PMID- 37968819 OWN - NLM STAT- MEDLINE DCOM- 20231117 LR - 20231119 IS - 1872-2059 (Electronic) IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 41 IP - 11 DP - 2023 Nov TI - [Determination of seven mycotoxins in cereals by ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry based on the self-built database]. PG - 1002-1009 LID - 10.3724/SP.J.1123.2023.07014 [doi] AB - A method for the determination of seven mycotoxins in rice and wheat by ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS) based on self-built database was established. Samples were extracted with 0.2% formic acid aqueous solution-acetonitrile (50ratio50, v/v), dehydrated and salted according to the QuEChERS method (4 g of magnesium sulfate, 1 g of sodium chloride, 1 g of sodium citrate, 0.5 g of citrate disodium salt), and separated on an HSS T3 column (100 mmx2.1 mm, 1.8 mum). UPLC-Q-TOF/MS with MS(E) screening was performed, and the positive and negative ions of the screened mycotoxins were calibrated and quantified using matrix-matched standard curves with time of flight multiple reaction monitoring (TOF-MRM). The results showed that aflatoxin G(1) (AFG(1)), aflatoxin G(2) (AFG(2)), aflatoxin B(1) (AFB(1)), aflatoxin B(2) (AFB(2)), and ochratoxin A (OTA) exhibited moderate matrix effects in rice, while OTA and zearalenone (ZEN) exhibited moderate matrix effects in wheat. The seven mycotoxins showed good linearities in their respective concentration ranges, with correlation coefficients (r) of 0.9900-0.9998. The limits of detection (LODs) for rice and wheat were 0.50-400 and 0.50-200 mug/kg, respectively, and the limits of quantification (LOQs) for both cereals were 1.00-800 mug/kg. In rice, the average recoveries at three spiked levels of low, medium, and high were 88.1%-123.9%, with relative standard deviations (RSDs) of 0.2%-13.6%. In wheat, the average recoveries at three spiked levels of low, medium, and high were 102.0%-123.4%, with RSDs of 0.8%-14.8%. As a result, one batch of 46 batches of rice was screened out for AFB(1) and AFB(2), with a screening rate of 2.2%, of which the measured values were 10.8 mug/kg and 1.2 mug/kg, respectively. According to GB 2761-2017, the maximum allowable level of AFB(1) in rice is 10 mug/kg; thus, the exceeding rate for AFB(1) is 2.2%. Deoxynivalenol (DON) was screened out in 9 out of 24 batches of wheat (screening rate, 37.5%), while ZEN was screened out in 19 batches (screening rate, 79.2%). According to GB 2761-2017, the maximum allowable levels of DON and ZEN in wheat are 1000 and 60 mug/kg, respectively. The levels of DON and ZEN detected in the wheat samples did not exceed these limits. The proposed method uses MS(E) for qualitative screening to avoid the occurrence of false positives caused by interfering compounds with mass numbers and retention times similar to those of the analytes. TOF-MRM mode is then used to quantify the positively screened mycotoxins. The method is fast, accurate, sensitive, and suitable for the isolation and quantitative detection of mycotoxin residues in rice and wheat samples. The findings provide powerful technical support for mycotoxin contamination monitoring in rice and wheat and early risk-warning efforts. FAU - Zhang, Lu-Xing AU - Zhang LX AD - Zhejiang Pharmaceutical University, Ningbo 315100, China. FAU - Zhou, Zheng AU - Zhou Z AD - Ningbo Institute for Drug Control, Ningbo 315048, China. FAU - Cao, Lin AU - Cao L AD - Ningbo Institute for Drug Control, Ningbo 315048, China. FAU - Qian, Jiang AU - Qian J AD - Zhejiang Pharmaceutical University, Ningbo 315100, China. LA - chi PT - English Abstract PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0 (Mycotoxins) RN - 5W827M159J (Zearalenone) SB - IM MH - *Mycotoxins/analysis MH - Edible Grain/chemistry MH - Chromatography, High Pressure Liquid MH - Tandem Mass Spectrometry/methods MH - Chromatography, Liquid MH - *Zearalenone/analysis PMC - PMC10654887 OTO - NOTNLM OT - QuEChERS OT - mycotoxins OT - rice OT - ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS) OT - wheat EDAT- 2023/11/16 06:44 MHDA- 2023/11/17 15:27 PMCR- 2023/11/08 CRDT- 2023/11/16 00:29 PHST- 2023/11/17 15:27 [medline] PHST- 2023/11/16 06:44 [pubmed] PHST- 2023/11/16 00:29 [entrez] PHST- 2023/11/08 00:00 [pmc-release] AID - 10.3724/SP.J.1123.2023.07014 [doi] PST - ppublish SO - Se Pu. 2023 Nov;41(11):1002-1009. doi: 10.3724/SP.J.1123.2023.07014.