32 May / June 2017 Table 3: Analysis results for glyphosate in beer
Commission Regulation 1058/2012 setting maximum residue limits for aflatoxins, ochratoxin A, patulin, deoxynivalenol, zearelenone, fumonisins, T2 and HT2 toxin in a variety of different products. Mycotoxins are not destroyed by temperature treatment, and are barely influenced by cooking, freezing or digestion. These properties make the investigation and quantitation of mycotoxins in food very important.
Aflatoxins are toxic and carcinogenic. Aflatoxin B1 the most common type of aflatoxin present in food products is one of the most genotoxic and carcinogenic species [2]. Ochratoxin is produced by penicillium and aspergillus species and is a contaminant in alcoholic beverages such as beer and wine. Patulin, produced by p. expansum, aspergillus, penicillium, and paecilomyces fungal species, is often found in mouldy fruits and vegetables. Zearalenone is produced by fusarium species and may be present in crops; AFM1 is often found in milk products.
In order to comply with the European regulation on food safety, manufacturers of food and beverages must control the quantities of these contaminants, so sensitive methods for detection of mycotoxins in complex matrices are essential.
Figure 3: Chromatograms of a 15 ng/mL beer sample – 15 ng/ml glyphosate/ FMOC- glyphosate Table 4: EU concentration limits for Mycotoxins Mycotoxin Screening System
AFB1, AFB2, AFG1, AFG2, AFM1, OTA, ZON, DON, NIV, and PAT were investigated using a mycotoxin screening system employing the Shimadzu i-Series integrated UHPLC system. The five commonly tested analytes (Aflatoxins, ZON, OTA, NIV and DON) in malt products were extracted and analysed in spiked and non-spiked beer samples from different batches.
PAT in apple juice and grape juice was also tested separately.
EU limits for Mycotoxins are shown in Table 4. Mycotoxins detection after UHPLC was performed using a combination of fluorescence and photodiode array (PDA) detection. The chromatograms of the standard mixture with PDA and fluorescence detection containing all 10 mycotoxins is shown in Figure 4.
The EU MRL for mycotoxins as specified by EU standards are the strictest in the world [9]. Mycotoxin standards were prepared using the concentration specified in the EU control criteria to determine the mycotoxin levels in the food samples under investigation contain mycotoxins. A simple, fast one point calibration was sufficient to assess compliance with the EU control criteria. Samples were created using the calibration standard and the food samples, and the subsequent results show the mycotoxins concentrations in the food samples and whether they complied to the EU control criteria.
The samples tested (apple juice, grape juice and two batches of beer) either contained no mycotoxins or were well below the EU criteria. The spiked samples showed mycotoxin concentrations above the EU criteria.
Figure 4: Mycotoxins detected by fluorescence and PDA detection
however the positive samples contained less glyphosate than the MRL of the commodities (e.g. barley, hops) [8].
Mycotoxin Analysis The European legislation for
mycotoxins in food, which are hazardous substances for humans when ingested, consists of two main regulations: The Commission Regulation 1881/2006 setting maximum levels for certain contaminants in foodstuffs, and the most recent mycotoxin related update by
For all mycotoxin standards, the limit of detection (LODs) and limit of quantitation (LOQs) were determined as shown in Table 5. The LODs and LOQs were approximately 50% of the EU MRL.
Determination of Heavy Metals Using ICP-MS
Heavy metals such as cadmium, chromium and lead are natural components of the earth’s crust and are typically present in our environment at various concentration levels. They enter the human body via food, drink and air. Some of these heavy metals, the so-called trace elements such as
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