Principal component analysis of molecularly based signals from infant formula contaminations using LC-MS and NMR in foodomics.

BACKGROUND: The challenge in developing analytical assessment of unexpected excess contaminations in infant formula has been the most significant project to address the widespread issue of food safety and security. Foodomics based on metabolomics techniques provides powerful tools for the detection of tampering cases with intentional contaminations. However, the safety and risk assessments of infant formula to reveal not only the targeted presence of toxic chemicals, but also molecular changes involving unexpected contaminations, have not been reported. In this study, a huge amount of raw molecularly based signals from infant formula was analysed using reversed phase and hydrophilic interaction chromatography with time-of-flight MS (LC-MS) and (1) H nuclear magnetic resonance (NMR) and then processed by a principal component analysis (PCA). RESULTS: PCA plots visualised signature trends in the complex signal-data batches from each excess contamination of detectable chemicals by LC-MS and NMR. These trends in the different batches from a portion of excess chemical contaminations such as pesticides, melamine and heavy metals and out-of-date products can be visualised from spectrally discriminated infant formula samples. CONCLUSION: PCA plots provide possible attempts to maximise the covariance between the stable lot-to-lot uniformity and excess exogenous contaminations and/or degradation to discriminate against the molecularly based signals from infant formulas. © 2015 Society of Chemical Industry.

Metabolomics approach of infant formula for the evaluation of contamination and degradation using hydrophilic interaction liquid chromatography coupled with mass spectrometry.

In this study including the field of metabolomics approach for food, the evaluation of untargeted compounds using HILIC-ESI/TOF/MS and multivariate statistical analysis method is proposed for the assessment of classification, contamination and degradation of infant formula. HILIC mode is used to monitor more detected numbers in infant formulas in the ESI-positive scan mode than the reversed phase. The repeatability of the non-targeted contents from 4 kinds of infant formulas based on PCA was less than the relative standard deviation of 15% in all groups. The PCA pattern showed that significant differences in the classification of types and origins, the contamination of melamine and the degradations for one week were evaluated using HILIC-ESI/TOF/MS. In the S-plot from the degradation test, we could identify two markers by comparison to standards as nicotinic acid and nicotinamide. With this strategy, the differences from the untargeted compounds could be utilized for quality and safety assessment of infant formula.

Quantitative determination of total L-carnitine in infant formula, follow-up formula, and raw materials by liquid chromatography with tandem mass spectrometry.

We developed a rapid and useful routine screening assay for total L-carnitine content in various infant formulas and materials by liquid chromatography coupled with a tandem mass spectrometric method (LC-MS/MS) and alkaline hydrolysis. For separation of L-carnitine, a multi-mode octadecylsilane (ODS) column was used that contained ODS ligands, anion ligands, and cation ligands to avoid using ion-pairing agents. The stable isotope L-carnitine-d3 (m/z 165 → 103/85) was used in electrospray MS/MS in the multiple reaction monitoring mode with the ion transitions of m/z 162 → 103/85 for detection and quantitation of L-carnitine. Alkaline hydrolysis of short/medium chain (C2 - C15) acyl-L-carnitines in infant formula was analyzed by LC with quadrupole time-of-flight mass spectrometry (QTOF-MS). The majority of short/medium chain acyl-L-carnitines were hydrolyzed to free L-carnitine. The overall standard deviations for L-carnitine in infant formula, follow-up formula and raw materials ranged from 2.1 to 4.0. The overall mean recoveries ranged from 90.2 to 94.2%.