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A tryptophan ionic liquid-loaded magnetic graphene oxide nanocomposite material and its tebuconazole extraction detection method

A nanocomposite material and ionic liquid technology, which is applied in the separation and analysis of tebuconazole by amino acid ionic liquid loaded magnetic graphene oxide nanocomposite, which can solve the problems of poor selectivity, weak adsorption capacity, easy oxidation and agglomeration

Active Publication Date: 2021-08-06
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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  • A tryptophan ionic liquid-loaded magnetic graphene oxide nanocomposite material and its tebuconazole extraction detection method
  • A tryptophan ionic liquid-loaded magnetic graphene oxide nanocomposite material and its tebuconazole extraction detection method
  • A tryptophan ionic liquid-loaded magnetic graphene oxide nanocomposite material and its tebuconazole extraction detection method

Examples

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] Concrete preparation steps are:

[0033] 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 h to prepare 1-butyl-3-methylimidazole bromide , and then 1-butyl-3-methylimidazole bromide is passed through a basic anion exchange resin column, and dropped into the tryptophan aqueous solution stirred in an ice bath at a rate of one drop per 3s; stirring while dripping; the alkali in it The strong anion 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, and then vacuum-dried at...

Embodiment 2

[0036] 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.

[0037] Concrete preparation steps are:

[0038] 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 h to prepare 1-butyl-3-methylimidazole bromide , and then 1-butyl-3-methylimidazole bromide is passed through a basic anion exchange resin column, and dropped into the tryptophan aqueous solution stirred in an ice bath at a rate of one drop per 5s; stirring while dripping; the alkali in it The strong anion exchange resin column was pre-washed with 10% sodium hydroxide; finally, the product obtained by exchanging the basic anion exchange resin column was evaporated to dryness at 50°C, and then dried in vacuum at 80°C for 12 hours to obt...

Embodiment 3

[0044] The extraction method is implemented as follows:

[0045] (1) Extraction samples: Take four 10.0 mL centrifuge tubes and add 200.0 μg mL -1 Tebuconazole standard solution 0.1 mL, then add 2.0 mL pH=7.0 buffer solution, dilute to 10.0 mL 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 min, separated by magnetic adsorption, discarded the supernatant, eluted with 2.0 mL of methanol, adsorbed by a magnet, and the supernatant was determined by HPLC.

[0046] Control sample: Take the same four 10.0 mL centrifuge tubes and add 200.0 μg mL -1 Tebuconazole standard solution 0.1 mL, then add 2.0 pH=7.0 buffer solution, and dilute to 10.0 mL with distilled water. None of the four solutions added magnetic solid-phase extractant.

[0047] Implementation of t...

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Abstract

The invention relates to a tryptophan ionic liquid-loaded magnetic graphene oxide nanocomposite material and its tebuconazole extraction detection method in the field of inorganic chemistry. The tryptophan ionic liquid is loaded on Fe 3 o 4 @SiO 2 On the surface of @GO nanoparticles, the material is then applied to the tebuconazole sample solution, and combined with high performance liquid chromatography-UV detector, the separation and analysis of the fungicide-tebuconazole in environmental samples can be realized. The results showed that: Fe 3 o 4 @SiO 2 @GO@[C 4 mim]Try nanoparticles can quickly and quantitatively adsorb tebuconazole, and the extraction rate of tebuconazole in the test sample can reach more than 95.0%, and the detection limit of this method is 0.014 μg mL ‑1 , the linear range is 0.016‑40.00μg mL ‑1 , enrichment factor 20.0. The method was successfully performed 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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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/02
CPCG01N30/02G01N30/06G01N2030/062
Inventor 陈思伊朱霞石
Owner YANGZHOU UNIV
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