The growing demands of milk and milk products necessitated the use of various kinds of chemicals including antibiotics, urea, and hormones. Although they are essential in the bulk production of milk, they can pose serious health issues not only to animals but also to consumers. To identify and quantify various contaminants (e.g., antibiotics, pesticides, and polycyclic aromatic hydrocarbons) in milk and its related products, it is desirable to establish reliable means for instrumental detection. This review was organized to summarize the analytical techniques currently available for the identification and quantification of contaminants in milk and dairy products. To this end, this review emphasizes the compositional diversity of various contaminants in milk and its products. This study thus aims to provide valuable insights into the essential protocols for the quantification of dairy-related contaminants while helping make the fast and firm decisions needed for the legislation, regulations, and health care.

Quantification techniques for important environmental contaminants in milk and dairy products

Immunoassay of chemical contaminants in milk: A review

This study aimed to develop an efficient, sensitive, and reliable analytical method for trace analysis of 17 different pyrethroids and chlorpyrifos in the fatty content of animal products, including beef, chicken, eggs, fish, and milk. The method developed is based on an ultrasound extraction using lyophilized samples, a solid phase extraction cleanup with basic alumina and C18 cartridges in tandem, and analysis by gas chromatography coupled to tandem mass spectrometry in negative chemical ionization mode. Recovery values were in the range of 27–128 % with relative standard deviation always below 25 %, and chiral analysis of recovery data showed predominance of isomers of cis form over trans. Limits of detection (LODs) ranged from 0.002 to 6.43 ng g−1 lipid weight (lw), and limits of quantification (LOQs) ranged between 0.006 and 21.4 ng g−1 lw. The developed methodology was used for the analysis of 25 samples of fatty foods. All samples were positive for at least one of the pesticides, chlorpyrifos, bifenthrin, cyhalothrin, permethrin, cypermethrin, or deltamethrin, with mass fraction levels ranging from 0.03 to 270 ng g−1 lw.

Methodology for trace analysis of 17 pyrethroids and chlorpyrifos in foodstuff by gas chromatography–tandem mass spectrometry

https://escholarship.org/content/qt5mn824ct/qt5mn824ct.pdf?t=pdyiz7

Magnetic effervescent tablets containing ionic liquids as a non-conventional extraction and dispersive agent for determination of pyrethroids in milk.

https://digital.csic.es/bitstream/10261/219417/1/1-s2.0-S0278691518301777-main.pdf

Residue of insecticides in foodstuff and dietary exposure assessment of Brazilian citizens.

A simple and inexpensive method based on solvent extraction followed by low temperature clean-up was applied for determination of seven pyrethroids residues in bovine raw milk using gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) and gas chromatography with electron-capture detector (GC-ECD). Sample extraction procedure was established through the evaluation of seven different extraction protocols, evaluated in terms of analyte recovery and cleanup efficiency. Sample preparation optimization was based on Doehlert design using fifteen runs with three different variables. Response surface methodologies and polynomial analysis were used to define the best extraction conditions. Method validation was carried out based on SANCO guide parameters and assessed by multivariate analysis. Method performance was considered satisfactory since mean recoveries were between 87% and 101% for three distinct concentrations. Accuracy and precision were lower than ±20%, and led to no significant differences (p < 0.05) between results obtained by GC-ECD and GC-MS/MS techniques. The method has been applied to routine analysis for determination of pyrethroid residues in bovine raw milk in the Brazilian National Residue Control Plan since 2013, in which a total of 50 samples were analyzed.

/pdf/multivariate-optimization-for-extraction-of-pyrethroids-in-13rrz5sx2f.pdf

Amanda Ceccon

Papers

Multivariate Optimization for Extraction of Pyrethroids in Milk and Validation for GC-ECD and CG-MS/MS Analysis