Novel dispersive solid phase extraction purification tube, its preparation method and use

Abstract

The invention discloses a dispersion solid phase extractive purification tube which is characterized in that the purification tube contains five fillings, namely anhydrous magnesium sulfate, octadecyl silane, aminopropyl, silica gel and graphitized carbon at a mass ratio of (100-200):(20-100):(20-100):(20-100):(7.5-20), preferably (130-170):(30-60):(30-60):(30-60):(7.5-18), most preferably 150:50:50:50:15. The invention also discloses a preparation method and application of the purification tube. Compared with purification filler of the traditional purification tube, the silica gel is added into the purification filler of the purification tube, so that obtained purification liquid is cleaner, the sensitivity and repeatability of pesticide measurement are improved, and the maintenance frequency of an instrument is reduced.

Description

technical field [0001] The invention relates to a novel dispersive solid-phase extraction purification tube, in particular to a dispersive solid-phase extraction purification tube for pesticide residue treatment. The invention also relates to the preparation method and application of the novel dispersed solid phase extraction purification tube. Background technique [0002] Pesticide residues and organic harmful residues are important factors that affect people's diet, life and health. In order to ensure people's food safety, governments around the world have formulated many maximum pesticide residue limits (MRL) for food. At the same time, many countries and regional organizations, such as the United States , a large-scale pesticide residue data monitoring project is carried out every year. Therefore, a reliable, efficient, and multi-residue determination method for pesticides is an important aspect to ensure the safety of people's diet and medication. In recent years, wi...

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Problems solved by technology

Since the developers of the QuEChERS method mostly applied the method to the determination of pesticide residues by gas chromatography-mass spectrometry, most of the data used to evaluate the purification efficiency of the purification materials came from the gas-mass measurement results, and its limitation was that it could not provide - Removal effect of non-volatile interfering components determined by mass spectrometry

In addition, the QuEChERS method or other extraction methods have not completely removed some highly polar components, such as sugars, polysaccharides, amino acids and other components. These compounds have the following problems for liquid mass determination: (i) Compared with other compounds, it will cause a stronger matrix effect (matix effect), which will pollute the ion source and reduce the sensitivity of the instrument; (ii) for gaseous determination, these compounds cannot be vaporized and will be deposited on the injection liner or chromatographic The front end of the column pollutes the gas chromatography system, resulting in a decrease in detection sensitivity, increasing the frequency of maintenance of the chromatography system and inspection costs; (iii) such components will be precipitated in the pre-treatment and concentration steps, affecting subsequent operations, and ultimately affecting the reproducibility of measurement results; For mass spectrometry, such compounds are difficult to gasify, and will deposit on the gas phase inlet at the front end of the gas chromatographic column, resulting in a change in instrument status and a decrease in detection sensitivity

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