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An integrated dispersive solid-phase extraction device and sample pretreatment method

A sample pretreatment and extraction device technology, which is applied in the direction of measurement devices, test sample preparation, material separation, etc., can solve problems such as leakage of the solution to be tested, difficult targets, and low separation efficiency

Active Publication Date: 2021-09-14
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, small column extraction technology (SPE), tube tip solid phase extraction technology (PT-SPE) and filter tip solid phase extraction technology (FT-SPE) are usually used. Among them, small column extraction technology (SPE) requires manual loading of adsorbents. Difficult to fill evenly, which will cause large errors in the extraction and separation process, and there will be incomplete adsorption and desorption, and the recovery rate will be low; the inner diameter of the tip solid phase extraction device is too small, and the flow path of the sample to be tested is very narrow. The contact time between the substance and the adsorbent is increased, and the adsorption rate and recovery rate are high, but the extraction and separation time is also greatly increased, and the separation efficiency is low; the cross section of the solid phase extraction device of the filter head is large, and the adsorbent is not easy to spread evenly in the device , it is difficult to fully contact with the target, and it is easy to leak the adsorbent or the solution to be tested. This method has a large relative standard deviation and the recovery rate is unstable.
[0004] In addition, after the dispersive solid-phase extraction method reaches the adsorption equilibrium, more complex means are needed to separate the adsorbent from the analyte, and since the extraction process is carried out in an open system, the volatilization of organic reagents will affect the health of analysts. cause harm

Method used

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  • An integrated dispersive solid-phase extraction device and sample pretreatment method
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  • An integrated dispersive solid-phase extraction device and sample pretreatment method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Take 10 mg of hydrophobic commercial adsorbent filler C 18 Add it into a 10 mL sample bottle, spread the 0.22 μm nylon microporous filter membrane on the bottle mouth, set the rubber stopper on the filter membrane at the bottle mouth of the sample bottle, and press down to make the filter membrane, rubber stopper and bottle mouth Closely fit; insert the catheter into the separation chamber from the first through hole located in the center of the bottle stopper; insert the fluid introduction part, that is, the needle of a 1.0mL syringe with a needle, into the extraction chamber along the second through hole, which is set on the rubber stopper On the wall of the stopper neck, the integrated dispersive solid phase extraction device is assembled.

[0059] Use a syringe to draw 1.0 mL of promethenil standard solution with a concentration of 5 μg / mL into the sample bottle, place it in an ultrasonic instrument for ultrasonic treatment for 30 s, and then vortex with a vortex os...

Embodiment 2

[0062] Using the integrated dispersive solid-phase extraction device basically the same as in Example 1, the hydrophobic commercial adsorbent filler C in Example 1 was replaced with 10 mg of hydrophilic commercial adsorbent filler activated silica gel 18 .

[0063] Use a syringe to draw 1.0 mL of diethylstilbestrol standard solution with a concentration of 5 μg / mL into the sample bottle, place it in an ultrasonic instrument for ultrasonic treatment for 30 s, and then vortex with a vortex oscillator for 30 s to rapidly mix the adsorbent with the standard solution. Use a syringe to draw 1.0 mL of nitrogen and inject it into the sample bottle, so that the internal pressure is higher than the external environment to form a positive pressure environment, so that the standard solution enters the separation chamber from the extraction chamber through the filter membrane, and finally flows out along the catheter to achieve Rapid separation of sorbent and sample solution.

[0064] Aft...

Embodiment 3

[0066] Using the integrated dispersive solid-phase extraction device basically the same as in Example 1, 10 mg of hydrophilic and lipophilic commercial adsorbent filler HLB was used to replace the hydrophobic-type commercial adsorbent filler C in Example 1 18 .

[0067] Use a syringe to draw 1.0 mL of sulfamethoxazole standard solution with a concentration of 5 μg / mL into the sample bottle, place it in an ultrasonic instrument for ultrasonic treatment for 30 s, and then vortex with a vortex oscillator for 30 s to make the adsorbent and standard solution Mix quickly for full contact; use a syringe to draw 1.0 mL of helium and inject it into the sample bottle, so that the internal pressure is higher than the external environment to form a positive pressure environment, so that the standard solution enters the separation chamber from the extraction chamber through the filter membrane, and finally along the catheter Flow out to realize the rapid separation of the adsorbent and the...

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Abstract

The invention provides an integrated dispersive solid-phase extraction device and a sample pretreatment method. The integrated dispersive solid-phase extraction device includes a sample bottle, a bottle stopper, a separator, a conduit, a fluid introduction part and an adsorbent. The extraction chamber and the separation chamber are formed inside the sample bottle with the separation part, and the separation of the sample solution and the adsorbent is realized by using the pressure difference. The device of the present invention has the advantages of simple structure, low cost, easy assembly, simple and safe extraction method, rapid separation of liquid and solid, and is safe and environmentally friendly. It is suitable for various types of solid adsorbents and is expected to be applied to complex samples such as food, environment and biology. Extraction and separation of trace components.

Description

technical field [0001] The invention relates to the field of extraction and separation of food, environment and biological sample components, in particular to an integrated dispersive solid-phase extraction device and a sample pretreatment method. Background technique [0002] With the continuous development of analytical chemistry, people have higher and higher requirements for the detection of trace substances in complex sample systems such as food, environment, and biology. However, in the analysis process, due to the diversity, complexity and Due to the characteristics of low component content, it is necessary to carry out appropriate physical or chemical pretreatment on the sample before using the instrument for determination. Currently commonly used sample pretreatment techniques include solid-phase extraction, dispersive solid-phase extraction, solid-phase microextraction, and membrane separation extraction. Among them, dispersive solid-phase extraction technology is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28G01N30/06
CPCG01N1/28G01N30/06
Inventor 闫宏远司润生王明伟韩晔红乔凤霞韩丹丹
Owner HEBEI UNIVERSITY
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