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 easy entrainment in sampling, high requirements for operating technology, and poor stability of the hanging drop process, and achieve stable and controllable process, high-magnification enrichment, and reduced Analyzing the effect of detection limits
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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 For the spectrum obtained for the first sample, ...
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. The initial...
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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