Institut für Lebensmittelchemie

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Analysis of acrylamide in vegetable chips after derivatization with 2-mercaptobenzoic acid by liquid chromatography–mass spectrometry
(2022) Oellig, Claudia; Gottstein, Eva; Granvogl, Michael
Since many years, acrylamide (AA) is a well-known toxicologically relevant processing contaminant (“food-borne toxicant”). However, only during the recent years, high levels of acrylamide have been reported in vegetable chips. In the present study, AA was quantitated via a modified derivatization procedure with 2-mercaptobenzoic acid based on stable isotope dilution analysis and liquid chromatography–mass spectrometry. Extraction with a modified QuEChERS (quick, easy, cheap, efficient, rugged, safe) method, defatting with n -hexane, and a solid phase extraction clean-up with strong cation-exchange material were performed prior to the derivatization step. Limits of detection and quantitation (LoD and LoQ) were 12 and 41 µg of AA/kg of vegetable chips (estimated via signal-to-noise ratios of 3:1 and 10:1, respectively), and thus below the LoQ of 50 µg/kg requested by the European Food Safety Authority. Recovery rates between 92 and 101% at four spiking levels with a good precision expressed as a relative standard deviation < 7% were determined. With this method at hand, a survey of the current AA amounts in 38 vegetable chips from the worldwide market was performed, showing a remarkable variability between the different vegetables, but also between different products of the same vegetable. Thereby, the AA amounts ranged between 77.3 and 3090 µg/kg, with an average of 954 µg/kg which was distinctly higher in comparison to commercially available potato chips also analyzed in the present study (12 samples, range: 117–832 µg/kg, average: 449 µg/kg). While for sweet potato and parsnip relatively low AA amounts were found, beetroot and carrot showed rather high contents.
Effect of relative humidity on the thin-layer chromatographic separation of E 472 emulsifiers
(2023) Schuster, Katharina; Oellig, Claudia
E 472 emulsifiers are organic acid esters of mono- and diacylglycerides. These emulsifiers are categorized into six subgroups (E 472a-f) based on the specific acid component, e.g., acetic acid, lactic acid, citric acid, tartaric acid, or mixtures of tartaric and acetic acid. The present study investigated the effect of relative humidity (RH) on the thin-layer chromatographic separation of four E 472 emulsifier subgroups, addressing practical concerns due to RH variations between seasons and within laboratories. Three RH-setting techniques affecting plate activity and chamber climate were assessed using saturated salt and aqueous sulfuric acid solutions. Aqueous sulfuric acid solutions for RH adjustment resulted in decreased hRF values, while no trends in hRF value changes were observed for saturated salt solutions. Unlike RH itself, the RH setting technique led to substantial changes in the chromatographic fingerprint. Thus, the choice of the RH setting method should be tailored to the specific analyte and analysis goal. Despite variations in chromatographic fingerprints between the three RH setting techniques, the fingerprint remained consistent within the same technique across the tested RH range.
Enzymatically formed fatty acid hydroperoxides determined through GC‐MS analysis of enantiomeric excess of hydroxy fatty acids after reduction and ibuprofen derivatization
(2025) Hotz, Lisa; Zartmann, Anne; Noack, Isabelle; Drees, Luca J.; Kuschow, Meret K.; Heinrich, Markus R.; Janssen, Hans‐Gerd; Hammann, Simon
Unsaturated fatty acids are susceptible to lipid oxidation through autoxidation, photooxygenation or enzymatical oxidation. A characteristic feature of enzyme‐catalyzed oxidation is the high regio‐ and stereospecificity of the formed fatty acid hydroperoxides. In this study, we present a method to quantify enzymatic lipid oxidation through reducing hydroperoxy fatty acid methyl esters to hydroxy fatty acid methyl esters and derivatizing them with enantiopure (S)‐ibuprofen, allowing the resolution of the enantiomer pairs as diastereomers via achiral GC‐MS. After application to enantiopure reference fatty acids, the approach was applied to autoxidation products of linoleic acid, and the expected racemic mixtures of the 9‐ and 13‐hydroperoxide derived hydroxy fatty acids were detected. On the other hand, when linoleic acid was oxidized using soybean lipoxygenase, clear enantiomeric excess of the (13S) enantiomer could be detected, proving the applicability of this method to detect enzymatic oxidation through enantiomeric excess.
GC/EI-MS method for the determination of phytosterols in vegetable oils
(2021) Schlag, Sarah; Huang, Yining; Vetter, Walter
Sterols are a highly complex group of lipophilic compounds present in the unsaponifiable matter of virtually all living organisms. In this study, we developed a novel gas chromatography with mass spectrometry selected ion monitoring (GC/MS-SIM) method for the comprehensive analysis of sterols after saponification and silylation. A new referencing system was introduced by means of a series of saturated fatty acid pyrrolidides (FAPs) as internal standards. Linked with retention time locking (RTL), the resulting FAP retention indices (RIFAP) of the sterols could be determined with high precision. The GC/MS-SIM method was based on the parallel measurement of 17 SIM ions in four time windows. This set included eight molecular ions and seven diagnostic fragment ions of silylated sterols as well as two abundant ions of FAPs. Altogether, twenty molecular ions of C27- to C31-sterols with 0–3 double bonds were included in the final method. Screening of four common vegetable oils (sunflower oil, hemp oil, rapeseed oil, and corn oil) enabled the detection of 30 different sterols and triterpenes most of which could be identified.
High-performance thin-layer chromatography for the detection of compositional changes in LACTEM emulsifiers during storage
(2025) Schuster, Katharina; Blankart, Max; Hinrichs, Jörg; Oellig, Claudia
Quality control of food emulsifiers, such as lactic acid esters of mono- and diacylglycerols (LACTEM), is crucial in the reproducible production of food products. The current study investigated compositional changes of LACTEM emulsifiers using high-performance thin-layer chromatography (HPTLC) during storage at 60 °C for 8 weeks. Ultraviolet (UV) and fluorescence images of the HPTLC silica gel F254s plates after primuline derivatization and densitometric data were analyzed to assess changes in the composition. Significant changes were observed for minor LACTEM components (< 10% relative intensity), specifically a decrease in higher-lactylated monoacylglycerols and an increase in triacylglycerols. Techno-functional properties, such as particle size distribution, apparent viscosity, overrun, foam firmness, drainage, and residual cream of aerosol whipping cream (0.8 g 100 g−1 LACTEM) were investigated. While emulsion stability was not affected, the foam firmness increased significantly, corresponding to a visibly more brittle foam. On the basis of these results, monitoring compositional changes in the food-manufacturing process is necessary to maintain constant food quality.
Monitoring a coffee roasting process based on near‐infrared and raman spectroscopy coupled with chemometrics
(2025) Munyendo, Leah; Schuster, Katharina; Armbruster, Wolfgang; Babor, Majharulislam; Njoroge, Daniel; Zhang, Yanyan; von Wrochem, Almut; Schaum, Alexander; Hitzmann, Bernd
Roasting is a fundamental step in coffee processing, where complex reactions form chemical compounds related to the coffee flavor and its health‐beneficial effects. These reactions occur on various time scales depending on the roasting conditions. To monitor the process and ensure reproducibility, the study proposes simple and fast techniques based on spectroscopy. This work uses analytical tools based on near‐infrared (NIR) and Raman spectroscopy to monitor the coffee roasting process by predicting chemical changes in coffee beans during roasting. Green coffee beans of Robusta and Arabica species were roasted at 240°C for different roasting times. The spectra of the samples were taken using the spectrometers and modeled by the k‐nearest neighbor regression (KNR), partial least squares regression (PLSR), and multiple linear regression (MLR) to predict concentrations from the spectral data sets. For NIR spectra, all the models provided satisfactory results for the prediction of chlorogenic acid, trigonelline, and DPPH radical scavenging activity with low relative root mean square error of prediction (pRMSEP < 9.649%) and high coefficient of determination ( R 2 > 0.915). The predictions for ABTS radical scavenging activity were reasonably good. On the contrary, the models poorly predicted the caffeine and total phenolic content (TPC). Similarly, all the models based on the Raman spectra provided good prediction accuracies for monitoring the dynamics of chlorogenic acid, trigonelline, and DPPH radical scavenging activity (pRMSEP < 7.849% and R 2 > 0.944). The results for ABTS radical scavenging activity, caffeine, and TPC were similar to those of NIR spectra. These findings demonstrate the potential of Raman and NIR spectroscopy methods in tracking chemical changes in coffee during roasting. By doing so, it may be possible to control the quality of coffee in terms of its aroma, flavor, and roast level.

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