Dynamic headspace GC-MS/MS analysis of ethylene oxide and 2-chloroethanol in dry food commodities: a novel approach.

With frequent RASFF notifications from the EU countries, the residue testing of ethylene oxide (EtO) and its metabolite 2-chloroethanol (2-CE) in food commodities has become essential to check their compliance with MRLs. This study, for the first time, aimed at establishing a dynamic headspace-GC-MS/MS method for the simultaneous determination of these two analytes in acetonitrile extracts of cumin, ashwagandha, chilli powder, turmeric powder, guar gum, locust bean gum, and ginger powder. The samples (4 g) were extracted using acetonitrile (10 mL). A dispersive-solid phase extraction cleanup step with primary secondary amine sorbent (50 mg/mL) reduced the interfering signal of (matrix-derived) acetaldehyde by >40% in chilli powder, ginger, turmeric, and guar gum. This cleanup was not required for sesame seeds. With high selectivity and sensitivity, the GC-MS/MS approach identified and quantified both compounds simultaneously. At the spiking levels of 0.01, 0.02, and 0.05 mg/kg, the recoveries and precision were satisfactory (70-120%, RSDs, ≤15%). The headspace method-performance was similar to liquid injections. The method provided reproducible results when evaluated by two different laboratories. The method provided high-precision results for incurred residue analysis. Given its efficiency, the validated method is anticipated to improve the effectiveness of monitoring of EtO residues in food commodities.

Multiresidue analysis of pesticides, polyaromatic hydrocarbons and polychlorinated biphenyls in poultry meat and chicken eggs by GC-MS/MS: method development and validation.

The study uses gas chromatography with tandem mass spectrometry (GC-MS/MS) to develop a reliable analytical approach for detecting multiclass pesticides, polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) in poultry meat and chicken eggs. The meat (2 g) and egg (4 g) samples were extracted with acidified acetonitrile (10 mL) as part of the optimized sample preparation technique. The cleanup consisted of freezing an aliquot of the extract (5 mL) at -20 °C, followed by dispersive solid phase extraction using 50 mg PSA + 100 mg C18+150 mg MgSO4. The matrix co-extractives were effectively removed and the method performance met the European Commission's analytical quality control criteria (SANTE/12682/2019). The method was validated at two spiking levels (10 and 20 ng/g of 225 pesticides, 9 PAHs and 8 PCBs), and good recoveries (70-120%) and precision-RSDs (≤20%) were achieved for 90% of the targeted pesticide residues. For 80% of the compounds, the LOQs were ≤10 ng/g. The results of the intra-laboratory (involving six analysts) and inter-laboratory validation studies (involving eight ISO 17025 accredited laboratories) established satisfactory ruggedness and reproducibility. It created potential applications in commercial residue testing laboratories for regulatory compliance check purposes.