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Perfluoro acid substance high-sensitivity detecting method assisted by organic proton alkali matrix

A matrix-assisted laser and perfluorinated acid technology, which is applied in the field of analytical chemical detection, can solve the problems of affecting the detection of small molecule targets, contamination of mass spectrometry equipment, matrix shedding, etc., and achieves the effects of convenient detection, high sensitivity and simple operation.

Inactive Publication Date: 2011-09-07
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

Although the above-mentioned matrices can avoid the interference of matrix peaks in low-mass regions to a certain extent, they all have different disadvantages. For example, porphyrin as a matrix can only be used for the study of saturated compounds, while for unsaturated compounds, all protonated peaks are A 14Da shift occurs; 9-aminoazanthracene as a matrix will also form single and double deprotonated matrix ions during the ionization process, and occasionally also form adduct ions such as potassium and sodium, so it will also affect small molecule targets. The detection of nanomaterials as the matrix, the matrix is ​​easy to fall off from the target during the laser excitation process, thus contaminating the mass spectrometry equipment

Method used

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  • Perfluoro acid substance high-sensitivity detecting method assisted by organic proton alkali matrix
  • Perfluoro acid substance high-sensitivity detecting method assisted by organic proton alkali matrix
  • Perfluoro acid substance high-sensitivity detecting method assisted by organic proton alkali matrix

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1, detection perfluorooctane sulfonic acid

[0028] Make 1,8-bis(tetramethylguanidinyl)naphthalene (TMGN) into a 100mmol / mL methanol matrix solution, and mix it with an environmental sample solution containing 1ng / mL perfluorooctanesulfonic acid (PFOS) in equimolar amounts , vortex, centrifuge, take 1 μL of the mixed solution to spot the target, dry at room temperature, put the MALDI stainless steel target with the sample into the MALDI-TOF-MS mass spectrometer for mass spectrometry analysis. Mass spectrometry results such as image 3 As shown in A, the results show that only the negatively charged ion peak (m / z 499.24) of PFOS deprotonation is formed when detected in the negative ion mode of mass spectrometry, and no matrix interference ions appear in the low mass region.

Embodiment 2

[0029] Example 2, detection of perfluorooctanoic acid

[0030] Prepare 1,8-bis(tetramethylguanidinyl)naphthalene as a 100mmol / mL methanol matrix solution, mix with an environmental sample solution containing 20ng / mL perfluorooctanoic acid (PFOA) in equimolar amounts, vortex, centrifuge, and take Spot the target with 1 μL of the mixed solution, dry it at room temperature, put the MALDI stainless steel target with the sample into the MALDI-TOF-MS mass spectrometer for mass spectrometry analysis. Mass spectrometry results such as image 3 As shown in B, the results show that only the negatively charged ion peak (m / z 413.56) of PFOA deprotonation, the decarboxylation ion peak (m / z 369.47) and the removal of 2 F radicals are formed when detected in the negative ion mode of mass spectrometry The decarboxylated ion (m / z 331.42), and no matrix interference ions appeared in the low mass region.

Embodiment 3

[0031] Embodiment 3, detect perfluoromethyl phosphoric acid

[0032] Prepare 1,8-bis(tetramethylguanidinyl)naphthalene as a 100mmol / mL methanol matrix solution, mix with an environmental sample solution containing 20ng / mL perfluoromethylphosphoric acid (PFMPA) in equimolar amounts, and vortex , centrifuge, take 1 μL of the mixed solution to spot the target, dry at room temperature, put the MALDI stainless steel target with the sample into the MALDI-TOF-MS mass spectrometer for mass spectrometry analysis. Mass spectrometry results such as image 3 As shown in C, the results show that only PFMPA deprotonated negatively charged ion peaks (m / z 149.50) are formed when detected in the negative ion mode of mass spectrometry, and no matrix interference ions appear in the low mass region.

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Abstract

The invention discloses a novel matrix of a matrix-assisted laser desorption-ionization flight time mass spectrometry and a method for the mass-spectrometric detection of perfluoro acid substance environmental pollutants by utilizing the same. The matrix 1, 8-di(tetramethyl guanidino) naphthalene has strong alkalinity and the double etramethyl guanidine group has the ability of anchoring a proton to ensure that acid loses the proton to form a negative ion and is convenient for detection in a negative ion mode of the mass spectrum; and meanwhile, the compound has a naphthalene ring structure, can absorb ultraviolet light at wavelengths of 330-350nm and can efficiently assist the ionization of sample molecules. In the invention, the 1, 8- di(tetramethyl guanidino) naphthalene serves as the matrix and is used for the matrix-assisted laser desorption-ionization flight time mass-spectrometric detection of the perfluoro acid substance environmental pollutants; and therefore, the inferior quality region interference problems of matrix peaks can be completely avoided, meanwhile, the problem that a sample is polluted by a perfluor polymer in instrument fittings can be avoided and the method has the advantages of high sensitivity, simpleness and convenience for operation and better salt tolerance.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry detection methods, and relates to a novel substrate for assisting laser desorption ionization time-of-flight mass spectrometry and a method for mass spectrometry detection of perfluorinated acid environmental pollutants. Background technique [0002] Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) technology is to mix the sample to be tested with the matrix compound, and after co-crystallization, under the irradiation of a laser beam of a certain wavelength, the matrix compound absorbs part of the laser energy, and at the same time assists The molecules of the sample to be tested are ionized to form charged sample ions, which are separated by the time-of-flight mass analyzer and then arrive at the detector for detection and analysis. "Soft" ionization mass spectrometry technology. It has been successfully applied in proteomics, genomics, sug...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/64
Inventor 曹冬康跃惠崔琳
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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