Air-flowing type dynamic liquid-phase micro-extracting method for online derivatization

A gas-flow, derivatization technology, applied in the preparation of test samples, etc., can solve the problems of adding derivatization steps of extracts, adverse effects of chromatographic columns, and unsatisfactory analysis results, and achieves the effect of simple operation and easy combination.

Inactive Publication Date: 2013-08-14
YANBIAN UNIV
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Problems solved by technology

However, direct gas chromatography / mass spectrometry analysis of some of the volatile and semi-volatile compounds such as phenolic compounds is not ideal, and it will also cause adverse effects on the chromatographic column. Usually, it is necessary to derivatize the analyte to generate a derivatized product instrumental analysis
Therefore, for such compounds, even the application of airflow dynamic liquid phase microextraction cannot complete the sample pretreatment process in one step, and the derivatization step of the extract needs to be added.

Method used

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  • Air-flowing type dynamic liquid-phase micro-extracting method for online derivatization

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Embodiment Construction

[0019] The specific implementation process is as follows: ① Inert gas 2 is introduced into the sample cell 1 at a certain airflow rate; ② Under the condition of a certain sample cell temperature of 150-300oC, the substance 3 to be measured in the sample matrix is ​​quickly desorbed into the gas phase to form a gaseous The substance to be tested is 4; ③ at the same time, the derivatization reagent 5 is continuously introduced into the sample pool 1, and the derivatization reagent 5 can be selected from silylating reagents, alkylating reagents or acetylating reagents that can react under high temperature and solvent-free conditions , such as trimethylsilane reagent, and vaporize at the sample phase temperature to become the gasified derivatization reagent 6; ④ Under the sample phase temperature condition, the gaseous analyte 4 and the gasified derivatization reagent 6 rapidly The reaction generates the derivatization product 7 of the gaseous substance to be tested; ⑤ driven by th...

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Abstract

The invention discloses an air-flowing type dynamic liquid-phase micro-extracting method for online derivatization. The air-flowing type dynamic liquid-phase micro-extracting method comprises the following steps of: introducing a derivatization reagent to an extracting system when air-flowing type dynamic liquid-phase micro-extracting is carried out on a sample, so that a substance to be tested is quickly subjected to a derivatization reaction in an extracting process; and completing a sample pre-treatment process when a derivatization product enters an extract phase. The air-flowing type dynamic liquid-phase micro-extracting method for online derivatization is a novel sample pre-treatment method which is highly integrated on the basis of the original air-flowing type dynamic liquid-phase micro-extracting method. Compared with the original air-flowing type dynamic liquid-phase micro-extracting method, the air-flowing type dynamic liquid-phase micro-extracting method disclosed by the invention can be used for simplifying the two-step process including extraction and derivatization onto one step, and can be used for the substance which is easy to thermally decompose and is difficult to extract by adopting the original technology. Compared with other derivatization reaction, the derivatization reaction in the air-flowing type dynamic liquid-phase micro-extracting method can be carried out without an independent step and solvent condition. Moreover, the whole technology has the characteristics of being simple to operate, quick, on-line, efficient, integrated, easy to link with a chromatographic system and capable of analyzing in a quantitative manner.

Description

technical field [0001] The invention relates to a sample pretreatment method integrating airflow dynamic liquid phase microextraction and derivatization, in particular to an airflow dynamic liquid phase microextraction method for on-line derivatization. Background technique [0002] In sample analysis, most samples cannot be directly analyzed by instruments. Sample pretreatment is a necessary process before samples are analyzed by instruments, especially for trace / trace components in samples. The sample pretreatment process (mainly including extraction, purification, Concentration and other processes) are particularly important. In recent years, the sample pretreatment technology has developed towards the direction of multi-step integration, multi-functional integration, and multi-technology online combination. The patent "air flow dynamic liquid phase microextraction method" (patent number: CN201010170882.8) improves the extraction efficiency of general microextraction tec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28
Inventor 李东浩王娟
Owner YANBIAN UNIV
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