The current work is the first study on online coupling of matrix solid-phase dispersion (MSPD) to direct analysis in real time mass spectrometry (DART-MS) bridging with solid-phase analytical derivatization (SPAD) based on a graphene oxide nanosheets (GONs)-coated cotton swab. Proof-of-concept demonstrations were explored for high-throughput analysis of a diversity of regulated chemicals in consumer products such as textiles, toys, and cosmetics. On-demand sorbent combinations were blended with samples, packed into MSPD columns, and mounted on a homemade 3D-printed rack module for automated sample feeding. To achieve good synergy between MSPD and DART-MS, a cotton swab with a conical tip deposited with GONs was attached to the bottom of the MSPD column. The swabs serve as a solid-phase microextraction probe for convenient enrichment of the eluted analytes from MSPD, thermal desorption of the enriched analytes by DART, and sensitive detection by a hybrid quadrupole-Orbitrap mass spectrometer. Furthermore, the utility of an on-swab SPAD strategy was demonstrated for the detection of formaldehyde by use of the derivatizing reagent of dansyl hydrazine, contributing to improved ionization efficiency without compromising the overall coherence of the analytical workflow. The MSPD-DART-MS methodology was systematically optimized and validated, obtaining acceptable recovery (71.7–110.3%), repeatability (11.8–19.3%), and sensitivity (limits of detection and quantitation in the ranges of 6.2–19.5 and 23.7–75.9 μg/kg) for 32 target analytes. The developed protocol streamlined sample extraction, clean-up, desorption, ionization, and detection, highlighting the appealing potential for high-throughput analysis of samples with complex matrices.

目前的工作是第一项关于基质固相分散 (MSPD) 与基于氧化石墨烯纳米片 (GON) 的固相分析衍生化 (SPAD) 桥接的实时质谱 (DART-MS) 直接分析的在线耦合研究) 涂层棉签。探索了概念验证演示，以对纺织品、玩具和化妆品等消费品中的多种受管制化学品进行高通量分析。按需吸附剂组合与样品混合，装入 MSPD 色谱柱，并安装在自制的 3D 打印机架模块上以实现自动进样。为了在 MSPD 和 DART-MS 之间实现良好的协同作用，将带有沉积有 GON 的锥形尖端的棉签连接到 MSPD 柱的底部。拭子用作固相微萃取探针，方便从 MSPD 中富集洗脱的分析物，通过 DART 热解吸富集的分析物，以及通过混合四极杆-Orbitrap 质谱仪进行灵敏检测。此外，通过使用丹磺酰肼的衍生试剂，证明了拭子上 SPAD 策略可用于检测甲醛，有助于提高电离效率，同时不影响分析工作流程的整体一致性。MSPD-DART-MS 方法经过系统优化和验证，获得了可接受的回收率 (71.7–110.3%)、重复性 (11.8–19.3%) 和灵敏度（检测限和定量限在 6.2–19.5 和 23.7–75.9 范围内） μg/kg) 用于 32 种目标分析物。开发的协议简化了样品提取、清理、