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A method for online enrichment and analysis of alkaloid compounds

A technology of alkaloids and analysis methods, applied in the field of analytical chemistry, can solve problems affecting analysis accuracy and achieve the effect of improving analysis accuracy and analysis efficiency

Active Publication Date: 2021-08-03
CHINA TOBACCO YUNNAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In addition, the content of some specific alkaloids is at trace level. In conventional chromatographic analysis, after these trace-level substances enter the chromatographic column together with a large amount of solvent in the sample and the mobile phase that transports the sample, their corresponding The chromatographic peak is too weak compared with the corresponding chromatographic peak of the solvent or flow, which also affects the analysis accuracy

Method used

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  • A method for online enrichment and analysis of alkaloid compounds
  • A method for online enrichment and analysis of alkaloid compounds
  • A method for online enrichment and analysis of alkaloid compounds

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Experimental program
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Embodiment

[0037] In order to better illustrate the effect of this method, we conducted a comparative analysis of tobacco samples using the traditional extraction method and this method.

[0038] Sample Preparation:

[0039] 5g of tobacco sample was ultrasonically extracted with 20ml of 50% methanol (adding 1% ammonia water) for 30min, filtered and adjusted to 20ml, and stored in the refrigerator until sample injection.

[0040] The obtained samples were directly analyzed by liquid chromatography, and analyzed by this system.

[0041] The analysis conditions are as follows:

[0042] Direct Chromatographic Analysis Conditions

[0043] Injection volume: 10μl,

[0044] Mobile phase: water (+0.01% triethylamine), acetonitrile (+0.01% triethylamine),

[0045] Flow rate: 1ml / min,

[0046] Gradient: 0~2min, 10% acetonitrile; 2~15min, 10-80% acetonitrile; 15~16.5min, 80% acetonitrile; 16.5~18min, 80-10% acetonitrile

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Abstract

The invention relates to an online enrichment and analysis method of alkaloid substances, comprising the following steps: A. making the first mobile phase carry the sample through a weak cation adsorption column, and adsorb the alkaloid substances and neutral substances in the sample on In the column, the remaining components are discharged with the first mobile phase; B. Use the second mobile phase to flow through the adsorption column. The adsorbed neutral substances are eluted and discharged with the second mobile phase and discarded. The substance still remains in the adsorption column; C. Use the third mobile phase to flow through the adsorption column, elute the alkaloid substance and enter the first collection column after being diluted with a diluent phase, wherein the alkaloid substance is Adsorbed in the first collection column, the third mobile phase is discharged, so accumulated until enough alkaloid substances are adsorbed in the first collection column; D, supplying the fourth mobile phase to the first collection column , to elute the accumulated alkaloids, and enter the analytical chromatographic column with the fourth mobile phase for analysis.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to an online enrichment and analysis method for alkaloid compounds. Background technique [0002] With the deepening of research on actual samples, people often face many complex and changeable matrices. The analysis of this sample brings many difficulties. How to eliminate the interference of matrix and non-target components has become a hot spot in the research of analytical technology. Usually researchers use liquid-liquid extraction, solid-phase extraction and other means to remove the matrix and non-target components in the sample in advance, and then conduct chromatographic analysis. Although the analysis of the target substance in the sample can be effectively realized, the analysis process usually requires a lot of In addition to increasing the burden on researchers, the manual operation is also easy to introduce uncontrollable errors. Therefore, the development of fully...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/08
CPCG01N30/02G01N30/08
Inventor 申钦鹏夏建军刘春波赵辉刘志华李源栋唐石云杨钰婷段沅杏王昆淼赵杨张凤梅司晓喜陈应庄
Owner CHINA TOBACCO YUNNAN IND
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