Direct determination of acrylamide in food by gas chromatography-high-resolution time-of-flight mass spectrometry

Simple and rapid gas chromatographic (GC) method employing a high-resolution time-of-flight mass analyzer that enables direct analysis (no derivatization) of acrylamide in various heat-processed foodstuffs has been developed and validated. Co-isolation of acrylamide precursors such as sugars and asparagine, constituting the risk of results overestimation due to additional formation of analyte in hot GC injector, is avoided by the extraction with n-propanol followed by solvent exchange to acetonitrile (MeCN). Introduction of a novel purification strategy, dispersive solid phase extraction, based on addition of primary-secondary amine (PSA) sorbent into deffated extract in MeCN, provides a significant reduction of some abundant matrix co-extracts (mainly free fatty acids). Isotope dilution technique (d₃-acrylamide as an internal standard) is employed for compensation of potential target analyte losses and/or matrix-inducted chromatographic response enhancement. Limits of quantifications (LOQs) ranged between 15 and 40 μg kg⁻¹ and recoveries were between 97 and 108% depending on the examined food matrix. The repeatability of measurements (expressed as relative standard deviation, R.S.D.) was as low as 1.9% for potato crisps containing acrylamide at a level of 1 mg kg⁻¹. Slightly higher values (R.S.D. < 4.0%) were achieved for breakfast cereals and crisp bread with approximately 10 times lower content of this processing contaminant. Trueness of results generated by this new method was demonstrated via FAPAS^® (Food Analysis Performance Assessment Scheme) interlaboratory proficiency tests.     

Precursor ion scanning for the non-targeted detection of individual arsenosugars in extracts of marine organisms

Arsenosugars are a group of arsenic compounds reported to be present in a wide variety of marine organisms. Numerous such compounds have been identified and characterized in marine organisms; however, unknown arsenosugar species may also be present. This indicates the need for an analytical technique suitable for their non-targeted detection. One such technique is tandem mass spectrometry operated in the precursor ion scanning mode. This technique is based on scanning for precursor ions that give specific product ions, characteristic of the compounds under investigation. In the present study two subgroups of arsenosugar species were examined, the oxo- and the thioarsenosugars, the CID behavior of which is well known from previous studies. In the case of the oxoarsenosugars characteristic product ions were observed at m/z 237 and 97, and for the thioarsenosugars at m/z 253 and 97. Validation of this approach was carried out by analyzing extracts of two commercial kelp powders with known contents of arsenosugar species. All arsenosugars reported to exist in these materials were detected successfully using the precursor ion scanning approach. The limits of detection for the oxo- and the thioarsenosugar species, and the selectivity and sensitivity of the method, strongly indicate the suitability of this approach for the non-targeted detection of arsenosugars in extracts of marine origin.     

A new chemical probe for the detection of the cancer-linked galectin-3

A chemical probe was developed for the detection of the emerging cancer marker galectin-3. The probe contains a benzophenone moiety which covalently attaches itself to the protein upon binding and irradiation. Introduction of a fluorescent label via'click' chemistry allows the labelled proteins to be visualized in a gel. With the probe, selective visualization of galectin-3 in protein mixtures was shown and remarkably even in cell lysates.