Determination of Total Taurine in Pet Foods by Liquid Chromatography of the Dansyl Derivative: Collaborative Study

2000 ◽  
Vol 83 (4) ◽  
pp. 784-788 ◽  
Author(s):  
Kieran McCarthy ◽  
Claudia Hischenhuber ◽  
Neil Joyce ◽  
G Cherix ◽  
C Hischenhuber ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Collaborative Study ◽  
Gradient Elution ◽  
Taurine Concentration ◽  
Dansyl Derivative ◽  
Relative Standard ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method for the determination of total taurine in pet foods was evaluated in a collaborative study. Ten laboratories assayed 6 blind duplicate pairs of wet and dry pet foods. The taurine in the 6 sample pairs ranged from low (170 mg/kg) to high (2250 mg/kg) concentrations as is. Collaborators also assayed a sample of known taurine concentration for familiarization purposes. Samples were hydrolyzed to release bound taurine, which was subsequently converted to the dansyl derivative and quantitated by gradient-elution LC with fluorescence detection. Repeatability relative standard deviations, RSDr, ranged from 3.2 to 10.0%; reproducibility relative standard deviations, RSDR, ranged from 6.1 to 16.1%. The method has been adopted Official First Action status by AOAC INTERNATIONAL.

scholarly journals Taurine Analysis in Milk and Infant Formulae by Liquid Chromatography: Collaborative Study

1997 ◽  
Vol 80 (4) ◽  
pp. 860-866 ◽  
Author(s):  
David C Woollard ◽  
Harvey E Indyk ◽  
G Angyal ◽  
J Borbon ◽  
W Chase ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Infant Formula ◽  
Lower Limit ◽  
Fluorescence Detection ◽  
Collaborative Study ◽  
Dansyl Derivative ◽  
Infant Formulae ◽  
Limit Of Determination ◽  
Liquid Chromatographic

Abstract A collaborative study was conducted on a liquid chromatographic (LC) method for determination of taurine in infant formula and milk powders. Twenty laboratories participated in the analysis of 8 blind duplicates over the range of approximately 3–60 mg/100 g sample. The method involved protein removal, conversion to the dansyl-derivative, and isocratic LC separation with UV and/or fluorescence detection. Following outlier treatment, overall mean RSDR has been estimated at 7.00% for sup. plemented products with a HORRAT value of 1.1. The poorer precision at endogenous levels establishes a lower limit of determination of about 5 mg/100 g. An overall mean RSDr:RSDR value of 0.7 for all products demonstrated acceptable performance.

scholarly journals Determination of Vitamins A (Retinol) and E (alpha-Tocopherol) in Foods by Liquid Chromatography: Collaborative Study

2002 ◽  
Vol 85 (2) ◽  
pp. 424-434 ◽  
Author(s):  
Jonathan W DeVries ◽  
Karlene R Silvera ◽  
S Al-Hasani ◽  
J Alfiere ◽  
C Berge ◽  
...  
Keyword(s):  
Fatty Acids ◽  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Water Solution ◽  
Collaborative Study ◽  
Alpha Tocopherol ◽  
Food Matrix ◽  
Peak Areas ◽  
Liquid Chromatographic

Abstract A collaborative study was conducted for the determination of vitamins A and E. Existing AOAC liquid chromatographic (LC) methods are suited for specific vitamins A and E analytical applications. This method differs from existing methods in that it can be used to assay samples in all 9 sectors of the food matrix. Standards and test samples are saponified in basic ethanol–water solution, neutralized, and diluted, converting fats to fatty acids and retinol esters and tocopherol esters to retinol and tocopherol, respectively. Retinol and alpha-tocopherol are quantitated on separate LC systems, using UV detection at 313 or 328 nm for retinol, and fluorescence detection (excitation 290 nm, emission 330 nm) for alpha-tocopherol. Vitamin concentrations are calculated by comparison of the peak heights or peak areas of vitamins in test samples with those of standards.

scholarly journals Determination of Ochratoxin A in Wine and Beer by Immunoaffinity Column Cleanup and Liquid Chromatographic Analysis with Fluorometric Detection: Collaborative Study

2001 ◽  
Vol 84 (6) ◽  
pp. 1818-1827 ◽  
Author(s):  
Angelo Visconti ◽  
Michelangelo Pascale ◽  
Gianluca Centonze ◽  
E Anklam ◽  
A M Betbeder ◽  
...  
Keyword(s):  
Ochratoxin A ◽  
Red Wine ◽  
Collaborative Study ◽  
White Wine ◽  
Fluorometric Detection ◽  
Immunoaffinity Column ◽  
Relative Standard ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract The accuracy, repeatability, and reproducibility characteristics of a liquid chromatographic method for the determination of ochratoxin A (OTA) in white wine, red wine, and beer were established in a collaborative study involving 18 laboratories in 10 countries. Blind duplicates of blank, spiked, and naturally contaminated materials at levels ranging from ≤0.01 to 3.00 ng/mL were analyzed. Wine and beer samples were diluted with a solution containing polyethylene glycol and sodium hydrogen carbonate, and the diluted samples were filtered and cleaned up on an immunoaffinity column. OTA was eluted with methanol and quantified by reversed-phase liquid chromatography with fluorometric detection. Average recoveries from white wine, red wine, and beer ranged from 88.2 to 105.4% (at spiking levels ranging from 0.1 to 2.0 ng/mL), from 84.3 to 93.1% (at spiking levels ranging from 0.2 to 3.0 ng/mL), and from 87.0 to 95.0% (at spiking levels ranging from 0.2 to 1.5 ng/mL), respectively. Relative standard deviations for within-laboratory repeatability (RSDr) ranged from 6.6 to 10.8% for white wine, from 6.5 to 10.8% for red wine, and from 4.7 to 16.5% for beer. Relative standard deviations for between-laboratories reproducibility (RSDR) ranged from 13.1 to 15.9% for white wine, from 11.9 to 13.6% for red wine, and from 15.2 to 26.1% for beer. HORRAT values were ≤0.4 for the 3 matrixes.

Liquid Chromatographic Method for Determination of Iodine in Milk: Collaborative Study

1993 ◽  
Vol 76 (4) ◽  
pp. 711-719 ◽  
Author(s):  
David Sertl ◽  
William Malone ◽  
◽  
P Beljaars ◽  
C Blake ◽  
...  
Keyword(s):  
Membrane Filter ◽  
Collaborative Study ◽  
Reversed Phase ◽  
Powdered Milk ◽  
Insoluble Material ◽  
Relative Standard ◽  
Repeatability And Reproducibility ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract Nine laboratories participated in an AOAC International/ International Dairy Federation collaborative study on a liquid chromatographic (LC) method for determination of iodine in milk. Liquid milk is passed through a 25 000 MW membrane filter to remove protein and insoluble material. Iodine (in the form of iodide) in the clear filtrate is separated by reversed-phase ion-pair LC and is detected electrochemically. Participants analyzed 2 commercial pasteurized whole milks and 5 nonfat dry milk powders in blind duplicate. Each sample was tested in duplicate on 2 days. Repeatability and reproducibility standard deviations (sr and SR, respectively) and repeatability and reproducibility relative standard deviations (RSDr and RSDR, respectively) for determinations of iodine in whole milk (mean recovery, 86.7%) were as follows: sr, 22 μg/L; SR, 22 μg/L; RSDr, 8.2%; and RSDR, 8.3%. For powdered milk (mean recovery, 91 %), the values were as follows: sr, 0.14 μg/g; SR, 0.22 μg/g; RSDr, 9.0%; and RSDR, 12.7%. The method was adopted first action by AOAC International.

scholarly journals Determination of Naringin and Neohesperidin in Orange Juice by Liquid Chromatography with UV Detection to Detect the Presence of Grapefruit Juice: Collaborative Study

2000 ◽  
Vol 83 (5) ◽  
pp. 1155-1166 ◽  
Author(s):  
Wilbur Widmer ◽  
A Brause ◽  
E Coppola ◽  
K Daniels ◽  
R Feicht ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Orange Juice ◽  
Sodium Benzoate ◽  
Grapefruit Juice ◽  
Collaborative Study ◽  
Potassium Sorbate ◽  
Sour Orange ◽  
Relative Standard ◽  
Standard Deviations

Abstract Fifteen collaborating laboratories were sent 9 samples of citrus juice mixtures as blind duplicates for determination of naringin and neohesperidin by liquid chromatography. Two sample pairs were 100% orange juice and did not contain any naringin or neohesperidin. The remaining 7 sample pairs contained naringin at levels ranging from 3.9 to 46.5 ppm and neohesperidin at levels ranging from 0.14 to 35.6 ppm. Five sample pairs consisted of orange juice mixtures containing 1, 3, and 5% grapefruit juice; 5% sour orange; and 5% K-Early citrus variety. Two sample pairs were orange juice spiked with naringin, neohesperidin, sodium benzoate, and potassium sorbate. Data were received from 13 laboratories. Data from 1 collaborator were eliminated because the method protocol was not followed. Neohesperidin values from another laboratory were also not used because of problems with a coeluting component. Repeatability relative standard deviations ranged from 2.95 to 15.23% for naringin and from 3.00 to 11.74% for neohesperidin. Reproducibility relative standard deviations ranged from 11.34 to 31.94% for naringin and from 10.45 to 26.17% for neohesperidin. The method is reliable for detecting the presence of grapefruit juice in orange juice as indicated by a finding of ≥10 ppm naringin and ≤2 ppm neohesperidin. The method was adopted First Action by AOAC INTERNATIONAL.

Liquid Chromatographic Method for Determination of Glycerol in Wine and Grape Juice: Collaborative Study

1992 ◽  
Vol 75 (3) ◽  
pp. 379-383 ◽  
Author(s):  
Arthur Caputi ◽  
Eric Christensen ◽  
Nancy Biedenweg ◽  
Susan Miller
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Grape Juice ◽  
External Standard Method ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
External Standard ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract An Ion-exchange liquid chromatographic method for the determination of glycerol in wine, white grape juice, and pink grape juice was collaboratively studied by 8 laboratories. Eight wine types and 12 juice samples were provided to each collaborator. Using a strong cation column, blind duplicates and standards were analyzed by an external standard method. Separate statistical evaluations were run on wine, white grape juice, and pink grape juice data. The averages of the relative standard deviations for repeatability, excluding outlying results, were 1.25% for the wine samples, 7.32% for the white grape juice samples, and 8.63% for the pink grape juice samples. The averages of the relative standard deviations for reproducibility, excluding outlying results, were 2.79% for the wine samples, 16.97% for the white grape juice samples, and 19.10% for the pink grape juice samples. The method has been adopted first action by AOAC International.

scholarly journals Determination of Fumonisins B1 and B2 in Corn and Corn Flakes by Liquid Chromatography with Immunoaffinity Column Cleanup: Collaborative Study

2001 ◽  
Vol 84 (6) ◽  
pp. 1828-1838 ◽  
Author(s):  
Angelo Visconti ◽  
Michele Solfrizzo ◽  
Annalisa De Girolamo ◽  
H Bresch ◽  
P Burdaspal ◽  
...  
Keyword(s):  
Collaborative Study ◽  
Immunoaffinity Column ◽  
Relative Standard ◽  
Repeatability And Reproducibility ◽  
Double Extraction ◽  
Standard Deviations ◽  
Corn Flakes ◽  
Liquid Chromatographic ◽  
Fumonisins B1 And B2

Abstract A liquid chromatographic (LC) method for the determination of fumonisins B1 (FB1) and B2 (FB2) in corn and corn flakes was collaboratively studied by 23 laboratories, which analyzed 5 blind duplicate pairs of each matrix to establish the accuracy, repeatability, and reproducibility characteristics of the method. Fumonisin levels in the corn ranged from <0.05 (blank) to 1.41 μg/g for FB1 and from <0.05 to 0.56 μg/g for FB2, whereas in the corn flakes they ranged from <0.05 to 1.05 μg/g for FB1 and from <0.05 to 0.46 μg/g for FB2. The method involved double extraction with acetonitrile–methanol–water (25 + 25 + 50), cleanup through an immunoaffinity column, and LC determination of the fumonisins after derivatization with o-phthaldialdehyde. Relative standard deviations for the within-laboratory repeatability (RSDr) of the corn analyses ranged from 19 to 24% for FB1 and from 19 to 27% for FB2; for the corn flakes analyses, RSDr ranged from 9 to 21% for FB1 and from 8 to 22% for FB2. Relative standard deviations for the between-laboratories reproducibility (RSDR) of the corn analyses ranged from 22 to 28% for FB1 and from 22 to 30% for the FB2; for corn flakes analyses, RSDR ranged from 27 to 32% for FB1 and from 26 to 35% for FB2. Mean recoveries of FB1 and FB2 from corn spiked with FB1 at 0.80 μg/g and with FB2 at 0.40 μg/g were 76 and 72%, respectively; for corn flakes spiked at the same levels recoveries were 110 and 97% for FB1 and FB2, respectively. HORRAT ratios for the analyses of corn ranged from 1.44 to 1.53 for FB1 and from 0.96 to 1.48 for FB2, whereas for corn flakes they ranged from 1.60 to 1.82 for FB1 and from 1.39 to 1.68 for FB2.

scholarly journals Liquid Chromatographic Determination of Fumonisins B1, B2, and B3 in Corn: AOAC–IUPAC Collaborative Study

1996 ◽  
Vol 79 (3) ◽  
pp. 688-696 ◽  
Author(s):  
Eric W Sydenham ◽  
Gordon S Shephard ◽  
Pieter G Thiel ◽  
Sonja Stockenström ◽  
Petra W Snijman ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Relative Standard ◽  
Valid Data ◽  
Liquid Chromatographic Determination ◽  
Standard Deviations ◽  
The Individual ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method for simultaneous determination of fumonisins B1 (FB1), B2 (FB2), and B3 (FB3) in corn was subjected to a collaborative study involving 12 participants from 10 countries, in which the accuracy and reproducibility characteristics of the method were established. Mean analyte recoveries from corn ranged from 81.1 to 84.2% for FB1 (at a spiking range of 500 to 8000 ng/g), from 75.9 to 81.9% for FB2 (at a spiking range of 200 to 3200 ng/g), and from 75.8 to 86.8% for FB3 (at a spiking range of 100 to 1600 ng/g). The valid data were statistically evaluated after exclusion of outliers. Relative standard deviations for within-laboratory repeatability ranged from 5.8 to 13.2% for FB1, from 7.2 to 17.5% for FB2, and from 8.0 to 17.2% for FB3. Relative standard deviations for between-laboratory reproducibility varied from 13.9 to 22.2% for FB1, from 15.8 to 26.7% for FB2, and from 19.5 to 24.9% for FB3. HORRAT ratios, calculated for the individual toxin analogues, ranged from 0.75 to 1.73. The LC method for determination of fumonisins B1, B2, and B3 in corn (at concentrations of 800–12800 ng total fumonisins/g) has been adopted by AOAC INTERNATIONAL.

Simultaneous determination of 8 fluoroquinolone antibiotics in sewage treatment plants by solid-phase extraction and liquid chromatography with fluorescence detection

2009 ◽  
Vol 59 (4) ◽  
pp. 805-813 ◽  
Author(s):  
L. Shi ◽  
X. F. Zhou ◽  
Y. L. Zhang ◽  
G. W. Gu
Keyword(s):  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Fluorescence Detection ◽  
Solid Phase ◽  
Sewage Treatment ◽  
Gradient Elution ◽  
Ammonium Bromide ◽  
Sewage Treatment Plants ◽  
Relative Standard

Fluoroquinolones (FQs) are among the most important antibiotics used in human and veterinary medicines. A simple and effective analytical method based on reversed-phased liquid chromatography with fluorescence was developed and validated for the simultaneous determination of eight FQs in wastewater at trace level. Aqueous samples were extracted using AnpelTM MEP cartridges where they were subsequently eluted by formic acid in methanol. The aqueous extracts were analyzed by gradient elution Liquid Chromatography with Fluorescence Detection (LC–FLD), whose mobile phase was composed of acetonitrile and 10 mM tetrabutyl ammonium bromide (TBAB). The limits of detection (LOD) and the relative standard deviation (RSD) were as low as 0.11–1.06 μg/L and 2–5%, respectively. The presented method was successfully applied to quantify FQs in the influent and effluent of several typical Sewage Treatment Plants (STPs) in Shanghai. For the extraction of 100 mL influent and 500 mL effluent sewage water samples, recoveries obtained were between 79–109% and 80%–105%, respectively. 7 FQs were occurred and identified in the STPs with the concentrations varying from 7 ng/L to 1 μg/L. Norfloxacin, ciprofloxacin and lomefloxacin were the most frequently detected antibiotics occurring in the wastewaters. The analytical procedure developed may be used for more in-depth studies on the occurrences and the fate of these commonly used pharmaceuticals in the sewage treatment plants and in the aquatic environment.

Liquid Chromatographic Determination of Penicillin V Potassium in Tablets: Collaborative Study

1989 ◽  
Vol 72 (6) ◽  
pp. 883-884
Author(s):  
Barry Mopper
Keyword(s):  
Collaborative Study ◽  
Potassium Phosphate ◽  
Internal Standard ◽  
Photometric Detection ◽  
Penicillin V ◽  
Relative Standard ◽  
Repeatability And Reproducibility ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for the determination of penicillin V potassium in tablets was collaboratively studied by 7 laboratories. The method uses an octadecyl silane reverse-phase column, a mobile phase of acetonitrile-methanol-O.OlM potassium phosphate monobasic (21 + 4 + 75 v/v/v), photometric detection at 225 nm, and sulfadimethoxine as an internal standard. Each collaborator received 6 samples: powdered composites of 2 commercial tablet preparations and 1 synthetic tablet powder mixture, each with blind duplicates. The mean repeatability and reproducibility relative standard deviations for commercial samples were, respectively, 1.10 and 1.46% (250 mg dosage), and 0.84 and 2.82% (500 mg dosage). The average standard recovery from the synthetic formulation was 99.1%, with repeatability and reproducibility relative standard deviations of 1.30 and 3.66%, respectively. The method has been adopted official first action.

Sign in / Sign up

Export Citation Format

Share Document