Method for simultaneously accumulating, enriching and separating multiple arsenic forms in natural medicine on line based on micelle-solvent accumulation
A technology of natural medicine and separation method, which is applied in the preparation of test samples, etc., can solve the problem of reduced sensitivity of capillary short light path injection volume, achieve rapid detection, efficient detection and separation, and improve sensitivity
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Embodiment 1
[0074] Embodiment 1. Investigate the influence of micelle species on detection effect
[0075] Wash and dry the kelp, crush and pass through a 100-mesh sieve, then accurately weigh 200 mg of each sample and place it in a 15 mL centrifuge tube, add 5 mL of 2% HNO 3 , sonicated for 1h (40°C), then shaken at room temperature for 2h, and finally centrifuged at 4000r / min for 15min. Extracts were neutralized with NaOH prior to analysis.
[0076] Fused silica capillaries were coated with 1% hemexonium bromide (HDMB) for 20 min to satisfy the condition of the same EOF orientation between anions and capillaries. The activated capillary column was rinsed with 100 mM borax buffer pH 9.2 for 5 minutes before injection. In the capillary column, 10mM micelles and 10mg / L target analyte were mixed and injected into the stack as a sample solution at -10kV for 60s, and then 100% MeOH5s was injected at -10kV at 50mbar, the scanned analytes were brought from the micelles to the MSS boundary, I...
Embodiment 2
[0079] Embodiment 2. investigate the influence of PAPS concentration on detection effect
[0080]On the basis of Example 1, PAPS was selected as the micelle, and the PAPS concentration was changed to 0, 5, 10, 20, 30, and 40 mM, and other conditions remained unchanged.
[0081] The concentration of micelles is a key parameter affecting the formation of micelles to the solvent packing boundary (MSSB). Therefore, the analysis of different PAPS concentrations in the sample solution, the results are as follows image 3 shown. When the surfactant concentration was varied from 0 to 20 mM, the peak areas of As(V), MMA and DMA gradually increased, while the peak area of As(III) decreased sharply when the micelle concentration was varied from 5 to 10 mM. While the PAPS concentration was further increased from 20 mM to 40 mM, the peak heights for all four analytes decreased slightly. It was demonstrated that an increase in PAPS concentration negatively affects the formation of mice...
Embodiment 3
[0082] Embodiment 3. investigate the influence of methanol content on detection effect
[0083] On the basis of Example 1, PAPS was selected as the micelle, and the concentration of MeOH was changed to 40, 60, 80, 100% (v / v), and other conditions remained unchanged.
[0084] Methanol is usually an organic solvent in MSS, which affects the interaction between analyte and micelles, reversing the effective electrophoretic mobility for enrichment. This example superimposes two steps of MeOH injection alone, and optimizes the percentage of MeOH in the range of 40-100% (v / v) to obtain the best resolution and enrichment of analytes under other conditions.
[0085] The result is as Figure 4 shown. Except As(III), when the methanol concentration was 40% (v / v), the peak areas of the other three compounds were all smaller than those when 60% was used. However, when the MeOH content was 60%-100% (v / v), the peak intensities of the three compounds [As(V), MMA, DMA] decreased, and the mi...
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