40%. In comparison with other collaborative studies, based on the ISO analytical method, the repeatability and reproducibility of this method agree well with the other results. This method was accepted as an official NMKL method by all national Committees, and has been adopted official first action by AOAC as an NMKLAOAC method.

Optimisation of microwave-assisted acid hydrolysis for the determination of seleno-amino acids bound to proteins in powdered milk, lyophilized milk and infant formula

2019 ◽  
Vol 79 ◽  
pp. 128-133
Author(s):  
Romina Lopez ◽  
Luis Escudero ◽  
Roberto D’Amato ◽  
Daniela Businelli ◽  
Massimo Trabalza-Marinucci ◽  
...  
Keyword(s):  
Amino Acids ◽  
Acid Hydrolysis ◽  
Infant Formula ◽  
Powdered Milk ◽  
Microwave Assisted

scholarly journals Indirect and Direct Determination of the Casein Content of Milk by Kjeldahl Nitrogen Analysis: Collaborative Study

1998 ◽  
Vol 81 (4) ◽  
pp. 763-774 ◽  
Author(s):  
Joanna M Lynch ◽  
David M Barbano ◽  
J Richard Fleming
Keyword(s):  
Standard Deviation ◽  
Nitrogen Content ◽  
Relative Standard Deviation ◽  
Collaborative Study ◽  
Direct Determination ◽  
Raw Milk ◽  
Method Performance ◽  
Relative Standard ◽  
Milk Casein

Abstract The classic method for determination of milk casein is based on precipitation of casein at pH 4.6. Precipitated milk casein is removed by filtration and the nitrogen content of either the precipitate (direct casein method) or filtrate (noncasein nitrogen; NCN) is determined by Kjeldahl analysis. For the indirect casein method, milk total nitrogen (TN; Method 991.20) is also determined and casein is calculated as TN minus NCN. Ten laboratories tested 9 pairs of blind duplicate raw milk materials with a casein range of 2.42- 3.05℅ by both the direct and indirect casein methods. Statistical performance expressed in protein equivalents (nitrogen ⨯ 6.38) with invalid and outlier data removed was as follows: NCN method (wt%), mean = 0.762, sr = 0.010, SR = 0.016, repeatability relative standard deviation (RSDr) = 1.287℅, reproducibility relative standard deviation (RSDR) = 2.146%; indirect casein method (wt℅), mean = 2.585, repeatability = 0.015, reproducibility = 0.022, RSDr = 0.560℅, RSDR = 0.841; direct casein method (wt℅), mean = 2.575, sr = 0.015, sR = 0.025, RSDr = 0.597℅, RSDR = 0.988℅. Method performance was acceptable and comparable to similar Kjeldahl methods for determining nitrogen content of milk (Methods 991.20, 991.21,991.22, 991.23). The direct casein, indirect casein, and noncasein nitrogen methods have been adopted by AOAC INTERNATIONAL.

Ozonolysis of unsaturated fatty acids. II. Esterification of the total products from the oxidative decomposition of ozonides with 2,2-dimethoxypropane

1967 ◽  
Vol 45 (13) ◽  
pp. 1405-1410 ◽  
Author(s):  
John D. Castell ◽  
R. G. Ackman
Keyword(s):  
Fatty Acids ◽  
Liquid Chromatography ◽  
Unsaturated Fatty Acids ◽  
Performic Acid ◽  
Acid Oxidation ◽  
Gas Liquid Chromatography ◽  
Positional Isomers ◽  
Flame Ionization ◽  
Hydrogen Flame

The total acidic products from the performic acid oxidation of the ozonide of methyl oleate formed in methanol may be esterified directly in a few hours with 2,2-dimethoxypropane. The ester concentrations are adequate for the determination of the positional isomers of monoethylenic fatty acids directly from the reaction mixture, using a hydrogen flame ionization gas–liquid chromatography detector. Dimethyl sulfoxide was not required to prevent the breakdown of 2,2-dimethoxypropane under the conditions employed.

scholarly journals Determination of uric acid in human serum by an enzymatic method using N-methyl-N-(4-aminophenyl)-3-methoxyaniline reagent

2003 ◽  
Vol 68 (8-9) ◽  
pp. 691-698 ◽  
Author(s):  
Milena Jelikic-Stankov ◽  
Predrag Djurdjevic ◽  
Dejan Stankov
Keyword(s):  
Uric Acid ◽  
Human Serum ◽  
Limit Of Detection ◽  
Ascorbate Oxidase ◽  
Acid Oxidation ◽  
Uric Acid Concentration ◽  
Enzymatic Method ◽  
Limit Of Quantification ◽  
Relative Standard

In this work a new enzymatic method for the determination of uric acid in human serum has been developed. The method is based on the oxidative coupling reaction between the N-methyl-N-(4-aminophenyl)-3-methoxyaniline (NCP) reagent and the hydrogen ? donor reagent N-ethyl-N-(2-hydroxy-3-sulfopropyl)-3-methylaniline (TOOS), in the system involving three enzymes: uricase, peroxidase and ascorbate oxidase. Using this method uric acid could be determined in concentrations up to 1.428 mmol/L, with a relative standard deviation of up to 1.8 %. The effect of the medium pH and the NCP concentration on the linearity of the chromogen absorbance versus the uric acid concentration curve was investigated. The influence of the uricase activity on the maximum rate of uric acid oxidation was also examined. The use of the NCP reagent demonstrated a more precise and more sensitive determination of the uric acid compared to the determination with 4-aminoantipyrine (4-AA) as the coupling regent. The sensitivity of the method determined from the calibration curve was 0.71 absorbance units per mmol/L of uric acid; the limit of detection was LOD = 0.0035 mmol/L and the limit of quantification was LOQ = 0.015 mmol/L of uric acid.

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