Evaluation of measurement uncertainties of an analytical method for the determination of aflatoxin M1 in milk and milk powder

Abstract A liquid chromatographic method for determining low aflatoxin M1 concentrations in milk was evaluated in an International Dairy Federation (IDF) interlaboratory study. The study involved 16 participants from 11 countries. The method, chosen after a comparison of several methods by a preparatory group, uses an immunoaffinity column for cleanup. As the sample passes through the column, antibodies selectively bind with aflatoxin M1 (antigen) present and form an antibody-antigen complex. All other components of the sample matrix are washed off the column with water. Then, aflatoxin M1 is eluted from the column with acetonitrile, which is collected. Final determination is carried out by reversed-phase liquid chromatography with fluorescence detection. Over the tested range (80-600 ng aflatoxin M1/kg milk powder), an RSDR ranging from 11 to 23% was obtained by analyzing 24 samples (blind duplicates), 2 samples of which were blanks.

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Determination of Aflatoxin M1 in Milk Powder by Ultrasonic-Assisted Extraction and Dispersive Solid-Phase Clean-up

Journal of Chromatographic Science ◽

10.1093/chromsci/bmu131 ◽

2014 ◽

Vol 53 (6) ◽

pp. 1000-1006 ◽

Cited By ~ 7

Author(s):

M. Manoochehri ◽

A. A. Asgharinezhad ◽

M. Safaei

Keyword(s):

Solid Phase ◽

Milk Powder ◽

Aflatoxin M1 ◽

Assisted Extraction ◽

Ultrasonic Assisted ◽

Ultrasonic Assisted Extraction

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Determination of aflatoxin M1 in milk and milk powder using immuno-affinity column and fluorescence measurement

Journal of Food and Drug Analysis ◽

10.38212/2224-6614.2989 ◽

2020 ◽

Vol 4 (2) ◽

Author(s):

Y.-M. Fu

Keyword(s):

Milk Powder ◽

Aflatoxin M1 ◽

Affinity Column ◽

Fluorescence Measurement

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A simple method for the fluorodensitometric determination of aflatoxin M1 in milk powder

Microchemical Journal ◽

10.1016/0026-265x(85)90026-8 ◽

1985 ◽

Vol 31 (2) ◽

pp. 170-172 ◽

Cited By ~ 3

Author(s):

G.S. Vasilikiotis ◽

I.N. Papadoyannis

Keyword(s):

Milk Powder ◽

Aflatoxin M1 ◽

Simple Method

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Ultra-trace determination of sodium fluoroacetate (1080) as monofluoroacetate in milk and milk powder by GC-MS/MS and LC-MS/MS

Analytical Methods ◽

10.1039/c8ay00767e ◽

2018 ◽

Vol 10 (28) ◽

pp. 3514-3524 ◽

Cited By ~ 1

Author(s):

Yiu-Tung Wong ◽

Wing-Ki Law ◽

Shirley Sau-Ling Lai ◽

Siu-Pan Wong ◽

Kong-Chi Lau ◽

...

Keyword(s):

Analytical Method ◽

Milk Powder ◽

Trace Determination ◽

Ultra Trace

A sensitive analytical method based on derivatization with 3-nitroaniline is established for the trace determination of sodium fluoroacetate (1080) in milk and milk powder.

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Method for the Determination of Aflatoxin M1 in Fluid Milk and Milk Products

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/56.6.1431 ◽

1973 ◽

Vol 56 (6) ◽

pp. 1431-1436 ◽

Cited By ~ 2

Author(s):

Walter A Pons ◽

Alva F Cucullu ◽

Louise S Lee

Keyword(s):

Neutral Lipids ◽

Milk Powder ◽

Aflatoxin M1 ◽

Reliable Determination ◽

Milk Products ◽

Average Recovery ◽

Acetone Water ◽

Freeze Dried ◽

Fluid Milk

Abstract The method described utilizes acetone-water (77+23) for extraction of M1 from milk and milk products in a 3 min blender extraction. Phospholipids and soluble proteins in the primary extract are removed by treatment with lead acetate, and residual neutral lipids in the treated extract are removed by partition into hexane. Aflatoxin M1 is partitioned into chloroform, which is then washed with salt solution, and the chloroform is evaporated. The residue is dissolved in chloroform, and M1 is resolved on silica gel-coated plates developed in chloroform-acetone-2-propanol (850+100+50). This basic procedure is applicable to fluid milk and reconstituted freeze-dried milk powder at levels as low as 0.1 μg M1/L. Extracts of nonfat dry milk, evaporated and condensed milk, and cheeses, which require further cleanup before TLC, are purified on a cellulose-aqueous methanol partition column to allow reliable determination of M1 at levels as low as 0.2 Mg/L or kg. Average recovery of M1 added to fluid milk at levels of 0.1–1.0 μg/L was 106% without the use of the cleanup column and 90% when the column was used to purify the extracts. Average recovery of M1 added to other milk products at a level of 0.2 Mg/L or kg was 88%. The precision of the method (coefficient of variation) was estimated to be ±16% at 0.2 Mg/L in fluid milk, and ±4% at a 34 Mg/kg level in contaminated freeze-dried milk.

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Development of Milk Powder Reference Materials Certified for Aflatoxin M1 Content (Part I)

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/70.4.605 ◽

1987 ◽

Vol 70 (4) ◽

pp. 605-610 ◽

Cited By ~ 1

Author(s):

Hans P Van Egmond ◽

Peter J Wagstaffe

Keyword(s):

Reference Material ◽

Reference Materials ◽

Extraction Efficiency ◽

Milk Powder ◽

Aflatoxin M1 ◽

Sources Of Error ◽

Content Part

Abstract The development of 3 full-cream milk powder reference materials, certified for their aflatoxin M1 content, is described. The materials were prepared and certified within the Reference Material Programme of the Community Bureau of Reference (BCR). The 3 reference materials, RMs 282, 284, and 285, contain aflatoxin M1 at concentrations of <0.05, 0.31 ± 0.06, and 0.76 ± 0.05 μg/kg, respectively. The preparation, testing for homogeneity, stability of the reference materials, and the certification exercise, which was preceded by 2 intercomparisons of methods, are discussed. Particular emphasis was placed on the independence of the measurements in the certification exercise and the control of errors associated with extraction efficiency and the aflatoxin M1 calibrant. Finally, some guidance is given on avoiding the principal sources of error in the determination of aflatoxin M1. Details concerning the supply of the reference materials will be provided by BCR on request.

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