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      Rapid characterization of complex viscous samples at molecular levels by neutral desorption extractive electrospray ionization mass spectrometry

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      Nature Protocols
      Springer Science and Business Media LLC

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          Abstract

          In this protocol, the sample (which could be a bulk or heterogeneous fluid, or a greasy surface) is treated with a neutral desorption (ND) sampling gas beam, and the resulting analyte mixtures are directly characterized by extractive electrospray ionization mass spectrometry (EESI-MS). The ND device can be specifically constructed such that the sampling gas beam is bubbled through the liquid sample (microjet sampling) or directed to impact the sample surface (e.g., for the analysis of a material like cheese). The ND-EESI-MS analysis process requires no sample pretreatment because it can tolerate an extremely complex matrix. ND-EESI-MS allows real-time, online chemical profiling of highly viscous samples under ambient conditions. Both volatile and nonvolatile analytes from viscous samples can easily be detected and quantified by ND-EESI-MS, thereby providing an MS-based analytical platform for multiple disciplines (e.g., for the food industry, for drug discovery, and for the biological and life sciences). Here we describe the ND-EESI-MS protocol for viscous sample analysis, including the experimental design, equipment setup, reagent preparation, data acquisition and analysis steps. The data collection process takes <1 min per sample, although the time required for the whole procedure, which largely depends on the experimental preparation processes, might be considerably longer.

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          Electrospray ionization for mass spectrometry of large biomolecules

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            Metal chlorides in ionic liquid solvents convert sugars to 5-hydroxymethylfurfural.

            Replacing petroleum feedstocks by biomass requires efficient methods to convert carbohydrates to a variety of chemical compounds. We report the catalytic conversion of sugars giving high yield to 5-hydroxymethylfurfural (HMF), a versatile intermediate. Metal halides in 1-alkyl-3-methylimidazolium chloride are catalysts, among which chromium (II) chloride is found to be uniquely effective, leading to the conversion of glucose to HMF with a yield near 70%. A wide range of metal halides is found to catalyze the conversion of fructose to HMF. Only a negligible amount of levulinic acid is formed in these reactions.
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              Versatile new ion source for the analysis of materials in open air under ambient conditions.

              A new ion source has been developed for rapid, noncontact analysis of materials at ambient pressure and at ground potential. The new source, termed DART (for "Direct Analysis in Real Time"), is based on the reactions of electronic or vibronic excited-state species with reagent molecules and polar or nonpolar analytes. DART has been installed on a high-resolution time-of-flight mass spectrometer (TOFMS) that provides improved selectivity and accurate elemental composition assignment through exact mass measurements. Although DART has been applied to the analysis of gases, liquids, and solids, a unique application is the direct detection of chemicals on surfaces without requiring sample preparation, such as wiping or solvent extraction. DART has demonstrated success in sampling hundreds of chemicals, including chemical agents and their signatures, pharmaceutics, metabolites, peptides and oligosaccharides, synthetic organics, organometallics, drugs of abuse, explosives, and toxic industrial chemicals. These species were detected on various surfaces, such as concrete, asphalt, human skin, currency, airline boarding passes, business cards, fruits, vegetables, spices, beverages, body fluids, horticultural leaves, cocktail glasses, and clothing. DART employs no radioactive components and is more versatile than devices using radioisotope-based ionization. Because its response is instantaneous, DART provides real-time information, a critical requirement for screening or high throughput.
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                Author and article information

                Journal
                Nature Protocols
                Nat Protoc
                Springer Science and Business Media LLC
                1754-2189
                1750-2799
                July 2011
                June 23 2011
                July 2011
                : 6
                : 7
                : 1010-1025
                Article
                10.1038/nprot.2011.337
                21720314
                20bed1e2-9d9e-434b-808b-c2a1b3b813bc
                © 2011

                http://www.springer.com/tdm

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