Fast Screening of Low Molecular Weight Compounds by Thin-Layer Chromatography and "On-Spot" MALDI-TOF Mass Spectrometry

Analytical Chemistry

Volumn 76, Issue 7, 2004, Pages 2144-2147

  Santos, Leonardo S ^a   Haddad, Renato ^a   Höehr, Nelci F ^a   Pilli, Ronaldo A ^a   Eberlin, Marcos N ^a  

^a UNIVERSITY OF CAMPINAS   (Brazil)

Author keywords

[No Author keywords available]

Indexed keywords

DESORPTION; IONIZATION; MOLECULAR WEIGHT; ORGANIC ACIDS; THIN LAYER CHROMATOGRAPHY;

IONIC LIQUIDS;

ANTIBIOTICS;

ALKALOID; ALPHA CYANO 4 HYDROXYCINNAMIC ACID; ANESTHETIC AGENT; ANTIBIOTIC AGENT; ARBORESCIDINE; CHEMICAL COMPOUND; IONIC LIQUID; LEVOBUPIVACAINE; MEPIVACAINE; TETRACYCLINE; TRIETHYLAMINE; UNCLASSIFIED DRUG;

ARTICLE; HIGH THROUGHPUT SCREENING; LIQUID; MATRIX ASSISTED LASER DESORPTION IONIZATION TIME OF FLIGHT MASS SPECTROMETRY; MOLECULAR WEIGHT; PHYTOCHEMISTRY; PROTON TRANSPORT; QUALITY CONTROL; SYNTHESIS; TECHNIQUE; THIN LAYER CHROMATOGRAPHY;

ALKALOIDS; ANESTHETICS; ANTI-BACTERIAL AGENTS; BUPIVACAINE; CHROMATOGRAPHY, THIN LAYER; INDOLE ALKALOIDS; INDOLES; MEPIVACAINE; MOLECULAR WEIGHT; PROTONS; SPECTROMETRY, MASS, MATRIX-ASSISTED LASER DESORPTION-IONIZATION; TETRACYCLINE; TIME FACTORS;

EID: 1842580811     PISSN: 00032700     EISSN: None     Source Type: Journal    
DOI: 10.1021/ac035387d     Document Type: Article

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19. 3N·α-CHCA ionic liquid in acetonitrile as well as different volumes dopped into the spot (1-10 μL) have been tested. The best results were obtained for 3-5 μL of a 0.1% (w/v) acetonitrile solution.
20. +. caused drastic reduction in ion formation (sensitivity).
21. Since positive ion MALDI and a proton donor ionic liquid matrix were employed, emphasis has been given to the TMT-MS analysis of basic low-MW compounds. Acid low-MW compounds such as phenols and carboxylic acids should be better ionized by negative ion MALDI.
22. For the tetracycline analysis, spectra subtraction from a side "blank" spot doped with the ionic liquid was beneficial likely due to coelution of impurities from the extracted material obtained from a commercial tablet.
23. Although sensitivity should vary considerably with the analyte, for those tested here, clear mass spectra (a greater than 3 signal-to-noise ratio for the ionized or protonated molecule) were obtained for a limit of 5-10 ng/spot.