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SFC/FTIR, SFC/APCI-MS and MALDI-TOF-MS for the analysis of siloxane-ethylene oxide copolymers
(2000)
Polydimethylsiloxanes (PDMSs) modified by introducing ethylene oxide units with the aim of forming sufficiently water-soluble siloxane compounds were characterized using supercritical fluid chromatography (SFC) coupled with Fourier transform infrared (FTIR) spectroscopy and atmospheric pressure chemical ionization mass spectrometry (APCIMS), and matrix-assisted laser desorptionionization time-of-flight mass spectrometry (MALDITOF-MS). SFC has a domain in analyzing oligomers. Hyphenated techniques enable elucidation of the components. Remarkable is the resolution and short analysis time of MALDITOF-MS. SFC also allows quantification of the basic and reaction products.
Mycotoxins are important non-anthropogenic food and feed contaminants, which can be present on almost every agricultural commodity. Effective consumer protection therefore essentially depends on food surveillance by reliable quantitative analysis enabled by appropriate quality control. Certified (matrix) reference materials (CRMs) are versatile tools to support Quality assurance. However, in the case of ochratoxin A (OTA), a hepato- and nephrotoxic mycotoxin, which is regulated in various foods, there is a lack of suitable CRMs. This lack has now been overcome by the development of two European Reference Materials (ERM®) for the Determination of OTA in roasted coffee (ERM®-BD475) and red wine (ERM®-BD476). This article discusses the material preparation process as well as the results of homogeneity and stability testing. Furthermore, the results of the inhouse certification studies carried out at BAM Federal Institute for Materials Research and Testing are presented and discussed. Interlaboratory comparison studies involving selected expert laboratories with documented Expertise in the field of mycotoxin analysis were conducted to confirm the certified values determined by BAM. The certified ochratoxin A values and their corresponding expanded uncertainties (k = 2) were assigned in full compliance with the requirements of ISO Guide 35 and are as follows:
(6.0 ± 0.6) µg kg-1 for roasted coffee, ERM®-BD475, and (0.52 ± 0.11) µg L-1 for red wine, ERM®-BD476.