scholarly journals Determination of Zearalenone in Cereal Grains, Animal Feed, and Feed Ingredients Using Immunoaffinity Column Chromatography and Liquid Chromatography: Interlaboratory Study

2007 ◽  
Vol 90 (6) ◽  
pp. 1610-1622 ◽  
Author(s):  
Harold M Campbell ◽  
J Fred Armstrong ◽  
K Aoyama ◽  
S Biselli ◽  
J Cea ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Column Chromatography ◽  
Animal Feed ◽  
Control Sample ◽  
The United States ◽  
Cereal Grains ◽  
Excitation Wavelength ◽  
Immunoaffinity Column ◽  
Feed Ingredients

Abstract A method using immunoaffinity column chromatography (IAC) and liquid chromatography (LC) for determination of zearalenone in cereal grains, animal feed, and feed ingredients was collaboratively studied. The test portion is extracted by shaking with acetonitrilewater (90 + 10, v/v) and sodium chloride. The extract is diluted and applied to an immunoaffinity column, the column is washed with water or phosphatebuffered saline or methanolwater (30 + 70, v/v), and zearalenone is eluted with methanol. The eluate is evaporated, the residue is dissolved in mobile phase and analyzed by reversed-phase LC with fluorescence detection. The presence of zearalenone can be confirmed using an alternate excitation wavelength or diode array detection. Twenty samples were sent to 13 collaborators (8 in Europe, 2 in the United States, one in Japan, one in Uruguay, and one in Canada). Eighteen samples of naturally contaminated corn, barley, wheat, dried distillers grains, swine feed, and dairy feed were analyzed as blind duplicates, along with blank corn and wheat samples. The analyses were done in 2 sample sets with inclusion of a spiked wheat control sample (0.1 mg/kg) in each set. Spiked samples recoveries were 89116, and for the 18 naturally contaminated samples, RSDr values (within-laboratory repeatability) ranged from 6.67 to 12.1, RSDR values (among-laboratory reproducibility) ranged from 12.5 to 19.7, and HorRat values ranged from 0.61 to 0.90.

scholarly journals Immunoaffinity Column Cleanup with Liquid Chromatography Using Post-Column Bromination for Determination of Aflatoxins in Hazelnut Paste: Interlaboratory Study

2005 ◽  
Vol 88 (2) ◽  
pp. 526-535 ◽  
Author(s):  
Hamide Z Senyuva ◽  
John Gilbert
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Aflatoxin B1 ◽  
The United States ◽  
Interlaboratory Study ◽  
Immunoaffinity Column ◽  
Test Portion ◽  
Relative Standard

Abstract An interlaboratory study was conducted to evaluate the effectiveness of an immunoaffinity column cleanup liquid chromatography (LC) method for determination of aflatoxin B1 and total aflatoxins in hazelnut paste at European regulatory limits. The test portion was extracted with methanol–water (6 + 4). The extract was filtered, diluted with phosphate-buffered saline (PBS) solution to a specified solvent concentration, and applied to an immunoaffinity column containing antibodies specific to aflatoxins. The aflatoxins were removed from the immunoaffinity column with methanol, and then quantified by reversed-phase LC with post-column derivatization (PCD) involving bromination. The PCD was achieved with electrochemically generated bromine (Kobra Cell®) followed by fluorescence detection (except for one participant who used pyridinum hydrobromide perbromide for bromination). Hazelnut paste, both naturally contaminated with aflatoxins and blank (<0.1 ng/g) for spiking by participants with aflatoxins, was sent to 14 collaborators in Belgium, The Netherlands, Spain, Turkey, the United Kingdom, and the United States. Test portions were spiked at levels of 4.0 and 10.0 ng/g for total aflatoxins by participants using supplied total aflatoxins standards. Recoveries for total aflatoxins and aflatoxin B1 averaged from 86 to 89%. Based on results for naturally contaminated samples (blind duplicates at 3 levels ranging from 4.0 to 11.8 ng/g total aflatoxins), the relative standard deviation for repeatability (RSDr) ranged from 2.3 to 3.4% for total aflatoxins and from 2.2 to 3.2% for aflatoxin B1. The relative standard deviation for reproducibility (RSDR) ranged from 6.1 to 7.0% for total aflatoxins and from 7.3 to 7.8% for aflatoxin B1. The method showed exceptionally good within-laboratory and between-laboratory precision for hazelnut paste, as evidenced by HORRAT values, which in all cases were significantly below target levels, the low levels of determination for both aflatoxin B1 and total aflatoxins.

Determination of Deoxynivalenol in Infant Cereal by Immunoaffinity Column Cleanup and High-Pressure Liquid Chromatography–UV Detection†

2010 ◽  
Vol 73 (6) ◽  
pp. 1073-1076 ◽  
Author(s):  
MARY ANN DOMBRINK-KURTZMAN ◽  
STEPHEN M. POLING ◽  
DAVID F. KENDRA
Keyword(s):  
High Pressure ◽  
Liquid Chromatography ◽  
High Pressure Liquid Chromatography ◽  
Primary Source ◽  
The United States ◽  
Immunoaffinity Column ◽  
European Standard ◽  
Low Concentrations ◽  
Wheat Products

The presence of deoxynivalenol (DON) in cereal-based baby food, a primary source of the first solid food for infants, was studied in order to develop a method to detect its presence at low concentrations. DON, produced primarily by Fusarium graminearum, is commonly isolated from grains and feed around the world and affects both animal and human health, producing diarrhea, vomiting, gastrointestinal inflammation, and immunomodulation. An aqueous extract of infant cereal was cleaned by means of an immunoaffinity chromatography column. After the eluate was evaporated and redissolved, DON was determined by high-pressure liquid chromatography–UV. The level of quantification for DON was 10 ppb for three types of infant cereal (mixed, barley, and oatmeal); the level of detection was 5 ppb. The protocol we have developed can measure DON between 10 to 500 ppb. An advisory level of 1 ppm for wheat products has been established by the U.S. Food and Drug Administration; however, the European Communities (EC) regulations have been set at 200 ppb for cereal-based foods for infants. Only 1 of 52 samples of barley-, mixed-, or oat-based infant cereal purchased in 2008 and 2009 in the United States exceeded the European standard.

Determination of Ochratoxin A in Animal Feed and Cereal Grains by Liquid Chromatography with Fluorescence Detection

1986 ◽  
Vol 69 (6) ◽  
pp. 957-959 ◽  
Author(s):  
Huguette Cohen ◽  
Michel Lapointe
Keyword(s):  
Acetic Acid ◽  
Liquid Chromatography ◽  
Ochratoxin A ◽  
Fluorescence Detection ◽  
Animal Feed ◽  
Cereal Grains ◽  
Fluorescence Detector ◽  
Animal Feeds ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method is described for determination of ochratoxin A in animal feeds and cereal grains. Samples are initially extracted with chloroform-ethanol (8 + 2) and 5% acetic acid in water. Extracts are purified using a silica gel cartridge followed by a cyano cartridge. The samples are evaporated, diluted to a known volume, and analyzed using a 10 cm column of 3 μm Cm and a fluorescence detector. The method was applied to a variety of animal feeds and cereal grains at levels of 1.0-0.005 ppm added ochratoxin A. The overall recovery was 90.6% ± 3.6.

Immunoaffinity Column Coupled with Solution Fluorometry or Liquid Chromatography Postcolumn Derivatization for Determination of Aflatoxins in Corn, Peanuts, and Peanut Butter: Collaborative Study

1991 ◽  
Vol 74 (1) ◽  
pp. 81-88 ◽  
Author(s):  
Mary W Trucksess ◽  
Michael E stack ◽  
Stanley Nesheim ◽  
Samuel W Page ◽  
Richard H Albert ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Peanut Butter ◽  
Collaborative Study ◽  
The United States ◽  
Affinity Column ◽  
Immunoaffinity Column ◽  
Relative Standard

Abstract An AOAC/IUPAC (International Union of Pure and Applied Chemistry) collaborative study was conducted to evaluate the effectiveness of an immunoaffinity column for the determination of af latoxin. The test portion Is extracted with methanol- water (7 + 3), filtered, diluted to ⦟30% methanol with water, and applied to the affinity column. The column Is washed with water and the concentrated aflatoxins are eluted with methanol. Total aflatoxins are determined by solution fluorometry with bromine (SFB), and Individual toxins are determined by reverse-phase liquid chromatography with postcolumn derlvatizatlon with Iodine (PCD). Corn naturally contaminated with aflatoxins, and peanuts, peanut butter, and corn containing added aflatoxins ( B1:B2:G1G2 = 7:1:3:1) were sent to 24 collaborators In the United States, France, Canada, and the Republic of South Africa. Twelve collaborators used the SFB method, 9 used the PCD method, and 3 used both SFB and PCD methods. Twenty collaborators completed the study (10 used the SFB method, 7 used the PCD method, and 3 used both SFB and PCD methods). Test portions were spiked at 10, 20, and 30 ng/g. For SFB analyses, recoveries of total aflatoxins were 123,105, and 107%, respectively; the relative standard deviation for repeatability (RSDr) ranged from 11.75 to 16.57%, and the relative standard deviation for reproducibility (RSDR) ranged from 10.97 to 33.09%. For PCD analyses, recoveries were 81, 81, and 83%, respectively; the RSDr ranged from 5.20 to 17.22%, and the RSDR ranged from 4.68 to 50.77%. The RSDr for aflatoxins B1, and G1 for spiked test portions ranged from 5.45 to 23.55%, and the RSDR ranged from 4.21 to 57.28%. The RSDr and RSDR for aflatoxins B2 and G2 were higher because of the small amounts added. Analyses by both SFB and PCD methods showed acceptable within-laboratory and betweenlaboratories precision. The method has been adopted official first action by AOAC as an AOAC-IUPAC method.

scholarly journals Liquid Chromatographic Method for the Quantification of Zearalenone in Baby Food and Animal Feed: Interlaboratory Study

2007 ◽  
Vol 90 (6) ◽  
pp. 1598-1609 ◽  
Author(s):  
Isabel Arranz ◽  
Carsten Mischke ◽  
Joerg Stroka ◽  
Eric Sizoo ◽  
Hans van Egmond ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Animal Feed ◽  
Baby Food ◽  
Excitation Wavelength ◽  
Immunoaffinity Column ◽  
Average Value ◽  
Sample Extract ◽  
Relative Standard

Abstract An interlaboratory trial for determination of zearalenone (ZON) in baby food and animal feed was conducted. The study involved 39 participants in 16 European Union member states, as well as Turkey, Uruguay, and China, representing a cross-section of industry, and official food control and research institutes. The method is based on immunoaffinity column cleanup followed by high-performance liquid chromatography using fluorimetry (HPLC-Fl). The test portion of the sample is extracted with methanolwater (75 + 25, v/v). The sample extract is filtered, diluted, and passed over an immunoaffinity column. ZON is eluted with methanol. The separation and determination of ZON is performed by reversed-phase HPLC-Fl with an excitation wavelength of 274 nm and an emission wavelength of 446 nm. Test portions of the samples were spiked at levels of 20 and 30 g/kg ZON in baby food and at levels of 100 and 150 g/kg ZON in animal feed. Mean recoveries from each participant ranged from 78 to 119 with an average value of 92 for baby food and from 51 to 122 with an average value of 74 for animal feed. Based on results for spiked samples (blind duplicates at 2 levels), as well as naturally contaminated samples (blind duplicates at 3 levels), the relative standard deviation for repeatability (RSDr) in baby food ranged from 2.8 to 9.0. For animal feed, this value ranged from 5.7 to 9.5. The relative standard deviation for reproducibility (RSDR) in baby food ranged from 8.2 to 13.3, and for animal feed this value ranged from 15.5 to 21.4. The Horwitz ratio (HorRat) in baby food ranged from 0.3 to 0.4, and for animal feed this value ranged from 0.6 to 0.9. The method showed acceptable within-and between-laboratory precision for each matrix, as required by European legislation.

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