PMID- 38115807 OWN - NLM STAT- PubMed-not-MEDLINE LR - 20240104 IS - 1759-9679 (Electronic) IS - 1759-9660 (Linking) VI - 16 IP - 2 DP - 2024 Jan 4 TI - Magnetic mesoporous Fe(3)O(4)@nSiO(2)@mSiO(2) nanoparticles for high-throughput mass spectrometry detection of hydrolyzed products of organophosphorus nerve agents. PG - 301-313 LID - 10.1039/d3ay01785k [doi] AB - Rapid and accurate detection of hydrolyzed products of organophosphorus nerve agents (OPNAs) is an important method to effectively confirm the use of these agents. OPNAs are rapidly hydrolyzed to the methyl phosphonates (MPs) in the environment, which can be used as environmental traceability marker for OPNAs. Herein, magnetic mesoporous materials combined with real-time in situ mass spectrometry (MS) were used to achieve high-throughput detection of MPs. Novel magnetic mesoporous nanoparticles Fe(3)O(4)@nSiO(2)@mSiO(2) were synthesized via co-condensation of tetraethyl orthosilicate and cetyltrimethylammonium bromide (CTAB) on the surface of nonporous silica-coated Fe(3)O(4) under alkaline conditions. CTAB templates were removed by the reflux of ethanol (0.0375 mM ammonium nitrate) to form mesoporous SiO(2), which has a large specific surface area of 549 m(2) g(-1) and an excellent magnetization strength of 59.6 emu g(-1). A quick, cost-effective, rugged, and safe magnetic preparation method, magnetic QuEChERS, was established with magnetic mesoporous nanoparticles (Fe(3)O(4)@nSiO(2)@mSiO(2)) as adsorption materials for direct analysis in real-time and tandem MS (DART-MS/MS) of MPs in environmental samples. The method exhibits good linearity (R(2) > 0.992) in the range of 20.0-4.00 mug mL(-1), the limits of detection were <5.00 ng mL(-1), the limits of quantification were <20.0 ng mL(-1), and the extraction recoveries were 70.2-98.1%, with relative standard deviations (RSDs) in the range of 1.97-10.6%. Additionally, using this method, analysis of 70 environmental samples could be completed within 20 min. Then, the M-QuEChERS-DART-MS/MS method was applied to the 52nd Organisation for the Prohibition of Chemical Weapons (OPCW) environmental spiked samples analysis, where the accuracy was 95.2-116%, and the RSD was 1.16-7.83%. The results demonstrated that Fe(3)O(4)@nSiO(2)@mSiO(2) based on the QuEChERS method can quickly and efficiently remove the matrix of environmental samples and when coupled with the DART-MS/MS can achieve high-throughput determination of MPs in environmental samples. FAU - Qu, Gang AU - Qu G AUID- ORCID: 0000-0002-5883-1144 AD - State Key Laboratory of NBC Protection for Civilian, Beijing 102205, P. R. China. ricdyihui@163.com. FAU - Zhao, Yuxin AU - Zhao Y AD - State Key Laboratory of NBC Protection for Civilian, Beijing 102205, P. R. China. ricdyihui@163.com. FAU - Zhang, Qiaoli AU - Zhang Q AD - State Key Laboratory of NBC Protection for Civilian, Beijing 102205, P. R. China. ricdyihui@163.com. FAU - Wu, Jina AU - Wu J AD - State Key Laboratory of NBC Protection for Civilian, Beijing 102205, P. R. China. ricdyihui@163.com. FAU - Li, Xiaosen AU - Li X AUID- ORCID: 0009-0004-7912-1266 AD - State Key Laboratory of NBC Protection for Civilian, Beijing 102205, P. R. China. ricdyihui@163.com. FAU - Yang, Yang AU - Yang Y AD - State Key Laboratory of NBC Protection for Civilian, Beijing 102205, P. R. China. ricdyihui@163.com. FAU - Liu, Shilei AU - Liu S AUID- ORCID: 0000-0001-6154-2661 AD - State Key Laboratory of NBC Protection for Civilian, Beijing 102205, P. R. China. ricdyihui@163.com. LA - eng PT - Journal Article DEP - 20240104 PL - England TA - Anal Methods JT - Analytical methods : advancing methods and applications JID - 101519733 SB - IM EDAT- 2023/12/20 06:42 MHDA- 2023/12/20 06:43 CRDT- 2023/12/20 03:43 PHST- 2023/12/20 06:43 [medline] PHST- 2023/12/20 06:42 [pubmed] PHST- 2023/12/20 03:43 [entrez] AID - 10.1039/d3ay01785k [doi] PST - epublish SO - Anal Methods. 2024 Jan 4;16(2):301-313. doi: 10.1039/d3ay01785k.