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Direct characterization of bulk samples by internal extractive electrospray ionization mass spectrometry.

Zhang H, Gu H, Yan F, Wang N, Wei Y, Xu J, Chen H - Sci Rep (2013)

Bottom Line: The method allows both qualitative and quantitative analysis of analytes distributed in a 3-dimensional volume (e.g., 1 ~ 100 mm(3)) of various synthetic and biological matrices (e.g., chewing gum, leaves, fruits, roots, pork, lung tissues) without either mashing the sample or matrix separation.Using different extraction solvents, online chromatographic separation of chemicals inside the sample volume was observed during iEESI-MS analysis.The presented method is featured by the high speed of analysis, high sensitivity, low sample consumption and minimal sample preparation and/or degradation, offering unique possibilities for advanced applications in plant science, clinical diagnosis, catalyst studies, and materials science.

View Article: PubMed Central - PubMed

Affiliation: Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation, East China Institute of Technology, Nanchang, Jiangxi 330013, China.

ABSTRACT
A straight-forward analytical strategy called internal extractive electrospray ionization mass spectrometry (iEESI-MS), which combines solvent extraction of chemicals inside a bulk sample with in situ electrospray ionization mass spectrometry, has been established to directly characterize the interior of a bulk sample with molecular specificity. The method allows both qualitative and quantitative analysis of analytes distributed in a 3-dimensional volume (e.g., 1 ~ 100 mm(3)) of various synthetic and biological matrices (e.g., chewing gum, leaves, fruits, roots, pork, lung tissues) without either mashing the sample or matrix separation. Using different extraction solvents, online chromatographic separation of chemicals inside the sample volume was observed during iEESI-MS analysis. The presented method is featured by the high speed of analysis, high sensitivity, low sample consumption and minimal sample preparation and/or degradation, offering unique possibilities for advanced applications in plant science, clinical diagnosis, catalyst studies, and materials science.

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Related in: MedlinePlus

Separation effects observed in iEESI-MS.a) a typical mass spectrum recorded after 60 min from the beginning of the experiment; b) a typical mass spectrum recorded after 80 min; c) selected chromatographic traces of aniline (m/z 94) and methylene blue dye (m/z 284) solution spiked into a fresh radish taproot sample.
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f4: Separation effects observed in iEESI-MS.a) a typical mass spectrum recorded after 60 min from the beginning of the experiment; b) a typical mass spectrum recorded after 80 min; c) selected chromatographic traces of aniline (m/z 94) and methylene blue dye (m/z 284) solution spiked into a fresh radish taproot sample.

Mentions: Interestingly, distinct separation of analytes extracted by the ESI solvent was observed when the distance between the tip of the ESI capillary and the sample edge was increased (≥5 mm). The iEESI-MS spectra of a chewing gum were continuously recorded using methanol as the extraction solvent. The time required to detect analytes originated from the chewing gum varied dramatically from 20 s to 60 min, depending on the distance of between the ESI tip and the sample edge, the solvent flow rate, air temperature and humidity. With low flow rates (1 μL/min), long distance (10 mm) and dry ambient air (25°C, 20–25% R.H.), it took 60 min to observe a chewing gum spectrum (Fig. 4a). The spectral pattern was unchanged for about 20 min, during which the mass spectra was dominated by low-mass signals (e.g., protonated menthone, m/z 155), probably because the small polar chemicals were relatively more volatile than the chemicals detected later on. The spectrum recorded after 80 min, on the other hand, revealed abundant signals of large chemicals including polymer molecules (Fig. 4b), suggesting significant chromatographic effects on the time scale of iEESI experiment. With high flow rates (4 μL/min), short distance (4 mm) and humid ambient air (25°C, 65% R.H.), only 20 s was required for iEESI to record the first spectrum (Fig. S7a) of a chewing gum sample, which shows the spectral pattern similar to that in Fig. 4a. Under the same conditions, polymer signals (Fig. S7b) were abundantly detected after 4 min by iEESI-MS from the same chewing gum sample.


Direct characterization of bulk samples by internal extractive electrospray ionization mass spectrometry.

Zhang H, Gu H, Yan F, Wang N, Wei Y, Xu J, Chen H - Sci Rep (2013)

Separation effects observed in iEESI-MS.a) a typical mass spectrum recorded after 60 min from the beginning of the experiment; b) a typical mass spectrum recorded after 80 min; c) selected chromatographic traces of aniline (m/z 94) and methylene blue dye (m/z 284) solution spiked into a fresh radish taproot sample.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC3750536&req=5

f4: Separation effects observed in iEESI-MS.a) a typical mass spectrum recorded after 60 min from the beginning of the experiment; b) a typical mass spectrum recorded after 80 min; c) selected chromatographic traces of aniline (m/z 94) and methylene blue dye (m/z 284) solution spiked into a fresh radish taproot sample.
Mentions: Interestingly, distinct separation of analytes extracted by the ESI solvent was observed when the distance between the tip of the ESI capillary and the sample edge was increased (≥5 mm). The iEESI-MS spectra of a chewing gum were continuously recorded using methanol as the extraction solvent. The time required to detect analytes originated from the chewing gum varied dramatically from 20 s to 60 min, depending on the distance of between the ESI tip and the sample edge, the solvent flow rate, air temperature and humidity. With low flow rates (1 μL/min), long distance (10 mm) and dry ambient air (25°C, 20–25% R.H.), it took 60 min to observe a chewing gum spectrum (Fig. 4a). The spectral pattern was unchanged for about 20 min, during which the mass spectra was dominated by low-mass signals (e.g., protonated menthone, m/z 155), probably because the small polar chemicals were relatively more volatile than the chemicals detected later on. The spectrum recorded after 80 min, on the other hand, revealed abundant signals of large chemicals including polymer molecules (Fig. 4b), suggesting significant chromatographic effects on the time scale of iEESI experiment. With high flow rates (4 μL/min), short distance (4 mm) and humid ambient air (25°C, 65% R.H.), only 20 s was required for iEESI to record the first spectrum (Fig. S7a) of a chewing gum sample, which shows the spectral pattern similar to that in Fig. 4a. Under the same conditions, polymer signals (Fig. S7b) were abundantly detected after 4 min by iEESI-MS from the same chewing gum sample.

Bottom Line: The method allows both qualitative and quantitative analysis of analytes distributed in a 3-dimensional volume (e.g., 1 ~ 100 mm(3)) of various synthetic and biological matrices (e.g., chewing gum, leaves, fruits, roots, pork, lung tissues) without either mashing the sample or matrix separation.Using different extraction solvents, online chromatographic separation of chemicals inside the sample volume was observed during iEESI-MS analysis.The presented method is featured by the high speed of analysis, high sensitivity, low sample consumption and minimal sample preparation and/or degradation, offering unique possibilities for advanced applications in plant science, clinical diagnosis, catalyst studies, and materials science.

View Article: PubMed Central - PubMed

Affiliation: Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation, East China Institute of Technology, Nanchang, Jiangxi 330013, China.

ABSTRACT
A straight-forward analytical strategy called internal extractive electrospray ionization mass spectrometry (iEESI-MS), which combines solvent extraction of chemicals inside a bulk sample with in situ electrospray ionization mass spectrometry, has been established to directly characterize the interior of a bulk sample with molecular specificity. The method allows both qualitative and quantitative analysis of analytes distributed in a 3-dimensional volume (e.g., 1 ~ 100 mm(3)) of various synthetic and biological matrices (e.g., chewing gum, leaves, fruits, roots, pork, lung tissues) without either mashing the sample or matrix separation. Using different extraction solvents, online chromatographic separation of chemicals inside the sample volume was observed during iEESI-MS analysis. The presented method is featured by the high speed of analysis, high sensitivity, low sample consumption and minimal sample preparation and/or degradation, offering unique possibilities for advanced applications in plant science, clinical diagnosis, catalyst studies, and materials science.

Show MeSH
Related in: MedlinePlus