Solid phase extraction method of attapulgite solid phase extraction column and its application in basic compounds
A technology of solid phase extraction column and solid phase extraction column, which is applied in the field of sample pretreatment to achieve the effect of low cost, good reproducibility, simple and practical loading and washing conditions
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Embodiment 1
[0024] Example 1: Attapulgite-based solid phase extraction cartridges were prepared according to the following steps.
[0025] (1) Acidification treatment of attapulgite
[0026] Grind and sieve the original soil of attapulgite to below 200 mesh, then add hydrochloric acid at a concentration of 4 mol / L, the ratio of attapulgite to hydrochloric acid is 1:10 g / mL, shake at 75 °C for 4 h, and then Wash with distilled water until neutral, dry in an oven at 110 °C for 8 h, and get acidified attapulgite after grinding.
[0027] (2) Preparation of solid-phase extraction cartridges
[0028] Weigh 0.03 g of the acidified attapulgite treated in step (1), put it into a 3 mL solid-phase extraction column with a sieve plate with a pore size of 5 μm, fill it into a 20 μm micropore upper sieve plate, and shake it evenly with a vibrating bed. Compact with a compactor.
Embodiment 2
[0029] Example 2: Using melamine as a sample, the concentration of acetonitrile was optimized when loading the sample.
[0030] The attapulgite solid-phase extraction column prepared in Example 1 was rinsed with 5 mL of methanol and 5 mL of deionized water respectively, and then replaced with a certain proportion of acetonitrile aqueous solution (consistent with the solvent ratio for dissolving melamine), Dissolve melamine in 95%, 75%, 45%, 20% and 0% aqueous acetonitrile (v / v) at a concentration of 1.0 μg / mL, load 1 mL of sample, and pass through the solid phase at a flow rate of 1 mL / min Extract the small column, collect the effluent sample, and analyze it by liquid chromatography after passing through a 0.45 μm filter membrane. Chromatographic analysis conditions: the analytical column is Shimadzu Inertsil-NH 2 (4.6×150 mm, 5 μm), the mobile phase was 80% acetonitrile, the flow rate was 1.0 mL / min, the injection volume was 5 μL, the column temperature was 30 °C, and the de...
Embodiment 3
[0031] Embodiment 3: Taking melamine as a sample, the concentration of eluted acetonitrile was optimized.
[0032] Use the attapulgite solid-phase extraction column prepared in Example 1, rinse with 5 mL methanol and 5 mL deionized water respectively, and dissolve melamine in 45% acetonitrile aqueous solution (v / v) at a concentration of 1.0 μg / mL, load 1 mL, pass through the solid phase extraction cartridge at a flow rate of 1 mL / min, rinse with 5 mL 45% acetonitrile, drain, discard the waste liquid, and then use 1 mL containing 0% and 10% , 30%, 40%, 60%, 80% and 95% acetonitrile in 10 mM ammonium acetate solution (pH=11.37) for elution and draining, collected the eluate, added solid citric acid to adjust the pH to 7~8, and passed 0.45 μm filter membrane for HPLC detection. Chromatographic analysis conditions: the analytical column is Shimadzu Inertsil-NH 2(4.6×150 mm, 5 μm), the mobile phase was 80% acetonitrile, the flow rate was 1.0 mL / min, the injection volume was 5 μL...
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