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Monolithic column solid phase extraction sample pretreatment method

A sample pretreatment and monolithic column technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems affecting the analysis speed and practical application value, the reduction of the detection limit of the enrichment multiple, and the impact on the sample analysis speed, etc., to improve the actual Applied value, shortened extraction time, effects of cheaper items

Inactive Publication Date: 2010-10-13
HUAZHONG NORMAL UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] (1) Capillary tubes (0.10-0.53mm) and PEEK tubes (micron grade) have small inner diameters and small extraction capacity, which limits the further improvement of the enrichment factor and the further reduction of the detection limit, making the sensitivity low
[0006] (2) When the capillary is used, the extraction flow rate is low (generally 0.04mL / min), which affects the sample analysis speed
[0007] (3) Due to the small inner diameter of the integral column and the long column length (1-3 cm), when the solution passes through, the back pressure is very large, which affects the analysis speed and practical application value

Method used

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  • Monolithic column solid phase extraction sample pretreatment method
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  • Monolithic column solid phase extraction sample pretreatment method

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Embodiment Construction

[0032] Examples of the monolithic column solid phase extraction sample pretreatment method device are as follows: figure 1 As shown, the monolithic column solid phase extraction device consists of a syringe 1 and a sieve plate 3 .

[0033] Determination of Aldehyde Compounds in Serum by This Method

[0034] The configuration consists of 0.024g of monomeric methacrylic acid, 0.43g of crosslinking agent ethylene glycol dimethacrylate, 0.05g of photoinitiator 1-hydroxycyclohexyl phenyl ketone, and binary porogen toluene 0.093 g, 0.43 g of dodecyl alcohol was mixed with the precursor solution obtained by ultrasound.

[0035] Add 12 μL of the prepared precursor solution dropwise onto a polypropylene sieve plate with a diameter of 4.8 mm and a thickness of 1.6 mm, and irradiate for 90 seconds under a high-pressure mercury lamp with a wavelength of 365 nm to synthesize the monolithic column material in situ on the sieve. board. The scanning electron micrographs of the blank sieve ...

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Abstract

The invention discloses a monolithic column solid phase extraction sample pretreatment method, which comprises the following steps of: 1) taking a 1-milliliter syringe and a sieve plate, wherein the sieve plate has the diameter of 4.8 millimeters, the thickness of 1.6 millimeters and micron-sized pores; 2) synthesizing the material of a monolithic column on the sieve plate, stuffing the sieve plate serving as a fixed phase into the 1-milliliter syringe, injecting sample solution serving as a liquid phase from the tail end of the syringe, pushing the solution, and enriching target analytes in the sample solution by using the material of the monolithic column on the sieve plate; and 3) analyzing the target analytes enriched on the sieve plate of the monolithic column by using analytic liquid, and performing high resolution liquid chromatographic separation detection. The monolithic column solid phase extraction method has the advantages of high extraction capacity, low extraction backpressure, effectively shortening of extraction time, high extraction efficiency, high detection sensibility, simple operation, good repeatability, and suitability for extracting and enriching trace components in complicated sample matrixes.

Description

technical field [0001] The invention relates to an integral column solid-phase extraction method for analysis sample pretreatment. Background technique [0002] The analysis and monitoring of substances in complex matrices has always been concerned by analysts. The commonly used detection methods include liquid phase microextraction (LLE), liquid membrane extraction (LMP), solid phase microextraction (SPME), solid phase extraction (SPE) and so on. Compared with liquid phase extraction and SPE, SPME technology is a relatively new green sample pretreatment method. This method was first proposed by Arthur and Pwahsyzn in 1990. It integrates sampling, enrichment, and sample injection and uses less organic solvents. , so it is widely used. There are two types of solid phase microextraction: exposed stationary phase and in-tube solid phase microextraction. In recent years, analysts started from the separation medium itself, developed a new generation of separation medium - mono...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/60G01N30/02
Inventor 徐晖闫志华王淑余辜艳琴梁璐
Owner HUAZHONG NORMAL UNIV
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