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Slug flow microextraction-paper spray mass spectrometry technology

A technology of electrospray mass spectrometry and slug flow, applied in the field of analytical chemistry, can solve problems such as limited organic solvents, difficulty in taking into account extraction efficiency and ionization effect at the same time, and reduced sensitivity of analytical methods

Inactive Publication Date: 2017-02-15
SUN YAT SEN UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, this method also has certain shortcomings. The extraction solvent of SFME-nanoESI-MS is also a spray solvent, which makes the selection of organic solvents extremely critical. It must be immiscible with biological fluid samples and have good properties for target analytes. Solubility, but also suitable for nanoESI-MS analysis, the organic solvents that can meet the above requirements at the same time are very limited, which makes it difficult to take into account the extraction efficiency and ionization effect in the analysis process, resulting in a decrease in the sensitivity of the analysis method

Method used

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Examples

Experimental program
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Embodiment 1

[0067] Rapid analysis of amphetamine drugs in blood and urine by SFME-PS-MS in embodiment 1

[0068] This embodiment has selected three kinds of amphetamine drugs that the World Anti-Doping Agency (WADA) and the United Nations Office on Drugs and Crime (UNODC) give priority to control, namely amphetamine (AM), methamphetamine (MA), methylene dioxygen Methyl methamphetamine (MDMA) was used as the research object, and the SFME-PS-MS analysis method of these three amphetamine drugs in whole blood and urine was established.

[0069] Experimental steps:

[0070] In the experiment, the parameters are firstly optimized. In general, the key parameters of SFME-PS-MS include SFME extraction solvent, SFME extraction times, and PS-MS spray solvent. In the experiment, 50 μg / L of AM, MA and MDMA were added to whole blood samples to study the influence of different conditions on the analysis results. The analysis adopts the internal standard method, and 500 μg / L caffeine is added to the s...

Embodiment 2

[0084] Example 2 SFME-PS-MS and PS-MS are used for the analysis of amphetamine drugs in whole blood respectively

[0085] In order to compare the sensitivity of SFME-PS-MS and PS-MS for analyzing whole blood samples, the same 50 μg / L AM, MA and MDMA whole blood spiked samples were analyzed by both methods, and 500 μg / L caffeine in acetonitrile was used as Internal standard.

[0086] For the analysis method of SFME-PS-MS see Example 1, for the analysis method of PS-MS see J.Liu, H.Wang, N.E.Manicke, J.M.Lin, R.G.Cooks, Z.Ouyang, Anal.Chem.2010,82,2463 –2471..

[0087] Only very weak AM, MA and MDMA mass spectrum signals can be observed in the PS-MS spectrum, accompanied by a large number of matrix signals ( Figure 5 ). However, the SFME-PS-MS spectra showed significantly higher target compound signals and lower matrix signals ( image 3 a). Compared with PS-MS, SFME-PS-MS can significantly improve the analytical sensitivity of AM, MA and MDMA in whole blood, and reduce th...

Embodiment 3

[0088] Example 3 SFME-PS-MS and SFME-nanoESI-MS are used for the analysis of amphetamine drugs in body fluids respectively

[0089] In order to compare the performance of SFME-PS-MS and SFME-nanoESI-MS in the analysis of amphetamines in whole blood samples, the two methods were analyzed in the same whole blood spiked sample with 50 μg / L AM, MA and MDMA, and 500 μg / L L caffeine in acetonitrile was used as internal standard.

[0090] For the analysis method of SFME-PS-MS, please refer to Example 1. For the analysis method of SFME-nanoESI-MS, please refer to Y.Ren, M.N.McLuckey, J.Liu, Z.Ouyang, Angew.Chem.Int.Ed.2014,53,14124 -14127.

[0091] Such as Figure 6 As shown, the signals of the three target compounds in the SFME-nanoESI-MS spectra are better than those in PS-MS, but not as ideal as in SFME-PS-MS. In the SFME-nanoESI-MS method, chloroform is the best extraction / spray solvent. Due to the lower ionization efficiency of chloroform than acetonitrile, SFME-nanoESI-MS is...

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Abstract

The invention belongs to the field of analytical chemistry, and relates to slug flow microextraction-paper spray mass spectrometry technology (SFME-PS-MS) and a system and application of the technology. According to the SFME-PS-MS technology, a capillary is adopted to fast extract and gather a trace compound from a complex base sample, the extracted liquid is dropwise added to paper, the obtained paper is allowed to be close to an entrance of mass spectrometry after an extraction solvent is dried through volatilization, the direct-current high-pressure electric field is applied to the paper, a spray solvent is dropwise added to the paper, and the target compound is desorbed and ionized in the action of the electric field and the spray solvent and enters the mass spectrometry for analysis. New microextraction and normal-pressure ambient mass spectrometry technology is developed, so that the trace compound in a complex biological and environmental sample can be fast, sensitively and accurately analyzed.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and relates to a combined technique of slug flow microextraction-paper-based electrospray mass spectrometry (SFME-PS-MS) for analyzing compounds in complex matrices. Background technique [0002] Liquid phase microextraction (Liquid Phase Microextraction, LPME) is a new type of sample pretreatment technology, which extracts the target substance from the sample into the extraction solvent according to the distribution coefficient of the target substance in the sample and the extraction solvent. It provides sensitivity and enrichment comparable to liquid-liquid extraction. At the same time, this technology integrates extraction, purification and concentration, and is easy to operate, and also has the characteristics of rapidity and low cost, and is especially suitable for the analysis and detection of small sample volumes. In addition, it uses very little organic solvent and is an environmentall...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N27/62
CPCG01N27/62G01N30/02G01N30/06G01N2030/062
Inventor 邓洁薇杨运云刘洪涛栾天罡
Owner SUN YAT SEN UNIV
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