Ionic liquid sol-gel coating stirring rod, preparation method and applications
An ionic liquid and sol-gel technology, which is applied in the field of analytical chemical sample pretreatment, can solve the problems of high detection limit, non-reusable, impervious to immersion extraction and solvent desorption, etc., and achieve resistance to organic solvents and mechanical stability Good, simple preparation, enhanced thermal stability and chemical stability
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Embodiment 1
[0036] (1) Prepare a dumbbell-shaped glass stirring rod
[0037] Cut a thin iron wire with a diameter of 0.50 mm into a small section of 1.7 cm, sand it smooth and straight, and then cut a glass capillary with an inner diameter of 0.9-1.1 mm and a wall thickness of 0.10-0.15 mm (purchased from the Instrument Factory of West China Medical University) into long pieces. A small segment with a height of about 2.5 cm. The treated thin iron wire was placed in a glass capillary, and the two ends of the capillary were sealed with the flame of an alcohol lamp to form a bulge, and finally a dumbbell-shaped glass stirring rod with a length of 2 cm was obtained.
[0038] (2) Activation of the glass stirring rod
[0039] The prepared dumbbell-shaped stirring rod was washed with ultrapure water and methanol in sequence, and then placed in 1 mol / L NaOH for activation for more than 3 h. Wash with pure water until neutral, and dry in an oven for later use.
[0040] (3) Preparation of ionic ...
Embodiment 2
[0049] The extraction and desorption process of the ionic liquid sol-gel coated stirring rod is as follows: put the ionic liquid sol-gel coated stirring rod in 10 mL sample solution, stir and extract at 800 rpm for 30 min, take out the stirring rod after the extraction, Dry the residual solution on the surface of the stirring rod with filter paper, transfer it to a desorption tube filled with 100 μL of methanol, and desorb it ultrasonically for 15 min. The desorbed solution was filtered through a 0.22 μm filter membrane and then used for subsequent high-performance liquid chromatography-ultraviolet (HPLC-UV) detection and analysis; the desorbed stirring rod was placed in methanol for 5 min, and it could be reused after regeneration.
[0050] Since the stirring bar of ionic liquid sol-gel coating is directly immersed and desorbed with organic solvent, the acid and alkali resistance and organic solvent resistance of the prepared ionic liquid extraction coating were investigat...
Embodiment 3
[0053] The ionic liquid sol-gel coated stirring rod prepared in Example 1 was applied to the stirring rod adsorption extraction-high performance liquid chromatography-ultraviolet detection (SBSE-HPLC-UV) to analyze three non-steroidal anti-inflammatory drugs in complex samples (ketoprofen, naproxen and fenbufen), through a series of condition optimization to obtain the best extraction, desorption and separation detection conditions. The optimal extraction and desorption conditions are as follows: the pH of the sample solution is 3, the mass concentration of NaCl is 15%, the extraction temperature is 20 °C, the stirring speed is 800 rpm, and the extraction time is 30 min; the desorbent is 7:3 volume ratio Methanol: 10 mM NaOH solution, ultrasonic desorption for 15 min. The optimal conditions for HPLC-UV separation and detection are: Agilent 1100 high-performance liquid chromatography (Agilent Technologies, Waldbronn, Germany), equipped with an online degasser, a quaternary mixi...
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Abstract
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