This is an outdated version published on 2023-06-12. Read the most recent version.

Single step fractionation of raw milk with FraMiTrACR® prior to detection of the residual contaminants chlorate and perchlorate

Authors

Keywords:

Milk, Raw Milk, Chlorate, Perchlorate, Sample Preparation, Fractionation, LC-MS/MS

Abstract

Residues of chlorate and perchlorate in dairy products are causing challenges for stakeholders in the dairy food chain. Both residues enter the dairy food chain almost exclusively as a disinfection or cleaning by-product. As these substances can endanger food safety, a cost-effective, passive and rapid raw milk sample preparation workflow was developed. By means of centrifugal ultrafiltration, unprocessed raw milk was fractionated into its constituent phases (water and fat/protein), using a FraMiTrACR®° unit. When the water phase prepared by this method was analyzed by liquid chromatography with tandem mass spectrometry (LC-MS/MS), it was possible to achieve quantification and detection levels of 0.001 mg/kg and 0.0005 mg/kg, respectively, for perchlorate, and quantification and detection levels of 0.01 mg/kg and 0.005 mg/kg, respectively, for chlorate.

References

Metrohm Application Note AN-PAN-1046: Online determination of anionic impurities in 50% NaOH and KOH. Process ion chromatography according to ASTM E1787, 1-3

McCarthy WP, O’Callaghan TF, Danahar M, Gleeson D, O’Connor, C, Fenelon MA, Tobin JT: Chlorate and Other Oxychlorine Contaminants Within the Dairy Supply Chain. Comprehensive Reviews in Food Science and Food Safety Vol.17,2018, 1561-1575

Kirk AB, Smith EE, Tian K, Anderson TA, Dasgupta PK: Perchlorate in Milk. Enviromental Science Technology 2003, 37, 21, 4979–4981.

COMMISSION REGULATION (EU) 2020/749 of 4 June 2020 amending Annex III to Regulation (EC) No 396/2005 of the European Parliament and of the Council as regards maximum residue levels for chlorate in or on certain products

COMMISSION REGULATION (EU) 2020/685 of 20 May 2020 amending Regulation (EC) No 1881/2006 as regards maximum levels of perchlorate in certain foods

European Food Safety Authority: Scientific Opinion on the risks to public health related to the presence of perchlorate in food, in particular fruits and vegetables. EFSA Journal 2014;12(10):3869, 117 pp.

German Federal Institute for Risk Assesment: Frequently asked questions about perchlorate in food. Frequently asked questions about chlorate in food. BfR FAQ of 15 February 2018,1-3

Anastassiades M, Wachtler A-K, Kolberg DI, Eichhorn E, Benkenstein A, Zechmann S, Mack D, Barth A, Wildgrube C, Sigalov I, Görlich S, Dörk D, Cerchia G: Quick Method for the Analysis of Numerous Highly Polar Pesticides in Food Involving Extraction with Acidified Methanol and LC MS/MS Measurement II. Food of Animal Origin (QuPPe AO Method). EU Reference Laboratory for pesticides requiring Single Residue Methods (EURL-SRM), 1-24

Dyke JV, Kirk AB, Martinelango PK, Dasgupta PK: Sample processing method for the determination of perchlorate in milk. Analytica Chimica Acta 567 (2006), 73–78

DIN ISO 11352:2013: Wasserbeschaffenheit - Abschätzung der Messunsicherheit beruhend auf Validierungs- und Kontrolldaten

Lieck G: Nachweisgrenze und Rauschen. LaborPraxis, Juni 1998, 62-67

EU Reference Laboratories for Residues of Pesticides: Analytical quality control and method validation procedures for pesticide residues analysis in food and feed - SANTE/2021/11312, 1-57 https://www.eurl-pesticides.eu/userfiles/file/EurlALL/SANTE_11312_2021.pdf

Downloads

Published

2023-06-06 — Updated on 2023-06-12

Versions