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Hanging drop type liquid-liquid micro-extraction method

A hanging drop extraction technology, applied in the field of material separation and analysis, can solve the problems of high operational technology requirements, poor stability of the hanging drop process, easy sampling entrainment, etc., to achieve stable and controllable process, lower analysis detection limit, lower Analyze cost effects

Inactive Publication Date: 2007-07-18
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with SPME, the LPME method based on hanging drop technology has high mass transfer efficiency, low price, good reproducibility, and is easy to be used with various instruments. high requirements

Method used

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  • Hanging drop type liquid-liquid micro-extraction method
  • Hanging drop type liquid-liquid micro-extraction method
  • Hanging drop type liquid-liquid micro-extraction method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Decoct with water to obtain the extract of Scutellaria baicalensis, a traditional Chinese medicine. Divide the extract into two portions. The first part was filtered through a 0.2 μm microporous membrane, diluted 10 times with methanol, and 2 μL was drawn for HPLC analysis. The second part is treated with hanging drop liquid-liquid microextraction, the steps are as follows: take 10 μL of the extract and place it in a jacketed extraction bottle, add deionized water to dilute to 100 times, and pass through the jacket of the extraction bottle with a super constant temperature Water at 25°C provided by the water bath, start the stirring device to stabilize the stirring frequency at 10s -1 ; Take 10 μL of n-octanol as the extractant, drop it into the extraction bottle and start timing; when the timing reaches 300 s, use a micro sampler to draw 2 μL of the extract phase from the suspension droplet for HPLC analysis. Figure 2 is the spectrum obtained from the first sample, i...

Embodiment 2

[0036] The extract of Scutellaria baicalensis, a traditional Chinese medicine, was extracted with ethanol, and the concentration of baicalein was 462.3mg / L. Take 0.1, 0.3, 0.5, 0.7, 0.9mL respectively and place them in a 100mL volumetric flask, add deionized water to dilute to the mark, and prepare the sample solution. Carry out hanging drop liquid-liquid microextraction on the sample liquid, the steps are as follows: take 1000 μL of the extract and place it in a jacketed extraction bottle, pour water at 25°C provided by a super constant temperature water bath into the jacket of the extraction bottle, and start stirring The device stabilizes the stirring frequency at 1s -1 Take 2 μL of the extractant n-octanol, drop it into the extraction bottle and start timing; when the timing reaches 3600s, use a micro sampler to draw 1 μL of the extract phase from the suspension drop, and measure the concentration of baicalein in it with high performance liquid chromatography. Figure 4 wa...

Embodiment 3

[0038] Take 5 g of rhubarb, a traditional Chinese medicine, soaked in 100 mL of water for 24 hours, and then filter with filter paper to obtain a clarified rhubarb extract. Take 1mL, 2mL, 3mL, 4mL, and 10mL extract respectively, add deionized water to make up to 100mL, and obtain the sample solution. Perform hanging drop liquid-liquid micro-extraction on the sample liquid, the steps are as follows: take 5000 μL of the sample liquid and place it in a jacketed extraction bottle, pour water at 25 °C provided by a super constant temperature water bath into the jacket of the extraction bottle, and start The stirring device stabilizes the stirring frequency at 50s -1 ; Take 100 μL of extractant benzene, drop it into the extraction bottle and start timing; when the timing reaches 300s, use a micro sampler to draw 50 μL of the extract phase from the suspension drop, add it to the cuvette, and take another 1000 μL of 1% acetic acid Magnesium methanol solution is injected into the cuve...

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Abstract

The invention discloses a pendent drop liquid-liquid extraction method, which adds un-analyzed liquid sample in the extraction bottle with agitating, and quantitatively abstract extraction agent and drop it on the sample liquid. When the time is up to the setting time, use sampler to absorb the extraction agent, and use the analyzing instrument to detect. The method of the invention needs little amount of sample and can effectively exclude the interference of co-existing components of the compled samples to realize high multiplying factor gathering and to lower the analyzing limit and cost. It is very convenient for the invention to unite all kinds of chromatogram, spectrum and electro-chemical analyzing method. The invention can be utilized to food safety detection, environmental monitoring, natural resources extraction and the analyzing procedure of medicine and chemicals' manufacturing. The invention has strong technological priority and wide utilization foreground.

Description

technical field [0001] The invention relates to a hanging drop liquid-liquid micro-extraction method, in particular to a hanging drop liquid-liquid micro-extraction method for analyzing sample pretreatment, and belongs to the technical field of material separation and analysis. Background technique [0002] High-efficiency analysis and detection methods characterized by rapidity and high selectivity are necessary conditions for realizing clean production and improving the quality of life. With the continuous improvement of the degree of social modernization, people have put forward higher requirements for the analysis process applied in the fields of food safety testing, environmental monitoring, and quality control of traditional Chinese medicine. The systems involved in these processes all have the characteristics of complex systems with many interference components and low content of target substances, so direct quantitative analysis is very difficult. The key to realizi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D11/04G01N1/28
Inventor 吕阳成林泉骆广生戴猷元
Owner TSINGHUA UNIV
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