Sample preprocessing method with pollen as solid phase extractant

A technology of sample pretreatment and solid phase extraction agent, which is applied in the field of analytical chemistry, can solve the problems of long synthesis and preparation process, cumbersome operation, and increased processing time, and achieve good impurity removal effect, simple cleaning method, and simple method Effect

Inactive Publication Date: 2014-12-17
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For solid-phase extraction, the choice of adsorbent is the key. However, the synthesis and preparation process of most adsorbents is long, the operation is cumbersome, and the phase change increases the time of the entire sample pretreatment.

Method used

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  • Sample preprocessing method with pollen as solid phase extractant
  • Sample preprocessing method with pollen as solid phase extractant
  • Sample preprocessing method with pollen as solid phase extractant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Analysis and detection of pollen applied to plant growth regulators in fruits and vegetables

[0025] Eight kinds of common fruits and vegetables (cucumber, bean sprouts, eggplant, tomato, watermelon, peach, apple and pear), respectively weighed 10g of the homogenized vegetable and fruit samples in a 50mL plastic centrifuge tube, added 15mL of acetonitrile solution containing 1% acetic acid, Add 1.5g of sodium acetate, 6g of magnesium sulfate, and 10g of sodium chloride, vortex and extract for 5min, centrifuge at 9000r / min for 10min, and take the supernatant for testing.

[0026] Accurately weigh 0.4g of pollen into a 3mL solid-phase extraction empty column tube with a sieve plate, beat continuously to fill it evenly, cover the upper end with a sieve plate and press it tightly; 10, v / v) solution and 2mL of acetonitrile pass through the solid phase extraction column in turn, the flow rate is less than 1mL / min; then add the above 1mL vegetable and fruit acetoni...

Embodiment 2

[0034] Embodiment 2: pollen is applied to the extraction analysis of resveratrol in peanut oil

[0035] Weigh 2g of six common peanut oils into a 10mL volumetric flask, add n-hexane to dilute to the mark, and set aside.

[0036] Accurately weigh 0.3g pollen into a 3mL solid-phase extraction empty column tube with a sieve plate, beat continuously to fill it evenly, cover the upper end with a sieve plate and press it tightly; under the negative pressure of the vacuum pump, add 3mL acetone and 2mL n-hexane Through the solid-phase extraction column, the flow rate is less than 1mL / min; then 2mL of the above-mentioned sample solution is added to the solid-phase extraction column, so that it slowly flows through the extraction column under the action of gravity; then add 3mL of n-hexane / isopropanol (80 / 12, v / v) solution is used as the cleaning solution, keep the flow rate less than 1mL / min through the extraction column to remove the residual matrix adsorbed on the column, and drain ...

Embodiment 3

[0039] Embodiment 3: pollen is applied to the content determination of insecticide in environmental water sample

[0040] Five kinds of environmental water samples (river, river, lake, tap water and farmland water) were used to filter the sediment through the filter membrane for later use.

[0041] Accurately weigh 0.3g pollen into a 3mL solid-phase extraction empty column tube with a sieve plate, beat continuously to fill it evenly, cover the upper end with a sieve plate and press it tightly; under the negative pressure of the vacuum pump, mix 3mL acetone and 2mL pure water Through the solid phase extraction column, the flow rate is less than 1mL / min; then add 10mL of the above water sample to the solid phase extraction column, keep the flow rate less than 1mL / min and flow through the extraction column; then add 5mL pure water as a cleaning solution, keep the flow rate less than 1mL / min through the extraction column to remove the residual matrix adsorbed on the column, and d...

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Abstract

The invention relates to a sample preprocessing method with natural pollen as solid phase extractant. The method comprises performing Soxhlet extraction and cleaning through polar solvent and then drying to obtain pollen materials. The material cleaning method is simple, safe and easy to implement, and the raw materials are cheap and easy to obtain. Materials obtained through the material cleaning method are high in reproducibility, can be taken as solid phase extracting fillings for separation and enrichment of polar compounds and Pi-electron compounds of plant, food, environmental and biological samples and have the advantages of being good in impurity removing effects, high in recovery rate, good in stability and the like.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry and relates to a sample pretreatment method using natural product pollen as an adsorption medium for solid phase extraction. Background technique [0002] Solid phase extraction (solid phase extraction, solid phase extraction) is a sample pretreatment method that has developed rapidly in recent years. of. Compared with traditional liquid-liquid extraction, solid-phase extraction has the advantages of simplicity, time saving, non-emulsification, low consumption of organic solvents, etc., and can meet the analysis requirements of high recovery and high sensitivity at the same time, so it is widely used in complex matrices Extraction detection of medium and trace analytes. For solid-phase extraction, the choice of adsorbent is the key. However, the synthesis and preparation process of most adsorbents is long, the operation is cumbersome, and the phase change increases the time of the e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/34G01N1/40G01N30/08
Inventor 冯钰锜卢倩余琼卫
Owner WUHAN UNIV
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