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Rapid liquid-phase microextraction of analytes from complex samples on superwetting porous silicon for onsite SALDI-MS analysis
摘要: To simplify the pretreatment process of complex samples is a key step for rapid detection. Herein, we report a single-step method to rapidly extract analytes with liquid-phase microextraction (LPME) from complex samples on a superwetting porous silicon (PSi) for onsite detection with surface-assisted laser desorption/ionization mass spectrometry (SALDI-MS). The operation time is less than 3 min with this simple method. The limit of detection (LOD) of malachite green in lake water is lowered to 10-13 M, that of verapamil and methadone in whole blood is down to 10-11 M and 10-13 M, in urine is 10-13 M and 10-14 M, respectively; and the ranges of quantification is up to 8 or 9 orders of magnitude with high precision (coefficients of determination (R2) > 0.98) for the complex samples. This method could provide an approach to directly extract target compounds from complex samples on substrate for SALDI-MS analysis.
关键词: SALDI-MS,porous silicon,onsite,rapid liquid-phase microextraction,superhydrophobic
更新于2025-09-23 15:22:29
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Enhanced Synergetic Catalytic Effect of Mo <sub/>2</sub> C/NCNTs@Co Heterostructures in Dye-Sensitized Solar Cells: Fine-Tuned Energy Level Alignment and Efficient Charge Transfer Behavior
摘要: This study proposed a new ballpoint connector-protected salt-oil-salt liquid phase microextraction for extraction and enrichment of trace rhein and chrysophanol in rhubarb prior to determination of the analytes by high performance liquid chromatography. In this study, a handy ballpoint connector (between ballpoint tip and ink chamber) was used as extraction device, in which its cavity was filled with n-octanol, and the bare n-octanol in its two opening ends was covered with a thin layer of sodium chloride film. The design subtly assembled salt film onto ballpoint connector for extraction and enrichment, which greatly improved the enrichment factors of the target analytes. Moreover, the novel procedure and its extraction mechanism were described and analyzed, and several crucial parameters reflecting the extraction effect were investigated and optimized. Under optimum conditions, high enrichment factors (247 and 127), good linearities with r ≥ 0.9998, limits of detection (0.6–1.1 ng/mL), relative standard deviations of intra- and interday (2.2–8.8% and 4.3–8.9%), and average recoveries (97.6–98.1%), were obtained, respectively. The proposed method can not only eliminate the negative effects from viscosity and ion strength at high salt concentration of sample phase, but also make salting-out effect be focused on small area so as to maximize the extraction effect.
关键词: high-performance liquid chromatography,rhubarb,liquid-phase microextraction,ballpoint connector,Traditional Chinese medicine
更新于2025-09-11 14:15:04