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Sample preparation method for mass spectrometry

A technology of sample preparation and mass spectrometry, which is applied in the preparation of test samples, analysis materials, material separation, etc., can solve the problems of weak anti-interference ability and unsatisfactory detection sensitivity, and achieve the effect of improving sensitivity

Inactive Publication Date: 2013-03-20
SHIMADZU RES LAB SHANGHAI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In view of the above problems, the present invention provides a sample preparation method suitable for environmental ionization mass spectrometry analysis, which can be used for direct analysis of trace analytes in complex matrices, and solves the problem of unsatisfactory detection sensitivity and weak anti-interference ability in the field of environmental mass spectrometry analysis. question

Method used

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  • Sample preparation method for mass spectrometry

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Weigh 10 mg Ganmaoling tablets into a disposable plastic centrifuge tube (volume 1.5ml), add two steel balls and 1.0ml ethanol, cover the lid, crush the sample on a vibrating ball mill, and extract the target analyte, chlorpheniramine . Take 10 microliters of the resulting suspension along the isosceles triangle filter paper ( Figure 2A Shown) drop evenly at 1.0 cm from the bottom edge.

[0047] Perform paper chromatography. The developer used is ethyl acetate saturated with ammonia water, and it takes about 3 minutes for the developer to climb from the bottom of the isosceles triangular filter paper to the tip. After being developed by the developing agent, the chlorpheniramine added in the Ganmaoling tablet is enriched on the tip of the triangular filter paper, and the tip is placed under the plasma probe of the DCBI ion source, and the target analyte is desorbed from the filter paper and ionized, The generated ions were analyzed by a single quadrupole mass spectr...

Embodiment 2

[0051] In order to measure the content of melamine in milk powder, weigh 10mg of Sanlu milk powder in a disposable plastic centrifuge tube (1.5mL), sample processing and analysis steps are the same as in Example 1. The resulting spectrum is shown in Figure 4 .

Embodiment 3

[0053] In order to determine the content of alkaloids in urine samples, 100 μL of urine was put into a disposable plastic centrifuge tube, and 2 μL of standard solution (ketamine, 10 μg / mL; amphetamine, 10 μg / mL; methamphetamine, 10 μg / mL; methylene di oxyamphetamine, 10 μg / mL), and mix well. Take 10 μL of the above solution and add it dropwise evenly along the distance 1.0 cm from the bottom edge of the isosceles triangular filter paper. The development of filter paper and mass spectrometry analysis are the same as in Example 1. The resulting spectrum is shown in Figure 5 .

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Abstract

The invention provides a sample preparation method for mass spectrometry, aiming to solve the problems of non-ideal detection sensitivity and poor resistance to interference in the field of environmental mass spectrometry. The method comprises the following steps of placing a mixed solution of a sample or specimen and a solvent on chromatography paper, wherein the chromatography paper has an end portion with the width shrunk gradually; performing paper chromatography operation, placing the chromatography paper in a developing solvent to make the sample move toward the end portion of the chromatography paper along with the developing solvent and enrich at the end portion of the chromatography paper; and placing the end portion of the chromatography paper at a detection point of a desorption ionization ion source in a mass spectrometer so as to be desorbed and ionized.

Description

technical field [0001] The invention relates to a method for combining paper chromatography and mass spectrometry, in particular to a sample preparation method for mass spectrometry analysis. Background technique [0002] Environmental ionization (Ambient Ionization) has developed rapidly in recent years. Among them, desorption electrospray ionization (DESI "Science", volume 306, page 471 (2004)) and direct real-time analysis (DART, "Analytical Chemistry" magazine, p. 77 volumes, 2297 pages (2005)) is the most representative. The use of environmental ionization mass spectrometry to analyze trace target substances does not require or only requires simple sample preparation, and shows good application potential in the field of rapid sample analysis. Up to now, various energy carriers such as charged droplets, plasma, ultraviolet light, laser, and heat have been used in ambient ionization techniques. Among them, desorption corona beam ion source technology (DCBI "Analyst" mag...

Claims

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Application Information

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IPC IPC(8): G01N1/34G01N1/40G01N30/90
Inventor 黄云清冯钰锜孙文剑
Owner SHIMADZU RES LAB SHANGHAI
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