A new method for screening pesticide residues in vegetable and fruit juices by the multi-plug filtration cleanup (m-PFC) method combined with gas chromatography-electrostatic field orbitrap high resolution mass spectrometry(GC-Orbitrap/MS) was developed. The samples were extracted with acetonitrile, purified with m-PFC and determined by GC-Orbitrap/MS. Qualitative analysis was confirmed by retention time, accurate molecular mass and quantitative analysis were performed with the matrix standard calibration. It could eliminate matrix interference effectively. Eight kinds of typical samples (orange juice, apple juice, grape juice, strawberry juice, celery juice, carrot juice, cucumber juice, tomato juice) were evaluated. The linear ranges of the 350 pesticides were from 5 to 500 μg/kg, with good correlation coefficients greater than 0.990. The limits of detection (LODs) were 0.3–3.0 μg/kg and the limits of quantification (LOQs) were 1.0–10.0 μg/kg. The average recoveries at three spiked levels of 10, 100, 200 μg/kg were in the range of 72.8–122.4%, with relative standard deviations (RSDs) of 2.0–10.8%. The method has effectively improved the determination efficiency of pesticide residue screening by high-resolution mass spectrometry in vegetable and fruit juices.
Eugenol compounds are widely used in the circulation and transportation of fresh aquatic products because of their good anesthetic effects. However, some studies have shown that eugenol compounds are potential carcinogens. Therefore, in order to ensure the edible safety of aquatic products, eugenol compounds in aquatic products need to be screened quickly. A method for determination of six eugenol residues in aquatic products was established by multiplug filtration cleanup (m-PFC), combined with gas chromatography-Orbitrap mass spectrometry (Orbitrap GC-MS). Samples were ultrasonically extracted with acetonitrile, and the extracts were frozen at −18°C for 1 h, then purified with the m-PFC column, and detected by Orbitrap GC-MS in full scan mode. The results showed the linear relationships for six eugenols were good in the range of 0.001–0.1 μg/mL, and the correlation coefficients (R2) were above 0.9950. The limits of detection (LODs) were 2–10 μg/kg, and the limits of quantitation (LOQs) were 5–20 μg/kg. The average recoveries at the spiked levels of 5–200 μg/kg were in the range of 76.4%–105.1%, with relative standard deviations (RSDs) of 1.2%–7.5%. Eighty aquatic products were detected by this method, of which only eugenol was detected in 12 samples, and eugenol and isoeugenol were detected in two samples at the same time. The other eugenol compounds were not detected in any sample. The detection rate of positive samples was 17.5%. The method is simple, accurate, and suitable for the rapid screening of eugenol compounds in aquatic products.
A method for simultaneous determination of 22 polycyclic aromatic hydrocarbons (PAHs) residues in vegetable oils by gas chromatography-electrostatic field orbitrap high resolution mass spectrometry (Orbitrap GC-MS) was established. The samples were vortexed with acetonitrile, centrifuged at 8,000 r/min for 5 min, and frozen at −70°C for 10 min. The extracts of upper layer were poured out, dried with nitrogen at 40°C, redissolved in dichloromethane, and measured by Orbitrap GC-MS. The matrix interference in vegetable oil could be effectively removed by determining the accurate mass number of target compounds under the full scan mode. Six typical vegetable oil samples (soybean oil, sesame oil, peanut oil, olive oil, rapeseed oil, sunflower oil) were used for method validation. The calibration curve displayed good linearity in the range of 1–100 ng/mL, with correlation coefficients > 0.9950. The limits of detection (LODs) were in the range of 0.10–0.60 μg/kg, and the limits of quantification (LOQs) were in the range of 0.35–2.00 μg/kg. The average spiked recoveries of 22 PAHs in 6 matrices at 5, 50 and 100 μg/kg levels were 76.4–115.4%, and the average relative standard deviations (RSDs) were 1.8–10.8%. The results showed that 22 PAHs were detected in 6 types of 90 edible vegetable oil samples in the Chinese market by this method. Meanwhile, the abundance of light PAHs (LPAHs) was higher than that of heavy PAHs (HPAHs), and its relative contribution of LPAHs to the total PAHs was higher. All levels of BaP conformed to the Chinese requirement of upper limit, 10 μg/kg. However, 13.3 and 11.1% of the samples exceeded the maximum limits of BaP and PAH4 set by EU, 2 and 10 μg/kg, respectively. The total concentrations of 22 PAHs (defined as PAH22) varies greatly among different oil species, and the average PAH22 contents were listed in descending order as follows: peanut oil > sesame oil > olive oil > rapeseed oil > soybean oil > sunflower seed oil. The established method effectively avoided interference from large amounts of lipids and pigments. Therefore, the method is simple, sensitive and suitable for rapid screening and confirmation of PAHs in vegetable oil.
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