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Tryptophan ionic liquid loaded magnetic graphene oxide nano composite material and tebuconazole extraction detection method thereof

A nanocomposite material and ionic liquid technology, applied in the separation and analysis of tebuconazole by amino acid ionic liquid-loaded magnetic graphene oxide nanocomposite, can solve the problems of poor selectivity, easy oxidation and agglomeration, weak adsorption capacity, etc., and achieve satisfactory results , Excellent adsorption capacity, and the effect of improving extraction performance

Active Publication Date: 2019-08-30
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, Fe 3 o 4 prone to oxidation and agglomeration
In addition, bare Fe 3 o 4 Weak adsorption capacity and poor selectivity

Method used

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  • Tryptophan ionic liquid loaded magnetic graphene oxide nano composite material and tebuconazole extraction detection method thereof
  • Tryptophan ionic liquid loaded magnetic graphene oxide nano composite material and tebuconazole extraction detection method thereof
  • Tryptophan ionic liquid loaded magnetic graphene oxide nano composite material and tebuconazole extraction detection method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] First, tryptophan ionic liquid was loaded on Fe by ultrasonic vibration 3 o 4 @SiO 2 Magnetic graphene oxide nanocomposite material Fe prepared on the surface of @GO magnetic nanoparticles by tryptophan ionic liquid 3 o 4 @SiO 2 @GO@[C 4 mim] Try.

[0032] conduct

[0033] Concrete preparation steps are:

[0034] Step 1: Mix 1-methylimidazole and 1-bromo-n-butane in a three-necked flask at a mass ratio of 1:1, and stir in a water bath at 70°C for 3 hours to prepare 1-butyl-3-methylimidazole bromide. Then pass 1-butyl-3-methylimidazole bromide through a basic anion exchange resin column, and drop it into the aqueous solution of tryptophan amino acid stirred in an ice bath at a rate of one drop every 3 seconds; stir while dripping; the basic anion in it The exchange resin column was pre-washed with sodium hydroxide with a mass concentration of 8%; finally, the product obtained by exchanging the basic anion exchange resin column was evaporated to dryness at 30°C, a...

Embodiment 2

[0037] First, tryptophan ionic liquid was loaded on Fe by ultrasonic vibration 3 o 4 @SiO 2 Magnetic graphene oxide nanocomposite material Fe prepared on the surface of @GO magnetic nanoparticles by tryptophan ionic liquid 3 o 4 @SiO 2 @GO@[C 4 mim] Try.

[0038] Concrete preparation steps are:

[0039] Step 1: Mix 1-methylimidazole and 1-bromo-n-butane in a three-necked flask at a mass ratio of 1:1, and stir in a water bath at 70°C for 3 hours to prepare 1-butyl-3-methylimidazole bromide. Then 1-butyl-3-methylimidazole bromide is passed through the basic anion exchange resin column, and dropped into the aqueous solution of tryptophan amino acid stirred in an ice bath at a rate of one drop every 5 seconds; stirring while dripping; the basic anion in it The exchange resin column was pre-washed with sodium hydroxide with a mass concentration of 10%; finally, the product obtained by exchanging the basic anion exchange resin column was evaporated to dryness at 50°C, and the...

Embodiment 3

[0045] The extraction method is implemented as follows:

[0046] (1) Extraction samples: Take four 10.0mL centrifuge tubes and add 200.0μg mL -1 Tebuconazole standard solution 0.1mL, then add 2.0mL pH=7.0 buffer solution, dilute to 10.0mL with distilled water. Accurately weigh (a) Fe 3 o 4 @SiO 2 @GO(b)Fe 3 o 4 @SiO 2 @GO@[C 4 mim]Br(c)Fe 3 o 4 @SiO 2 @GO@[C 4 mim]Gly(d)Fe 3 o 4 @SiO 2 @GO@[C 412.0 mg of mim]Try nanoparticles were placed in a centrifuge tube, shaken at room temperature for 15 minutes, separated by magnetic adsorption, discarded the supernatant, eluted with 2.0 mL of methanol, adsorbed by a magnet, and the supernatant was measured by HPLC.

[0047] Control sample: Take the same four 10.0mL centrifuge tubes and add 200.0μg mL -1 Tebuconazole standard solution 0.1mL, then add 2.0pH=7.0 buffer solution, dilute to 10.0mL with distilled water. None of the four solutions added magnetic solid-phase extractant.

[0048] Implementation of the method in...

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Abstract

The invention relates to a tryptophan ionic liquid loaded magnetic graphene oxide nano composite material and a tebuconazole extraction detection method thereof in the field of inorganic chemistry. Tryptophan ionic liquid is loaded on the surface of Fe3O4@SiO2@GO nano particles, and then the material is applied to tebuconazole sample solution, and separation and analysis of bactericide-tebuconazole in an environmental sample can be realized by combination with a high performance liquid chromatography-ultraviolet detector. Results show that: the tebuconazole can be rapidly and qualitatively adsorbed by Fe3O4@SiO2@GO@[C4mim]Try nano particles, the extraction rate of the tebuconazole in a detected sample reaches over 95.0%, the detection limit of the tebuconazole extraction detection method is 0.014[mu]g / mL, the linear range is 0.016-40.00[mu]g / mL, and a concentration factor is 20.0. The tebuconazole extraction detection method successfully performs measurement on water, rice, corn and soil samples.

Description

technical field [0001] The invention relates to the fields of inorganic chemistry, chromatographic multi-component analysis, drug detection and analysis, etc., and specifically relates to a method for separating and analyzing tebuconazole by amino acid ionic liquid-loaded magnetic graphene oxide nanocomposite materials. Background technique [0002] Tebuconazole, (R,S)-1-p-chlorophenyl-4,4-dimethyl-3-(1H-1,2,4-triazol-1-ylmethyl)pentan-3-ol , is a broad-spectrum chiral triazole fungicide used for the control of soil-borne and leaf diseases such as powdery mildew in leaf spot, rust and root rot in crops as steroid demethylated (sterol bio synthetic inhibitors) [1]. Tebuconazole is one of the most widely sold fungicides in the world and is widely used on agricultural crops [2]. Due to its widespread use and long-term accumulation, this fungicide will remain in crops, soil, and the surrounding water environment, inevitably causing potential risks to human health and ecosystem...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/02
CPCG01N30/02G01N30/06G01N2030/062
Inventor 陈思伊朱霞石
Owner YANGZHOU UNIV
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