PMID- 37968817 OWN - NLM STAT- MEDLINE DCOM- 20231127 LR - 20231127 IS - 1872-2059 (Electronic) IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 41 IP - 11 DP - 2023 Nov TI - [Determination of 22 mycotoxins in milk by liquid chromatography-quadrupole/orbitrap mass spectrometry]. PG - 986-994 LID - 10.3724/SP.J.1123.2023.07010 [doi] AB - Mycotoxins have carcinogenic, mutagenic, hepatotoxic, nephrotoxic, immunotoxic, neurotoxic, and teratogenic properties. Thus, these substances have attracted significant attention because they pose a threat to human health. As research on mycotoxins deepens, new structural analogues of mycotoxins are constantly being discovered. In this study, a method based on high performance liquid chromatography-quadrupole/orbitrap mass spectrometry was established for the simultaneous determination of 22 mycotoxins in milk. A simple, effective, and rapid pretreatment method was optimized by focusing on the solvent type, extractant volume, and extracting salt based on the characteristics of the mycotoxins and sample matrix. The analytes were extracted using 0.5% formic acid acetonitrile solution and added with sodium chloride to separate fats from water. The samples were centrifuged at 8000 r/min (4 ℃) for 5 min using a centrifuge and then concentrated using nitrogen. The dry residue was dissolved with 50% methanol aqueous solution. Twenty-two mycotoxins were separated on a ZORBAX Eclipse Plus C(18) chromatographic column (100 mmx2.1 mm, 1.7 mum), and quantitative analysis was performed using the isotope internal standard method. The analytes were determined by liquid chromatography-quadrupole/orbitrap mass spectrometry in positive electrospray ionization mode. Qualitative analyses of the compounds were performed in full mass spectrometry/data-dependent tandem mass spectrometry (MS/dd-MS(2)) mode. Good linearities in the range of 0.5-100.0 mug/L were observed for the 22 mycotoxins, and the correlation coefficients (R(2)) were greater than 0.999. The limits of detection (S/N=3) and quantification (S/N=10) ranged from 0.3 to 0.5 mug/kg and from 1.0 to 1.5 mug/kg, respectively. The average recoveries of the 22 mycotoxins at three spiked levels of 1.5, 5.0, and 15 mug/kg were between 84.7% and 100.8%, with relative standard deviations (RSDs) of 1.2%-9.9%. These findings indicate that the method has high sensitivity and accuracy as well as good precision. Finally, the method was applied to the detection and analysis of mycotoxins in 25 actual commercial milk samples. The results revealed that the selected samples were not contaminated with any of the mycotoxins analyzed. Thus, the proposed method is useful as a quick preprocessing and confirmatory method for the simultaneous determination of mycotoxins in milk. FAU - Tong, Lan-Yan AU - Tong LY AD - Chinese Academy of Inspection and Quarantine, Beijing 100176, China. AD - Key Laboratory of Food Quality and Safety for State Market Regulation, National Center of Technology Innovation for Dairy, Beijing 100176, China. AD - Chongqing Academy of Metrology and Quality Inspection, National Center of Quality Supervision & Inspection Agricultural Processed Products and Condiments, Chongqing 401123, China. FAU - Xu, Bo-Zhou AU - Xu BZ AD - Chinese Academy of Inspection and Quarantine, Beijing 100176, China. AD - Key Laboratory of Food Quality and Safety for State Market Regulation, National Center of Technology Innovation for Dairy, Beijing 100176, China. FAU - Nie, Xue-Mei AU - Nie XM AD - Chinese Academy of Inspection and Quarantine, Beijing 100176, China. AD - Key Laboratory of Food Quality and Safety for State Market Regulation, National Center of Technology Innovation for Dairy, Beijing 100176, China. FAU - Wang, Xiu-Juan AU - Wang XJ AD - Chinese Academy of Inspection and Quarantine, Beijing 100176, China. AD - Key Laboratory of Food Quality and Safety for State Market Regulation, National Center of Technology Innovation for Dairy, Beijing 100176, China. FAU - Ma, Jia-Hui AU - Ma JH AD - Chinese Academy of Inspection and Quarantine, Beijing 100176, China. AD - Key Laboratory of Food Quality and Safety for State Market Regulation, National Center of Technology Innovation for Dairy, Beijing 100176, China. FAU - Guo, Wei AU - Guo W AD - Chinese Academy of Inspection and Quarantine, Beijing 100176, China. AD - Key Laboratory of Food Quality and Safety for State Market Regulation, National Center of Technology Innovation for Dairy, Beijing 100176, China. FAU - Li, Gen-Rong AU - Li GR AD - Chongqing Academy of Metrology and Quality Inspection, National Center of Quality Supervision & Inspection Agricultural Processed Products and Condiments, Chongqing 401123, China. FAU - Gong, Ying-Kun AU - Gong YK AD - Chongqing Academy of Metrology and Quality Inspection, National Center of Quality Supervision & Inspection Agricultural Processed Products and Condiments, Chongqing 401123, China. FAU - Xu, Xiu-Li AU - Xu XL AD - Chinese Academy of Inspection and Quarantine, Beijing 100176, China. AD - Key Laboratory of Food Quality and Safety for State Market Regulation, National Center of Technology Innovation for Dairy, Beijing 100176, 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) SB - IM MH - Humans MH - Animals MH - *Mycotoxins/analysis MH - Milk/chemistry MH - Chromatography, Liquid MH - Tandem Mass Spectrometry MH - Chromatography, High Pressure Liquid PMC - PMC10654881 OTO - NOTNLM OT - liquid chromatography-quadrupole/orbitrap mass spectrometry OT - milk OT - mycotoxins OT - rapid pretreatment EDAT- 2023/11/16 06:44 MHDA- 2023/11/27 12:42 PMCR- 2023/11/08 CRDT- 2023/11/16 00:29 PHST- 2023/11/27 12:42 [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.1123.2023.07010 [doi] PST - ppublish SO - Se Pu. 2023 Nov;41(11):986-994. doi: 10.3724/SP.J.1123.2023.07010.