Molecularly imprinted solid-phase extraction column for amphetamine drugs and preparation method thereof
A solid-phase extraction column, molecular imprinting technology, applied in separation methods, chemical instruments and methods, analytical materials, etc., can solve the problems of unsatisfactory purification effect, unsatisfactory detection limit, and high analysis cost for low-content sample analysis requirements, Achieve the effect of increasing adsorption equilibrium speed and adsorption capacity, lowering detection limit, and high recovery rate
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Embodiment 1
[0033] Preparation of Molecularly Imprinted Solid Phase Extraction Column for Amphetamine Drugs:
[0034] (1) Add 0.4 parts of methamphetamine hydrochloride to the flask, add 1.2 parts of α-methacrylic acid, 100 parts of nano-sized titanium dioxide and 2200 parts of methanol using a micro injector. Seal it with a rubber stopper, and stir at a constant speed of 220r / min for 3h at room temperature.
[0035] (2) After the stirring is completed, open the rubber stopper, add 400 parts of ethylene glycol dimethacrylate and methanol, and then add 22 parts of azobisisobutyronitrile, and ultrasonically dissolve it. The glass catheter was inflated with nitrogen for 10 min and then quickly sealed with a rubber stopper.
[0036] (3) Prepare a disposable syringe with the middle push handle removed, and the tail is tightly sealed with a balloon and a rubber band. Fill the syringe with nitrogen from the head until the balloon expands to a medium size, and seal it with the needle of the syri...
Embodiment 2
[0039] Example 2 Application of imprinted solid phase extraction column
[0040] (1) Extraction operation and conditions:
[0041] ① Fix the solid-phase extraction column on the solid-phase extraction apparatus, activate the extraction column with 1 ml of methanol and 1 ml of deionized water in advance, and control the flow rate of the solid-phase extraction instrument to 3r n, which is about 1ml / 5min.
[0042] ② In a 5 ml polypropylene centrifuge tube, add 0.4 ml of mixed standard solutions of different concentrations and 1.6 ml of urine (the total solution volume is 2 ml), shake on a vortex shaker for 1 min, then centrifuge at 8500 r / min for 5 min, and put on Pipette 0.5ml of the supernatant each time, divide it into 4 times, add it to the pre-activated molecular imprinted solid phase extraction column one by one, pass through the extraction column at a flow rate of 1ml / 5 min, drain it, and then use methanol / acetic acid ( 90 / 10, V / V) 3ml for elution, the elution rate is cont...
Embodiment 3
[0046] This example uses capillary electrophoresis, uses the solid-phase extraction column of the present invention and other sample processing methods to process samples respectively, and compares the effects of qualitative and quantitative analysis of amphetamine in urine and blood.
[0047] Correlation coefficient: r 2 0.9967, quantitative detection limit 0.92ug / ml, minimum detection limit 0.45 ug / ml;
[0048] The two test samples of A and B are urine and blood respectively. Instructions attached Figure 4 Capillary electrophoresis diagrams of two samples of A and B respectively processed by solid-phase extraction columns; Figure 5 The capillary electrophoresis images of samples A and B that were processed by other sample processing methods. Comparing the two images, it can be seen that the samples processed by the solid phase extraction column have fewer electrophoretic interference peaks, fewer impurities, and better accuracy and precision. Outperforms samples treate...
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