Mixed solid phase extraction column, and preparation method and application thereof

Abstract

The utility model discloses a novel mixed solid phase extraction column used for the preprocessing of pesticide residue; the column is characterized in that the column is filled with three fillers including octadecyl silane, aminopropyl and graphitized carbon; and the filling weight ratio of the octadecyl silane, the aminopropyl and the graphitized carbon is (120-300): (50-80): (4.5-7), preferably, is (150-250): 50: (4.5-7). The invention further discloses a preparation method and an application of the mixed solid phase extraction column. The leaching solvent used in the column is acetonitrile, which is the same as the extracting solvent generally used in pesticide residue detection, so that the purification step is simplified, the solvent exchanging step which is complex, and is possible to cause loss in the pesticide to be detected is eliminated, and the purpose of removing a plurality of interfere substances in only one column filtering process is fulfilled.

Description

technical field [0001] The invention relates to a kind of mixed solid phase extraction column, in particular to a mixed solid phase extraction column used for pretreatment of pesticide residues. The invention also relates to the preparation method and application of the mixed solid phase extraction small column. Background technique [0002] Pesticide residues and organic harmful residues are important factors that affect people's diet, life and health. Governments around the world have formulated many maximum pesticide residue limits (MRLs) for food in order to ensure people's food safety. 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, with the development of mass spectr...

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Problems solved by technology

However, large-volume sampling will cause great pollution to the injection port, increase the frequency of instrument maintenance, and affect the continuous analysis performance of the instrument. Moreover, due to the high price of LVI, some laboratories do not have this sampling system, which makes the application of this method difficult. subject to certain restrictions

The national standard of China contains a pretreatment method using solid phase extraction purification (see GB / T 19648-2006.Method for determination of 500 pesticides and related chemicals residues fruits and vegetables by GC-MS method[S], 2006: 1-48 and GB / T20769-2006.Method for determination of 405 pesticides and related chemicals residues in fruits and vegetables by LC-MS-MS method [S], 2006: 1-58), the amount of the obtained test solution converted to the sample Each 1ml is equivalent to 10g sample, which can reach a lower detection limit, but the sample is pre-treated twice by C18 and graphitized carbon and amino series column, and the two purifications use different eluents respectively. The solid-phase extraction column is eluted with acetonitrile, and the graphitized carbon and amino series column is eluted with toluene + acetonitrile (3+1, v / v). Although a good purification effect is obtained, there are many operating steps and the pretreatment The time is long, which greatly affects the measurement efficiency

[0003] In the Chinese Journal of Health Inspection, the paper "Development of a New Mixed Solid Phase Extraction Column for the Determination of Pesticide Residues" published at 2011 (21) 1:7 discloses a solid phase extraction column, but due to the problem of its ratio, Purification effect is still not satisfactory

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