研究目的
To simplify the pretreatment process of complex samples for rapid detection using a single-step method involving liquid-phase microextraction on superwetting porous silicon for onsite SALDI-MS analysis.
研究成果
The LPME-SALDI-MS method enables rapid (less than 3 min), sensitive detection of trace analytes in complex samples with wide linear ranges and low LODs. It leverages superwetting PSi for efficient extractant separation, offering advantages in simplicity and sensitivity for applications in environmental monitoring, clinical diagnosis, and forensics.
研究不足
The method is only applicable for binary systems (oil-water mixtures) and analytes with high partition coefficients in water. It cannot handle analytes that require back-extraction into aqueous phase, as in SDME and HF-LPME methods. Potential optimizations include extending to multi-component systems and improving substrate stability.
1：Experimental Design and Method Selection:
The study employs a liquid-phase microextraction (LPME) method combined with surface-assisted laser desorption/ionization mass spectrometry (SALDI-MS) for rapid extraction and detection of analytes from complex samples. The method utilizes a superwetting porous silicon (PSi) substrate to separate organic extractants based on oil-water separation effects, eliminating the need for centrifugation or other complex separation steps.
2：Sample Selection and Data Sources:
Samples include environmental water (lake water spiked with malachite green), biological fluids (human whole blood and urine spiked with verapamil and methadone), obtained from Yan Lake in Jilin University and Fourth Clinical Hospital of Jilin University, respectively. Samples were prepared by serial dilution and stored under specified conditions.
3：List of Experimental Equipment and Materials:
Equipment includes a Hitachi SU8020 Field Emission Scanning Electron Microscope for SEM imaging, Krüss DSA10 MK2 contact angle analyser for contact angle measurements, UV3600 UV-Vis spectrophotometer for absorption spectra, and Autoflex speed TOF/TOF spectrometer for SALDI-MS analysis. Materials include Si wafers, polyvinylpyrrolidone (PVP), trichloro(octadecyl)silane (OTS), verapamil hydrochloride, methadone, malachite green, and various organic solvents.
4：Experimental Procedures and Operational Workflow:
PSi substrates were prepared via metal-assisted etching and modified for superwettability. LPME involved adding organic extraction solvent to sample solutions, vibrating for extraction, immersing the PSi substrate to separate the extractant, and directly analyzing with SALDI-MS. Control samples were prepared by drop-drying without LPME.
5：Data Analysis Methods:
SALDI-MS spectra were obtained with 500 laser shots, and data were analyzed for signal intensity, signal-to-noise ratio, and linearity using coefficients of determination (R2). Statistical analysis included mean and standard deviation calculations.
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Field Emission Scanning Electron Microscope
SU8020
Hitachi
Used for taking SEM images of the substrates.
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UV-Vis spectrophotometer
UV3600
Shimadzu
Used for collecting absorption spectra of substrates.
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TOF/TOF spectrometer
Autoflex speed
Brucker
Used for SALDI-MS analysis to obtain mass spectra.
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Steel plate
MTP 384 polished steel target
Bruker
Used as the target plate for attaching PSi substrates during SALDI-MS detection.
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Si wafers
n type [100]
GRINM Advanced Materials
Used as the base material for preparing porous silicon substrates.
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Contact angle analyser
DSA10 MK2
Krüss
Used for measuring contact angles of water and oil on substrates.
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Filter paper
0.22 μm
Membrane Company
Used for filtering lake water samples to remove particulates.
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