Organophosphate nerve agents (OPNAs) are lethal chemical weapons (CWs) which hydrolyze rapidly to alkyl phosphate compounds in the environment. The identification of alkyl phosphate compounds in the environment is critical for the verification of OPNAs. Currently, due to the complex sample preparation and long detection process for organophosphate nerve agent hydrolysis products (OPNAHPs), their high-throughput determination is difficult. To simplify sample preparation and detection of OPNAHPs from environmental samples, a quick, easy, cheap, effective, rugged and safe (QuEChERS) method for the simultaneous purification of the five OPNAHPs in environmental samples combined with detection through direct analysis in real-time ionization source coupled with tandem mass spectrometer (DART-MS/MS) was developed. An internal standard method was applied for the quantification. The method exhibited a good linearity ( R 2 > 0.991) in the range of 1.00 ng/mL-4.00 μg/mL. The limits of detection and limits of quantification were 1.00–7.00 ng/mL and 10.0–20.0 ng/mL, respectively. The recoveries of OPNAHPs in environmental samples were between 65.3% and 107%, with relative standard deviations ranged from 1.6% to 19%. In addition, the sample preparation and analysis process for OPNAHPs could be completed in less than 10 min. The results demonstrated that the modified QuEChERS method could quickly and efficiently remove the matrix of environmental samples. Combined with DART-MS/MS, an accurate and high-throughput detection method of OPNAHPs in environmental samples was provided. The developed method has great potential in the fields of early warning, clinical treatment and environmental decontamination.
Li Huaqiang,Wu Feifei,Ding Yuxian,Long Guozhou,Yin Lei
A novel and rapid analytical assay based on direct analysis in real-time tandem mass spectrometry (DART-MS/MS) technology was established for quantification of butachlor in this study. The assay incorporated micro-solid-phase extraction (μ-SPE) for sample pretreatment, with acetochlor as an internal standard. Quantification was achieved via transitions from [M + H] + precursor ions to primary and secondary fragment ions at m/z 312.1 → 238.0 → 162.1 (butachlor) and 270.1 → 224.1 → 148.0 (acetochlor). This chromatography-free approach eliminated reliance on mobile phases and chromatographic instrumentation, significantly improving analytical throughput (0.4 min/sample) while reducing environmental impact. Method validation demonstrated linearity over 0.5–100 ng/mL ( R 2 > 0.995), with intra-/inter-day precision < 13.1% and accuracy ranging from −6.00% to 11.0%. The assay was used to evaluate the cellular uptake kinetics of butachlor in MCF-7 cells. These findings underscore the utility of DART-MS/MS assay for rapid environmental and toxicological assessments while highlighting potential safety concerns associated with butachlor exposure. The integration of DART-MS/MS with μ-SPE offers a sustainable alternative to conventional bioanalytical workflows, combining speed, sensitivity, and reduced chemical consumption for ecotoxicological studies. Graphical abstract
危险品化学品经营许可证（带存储）