2. Gıda Kimyası Kongresi, Antalya, Türkiye, 15 - 19 Mart 2023, ss.60-61
Ethylene oxide (EO) is
widely used as a food fumigant due to its strong antibacterial properties. Because
of its carcinogenic, mutagenic and reprotoxic potentials, EO has been banned in
European Union (EU) countries in recent years. But, the use of this compound is
still permitted in several countries and numerous alerts for EO residues in
various food samples, especially sesame, were reported by European Commission (EC)
Rapid Alert System for Food and Feed portal (RASFF)1. In the last two
years, EO was detected in only 8 samples of food additives originated from
Turkey. Because of its high volatility, EO rapidly dissipates to its less
volatile metabolite “2-chloroethanol (2-CE)”. Based on the EC Regulation
(396/2995), EO residue is defined as sum of ethylene oxide and its main
metabolite 2-CE. The aim of the present study was to validate a reliable chromatographic method for the determination
of EO and 2-CE by GC-MS/MS in commodities with high oil content. Dried walnut
samples were chosen as a representative of this commodity group and validation
studies were performed according to the SANTE/11312/2021 guidelines3. After
a pretreatment at 70°C for 40 min, the extraction and cleaning up
procedures were conducted with QuEChERS method2. Matrix-matched
internal curves of EO and
2-CE in the range of 5-100 μg kg−1
showed good linearity. Average recovery rates were 96.4 and 100.3% for EO and
95.9 and 89.3% for 2-CE, when tested at 2 concentration levels of 10 and 40 µg
kg-1, respectively. The maximum RSD values of repeatability (RSDr)
were 12.7 and 15.6% for EO; 11.8 and 16.2% for 2-CE for 10 and 40 µg kg-1
concentrations of the compounds, respectively. The maximum RSD values of reproducibility
(RSDwR) for same concentrations were 14.7 and 15.3% for EO; 10.9 and
13.6% for 2-CE, respectively. Limit of quantification (LOQ) values for 5 µg kg-1
of both compounds were found as 7.6 and 8.9 μg kg−1 for EO and 2-CE. The validated LOQ values
for EO and 2-CE were under the lowest Maximum Residue Limits of EU (50 and 10
μg kg−1, respectively) of
the compounds for walnut sample. The validation data of both compounds obtained
in GC-MS/MS analysis was quite reliable and were in line with the SANTE/11312/2021
Guideline3. This study was funded by Perla Fruit Company with
the grant number of ULUTEK STB079417.