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Published on: August 5, 2016
Determination of polycyclic aromatic hydrocarbons in infant formula using solid state urea clathrate formation with
Zoltán Nyiri1, Márton Novák1, Zsolt Bodai1
1Joint Research and Training Laboratory on Separation Techniques, Institute of Chemistry, Eötvös Loránd University, Pázmány Péter stny. 1/A, H-1117 Budapest, Hungary.
Insights
A new method accurately quantifies 16 EU priority polycyclic aromatic hydrocarbons (PAHs) in infant formula using gas chromatography-tandem mass spectrometry. This ensures infant formula safety by meeting stringent European Commission limits.
Area of Science:
- Analytical Chemistry
- Food Safety Analysis
- Environmental Health
Background:
- Polycyclic Aromatic Hydrocarbons (PAHs) are environmental contaminants.
- Infant formula requires rigorous safety testing for contaminants like PAHs.
- European Union (EU) regulations set strict limits for PAHs in foodstuffs.
Purpose of the Study:
- To develop and validate a quantitative analytical method for 16 EU priority PAHs in infant formula.
- To establish reliable detection and quantification limits for PAHs in infant formula.
- To ensure infant formula complies with European Commission regulations.
Main Methods:
- Sample preparation involved PAH extraction, triglyceride transesterification to fatty acid methyl esters (FAMEs), and FAME removal via urea clathrate formation.
- Quantitative analysis was performed using gas chromatography-tandem mass spectrometry (GC-MS/MS).
- Method validation included assessment of trueness, precision, LOD, LOQ, selectivity, sensitivity, and linearity.
Main Results:
- The method achieved a measurement range of 200-1500 ng/kg, aligning with EU limits.
- Limit of detection (LOD) ranged from 50-75 ng/kg for the 16 PAHs.
- Limit of quantification (LOQ) was 200 ng/kg for all 16 PAHs, with trueness between -29.7% and 29.8% and precision (RSD) between 0.5% and 24.7%.
Conclusions:
- A robust analytical method for determining 16 EU priority PAHs in infant formula has been successfully developed.
- The method's validated parameters demonstrate its suitability for routine monitoring and regulatory compliance.
- This contributes to enhanced infant safety by ensuring the quality of infant formula.
Abstract:
An analytical method has been developed for the quantitative determination of the 16 EU priority polycyclic aromatic hydrocarbons (PAHs) in infant formula. Prior to analysis infant formula is subjected to sample preparation including the extraction of PAHs from the sample, transesterification of the triglyceride content of the extract to fatty acid methyl esters (FAMEs), and solid state urea clathrate formation to remove the FAMEs. Measurements were carried out with gas chromatography - tandem mass spectrometry. The developed method has been evaluated in terms of trueness, precision (repeatability), limit of detection (LOD), limit of quantification (LOQ), selectivity, sensitivity and linearity. Measurement range of 200-1500ngkg-1 was selected in accordance with the limit values set by the European Commission (835/2011/EC). LOD values were 75ngkg-1 for dibenzo(a,e)pyrene, dibenzo(a,i)pyrene and dibenzo(a,h)pyrene while 50ngkg-1 for the rest of the PAHs (benzo(c)fluorene, benzo(a)anthracene, cyclopenta(cd)pyrene, chrysene, 5-methylchrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(j)fluoranthene, benzo(a)pyrene, indeno(1,2,3-cd)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene, dibenzo(a,l)pyrene), LOQ was 200ngkg-1 for all 16 PAHs. Trueness ranged between -29.7 and 29.8% while precision values were between 0.5 and 24.7% (RSD, n=3).
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