The coupling of micro solid-phase extraction (μSPE) with mass spectrometry (MS) was reported and coupled with a miniature mass spectrometer for the first time. μSPE is a promising pretreatment technique that can purify the matrix and extract target analytes in complex samples. With the online combination of μSPE with MS, the concentrated analytes eluted from the μSPE cartridge were directly ionized via electrospray ionization (ESI) and introduced into the mass spectrometer for detection. After optimization, ion intensities of drugs in saliva and rhodamine B in chili powder were enhanced 145 to 214-fold and 74 to 170-fold, respectively. The limit of quantitation (LOQ) was 2 ng/mL for drugs and 1 ng/mL for rhodamine B. Moreover, the μSPE was also coupled online with a miniature mass spectrometer, which improved the sensitivity of the miniature mass spectrometer more than 10 times. The combination of μSPE and MS significantly improved the detection sensitivity and identification capability for complex sample analyses. As a convenient and compact device, μSPE could enhance the analytical performances of mini-MS, and would benefit its field applications.

首次报道了微固相萃取（μSPE）与质谱（MS）的耦合，并首次与微型质谱仪耦合。μSPE 是一种很有前景的预处理技术，可以纯化基质并提取复杂样品中的目标分析物。通过 μSPE 与 MS 的在线组合，从 μSPE 小柱洗脱的浓缩分析物通过电喷雾电离 (ESI) 直接电离，并引入质谱仪进行检测。优化后，唾液中药物和辣椒粉中罗丹明B的离子强度分别提高了145～214倍和74～170倍。药物的定量限 (LOQ) 为 2 ng/mL，罗丹明 B 的定量限为 1 ng/mL。此外，μSPE 还与微型质谱仪在线耦合，使微型质谱仪的灵敏度提高了 10 倍以上。μSPE 和 MS 的结合显着提高了复杂样品分析的检测灵敏度和识别能力。作为一种方便且紧凑的装置，μSPE 可以提高 mini-MS 的分析性能，并有利于其现场应用。