Composite solid-phase extraction column used in vegetable pesticide removing, and preparation method thereof

A solid-phase extraction column and extraction technology, which is applied in the field of analytical instruments, can solve the problems of small sampling volume, long purification process, and increased analysis time, and achieve the effects of short purification process time, strong pigment adsorption ability, and solvent saving

Inactive Publication Date: 2012-06-13
CHINESE ACAD OF INSPECTION & QUARANTINE
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

In the detection of pesticide residues, since most vegetable matrices contain more pigments and other interfering substances, matrix interference occurs during the detection of pesticide residues, which affects the accuracy of the determination results, especially for some vegetable samples with high pigment content. The presence of pigment not only interferes with the measurement results, but also greatly damages the chromatographic column of the gas chromatography, shortening the service life of the chromatographic column
[0004] At present, there are many researches on the detection technology of pesticide residues in colored vegetables at home and abroad. AOAC in the United States adopts the QuChERS method to purify vegetable samples. By adding corresponding adsorption materials in the matrix solid-phase dispersion process, the matrix interference components such as pigments can be purified. However, the sampling amount of this method is small (about 0.5g), and the representativeness of the sample is not strong. It is easy to cause the loss of pesticide compounds in the operation process of matrix solid phase dispersion, which makes the measurement results have large deviations, and is used to purify pigments. The PSA adsorption material has a limited adsorption effect on the pigment. If the sampling volume is increased, a better purification effect cannot be achieved, and the high price of PSA is not conducive to the large-scale use in the method.
In addition, there are also reports on methods for purifying pigments and other matrices in vegetable samples by using gel permeation chromatography (GPC). The conventional purification time also takes about 30 minutes, and after GPC purification, it is necessary to perform operations such as concentration and constant volume, which increases the analysis time
In addition, solid phase extraction is also used more at present as a purification means for pesticide residue detection in colored vegetables. Most of them use a single column, and there are a few methods that use a composite solid phase extraction column. Using the composite solid phase extraction column in the present invention, also No other reports

Method used

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  • Composite solid-phase extraction column used in vegetable pesticide removing, and preparation method thereof
  • Composite solid-phase extraction column used in vegetable pesticide removing, and preparation method thereof
  • Composite solid-phase extraction column used in vegetable pesticide removing, and preparation method thereof

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Effect test

Embodiment 1

[0039] 1) Column material and specification

[0040] The specifications of the existing solid-phase extraction empty columns range from 50mg / 1mL to 10g / 60mL, and the column material is polypropylene, equipped with a polyethylene sieve plate with a pore size of 20 μm. All of the above-mentioned column tubes are applicable to the present invention. In the following examples, the present invention uses a 0.5g / 6mL solid-phase extraction empty column.

[0041] 2) The particle size of the adsorbent material

[0042] The particle size of the adsorption material is from 20 μm to 100 μm, which is suitable for the present invention. In the following examples, graphitized carbon black and florisil with a particle size of 40 μm are used.

[0043] 3) Selection of filling volume and filling height

[0044] The filling amount and filling height of the adsorption material determine the performance and column efficiency of the solid phase extraction column. The total mass of the two adsorpti...

experiment example 1

[0046] Purify colored vegetables and complex matrix vegetable samples with the composite solid-phase extraction column in Example 1, the specific process is as follows:

[0047]A. Sample treatment: Take 500.0g of vegetable samples (leeks, green onions, garlic sprouts, spinach, tomatoes), homogeneously pulverize them with a food processor, weigh 5.0g of homogeneous samples into a 50mL polytetrafluoroethylene centrifuge tube, and add 2.0g sodium chloride and 5.0g anhydrous sodium sulfate, then add 25mL ethyl acetate, mix by hand for 30s, shake and extract for 20min, after the extraction is completed, centrifuge at 8000r / min for 10min at 4°C, take the supernatant and Transfer to a 200mL pear-shaped bottle; add the remaining residue to 15mL ethyl acetate and repeat the extraction once again, centrifuge at low temperature, take the supernatant, and combine the extracts. Rotary evaporate the extract at 38°C to nearly dryness, blow dry with nitrogen, dissolve the sample with 2mL of n...

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Abstract

The invention relates to a composite solid-phase extraction column used in vegetable pesticide removing. Graphitized carbon black and florisil are filled in a solid-phase extraction hollow pipe, such that the solid-phase extraction column is obtained. A mass ratio of the florisil to the graphitized carbon black is 1:1-5:1. The invention is suitable for normal-phase extractions of low-pole or middle-pole pesticide compounds, and is especially suitable for organic phosphorus pesticide residue removing of colored vegetables and vegetables with relatively complicated groundmass. Compared to other solid-phase extraction columns with single filling materials, the solid-phase extraction column provided by the invention is advantaged in faster and more convenient processing process, large adsorption capacity, and low solvent dosage. The prices of the florisil and the graphitized carbon black are not high. Commercialized solid-phase extraction hollow pipes are adopted. The preparation method is simple, and is suitable for batch productions.

Description

technical field [0001] The invention belongs to the technical field of analytical instruments, and in particular relates to a composite solid-phase extraction column used for purifying organophosphorus pesticide residues in vegetables. [0002] The present invention also relates to a method for preparing the composite solid phase extraction column. Background technique [0003] my country is a big country in the production and consumption of vegetables. Vegetables are an indispensable food in people's daily life, but they are also one of the foods with serious pesticide pollution. In the detection of pesticide residues, since most vegetable matrices contain more pigments and other interfering substances, matrix interference occurs during the detection of pesticide residues, which affects the accuracy of the determination results, especially for some vegetable samples with high pigment content. The presence of pigment not only interferes with the determination results, but a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/30G01N1/34
Inventor 张峰储晓刚赵延胜王秀娟许成保董英
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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