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Between 2013 and 2015, an estimated 9.2 billion pounds of milk powder (MP) were produced. Such a large number highlights the importance of these products in the diet of the general population, as they contain important nitrogen-rich proteins.
In order to pass quality assurance (QA) testing, certain organizations add compounds with high nitrogen content to these products. This fraudulent process allows companies to increase profits by adding proteins with lower nitrogen content to their products. This process can have dangerous consequences. In 2008, melamine was added to MP, resulting in poor health of 300,000 people and death of 6 babies.
Since only specific compounds were screened at this time, these MPs can pass QA because melamine is an unknown adulterant. Since then, the food safety industry has adopted non-targeted technologies to identify unknown and known adulterants.
This viewing angle uses chemometric techniques, such as Raman spectroscopy and infrared (NIR) spectroscopy, to analyze multiple real samples and generate a reference set.
Then determine the variance and calculate the confidence limit to classify the unknown sample as unqualified or true. Even small changes between data points can be used to detect adulteration using Concordance Index (CI) analysis.
A recent proof-of-concept study showed that the combination of solution-state 1H NMR spectroscopy and CI analysis can provide non-targeted detection of multiple MP adulterants. This method also has the advantages of high sample throughput, high sensitivity and minimal sample preparation.
A Bruker Avance III 600 MHz spectrometer was used to test authentic MP samples from 46 international sources to generate a reference set. The variance of the data was determined by CI analysis, and a maximum CI (MaxCI) limit of ≥7.38 was established. Then various adulterants were investigated, and any samples with MaxCI ≥ 7.38 were classified as nonconforming products.
This technology is highly sensitive to the small nitrogen-rich organic molecules dicyandiamide (DCD) and melamine that are harmful to human health. Each of these compounds has a peak in an area not obscured by the MP signal (5.95 ppm and 6.58 ppm, respectively), which can identify concentrations of 0.005% w/w and 0.05% w/w, respectively.
It also evaluated adulterants that do not pose a significant risk to health. Maltodextrin and sucrose also contain signals in areas lacking MP metabolite peaks (5.16 ppm and 5.46–5.47 ppm, respectively), and can be detected at concentrations as low as 0.5% w/w.
Ammonium sulfate (5% w/w) and urea (0.5% w/w) have also been identified, but the technique is less sensitive because these dopants do not contain peaks in unobstructed areas. Although protein adulterants were investigated, they could not be detected due to their poor solubility in DMSO.
Compared with non-targeted technologies that combine Raman and NIR, the sensitivity achieved when detecting dangerous adulterated melamine is much higher, indicating that this method has great prospects in the QA of MP.
Bruker BioSpin provides the world's most comprehensive NMR and EPR spectroscopy and preclinical research tools. Bruker BioSpin develops, manufactures and supplies technologies for research institutions, commercial enterprises and multinational companies in countless industries and professional fields.
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Last update: November 23, 2021 at 10:33 am
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