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Magnetic solid-phase extraction method of detecting ethoxyquine in fruits and vegetables

A plant growth regulator and magnetic technology, applied in chemical instruments and methods, measuring devices, alkali metal compounds, etc., can solve the problems of long extraction time, large amount of adsorbent, low sensitivity, etc., and achieve good extraction effect and stable structure. Good sex, easy to use effect

Active Publication Date: 2019-08-16
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the currently reported magnetic materials with a composite structure of magnetic core and functional shell have shortcomings such as large amount of adsorbent, long extraction time, and low sensitivity. With the increasing demand for detection sensitivity, a suitable compound was synthesized as an MSPE adsorbent. still challenging

Method used

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  • Magnetic solid-phase extraction method of detecting ethoxyquine in fruits and vegetables
  • Magnetic solid-phase extraction method of detecting ethoxyquine in fruits and vegetables
  • Magnetic solid-phase extraction method of detecting ethoxyquine in fruits and vegetables

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Preparation of Fe 3 o 4 @COF(TpDA) adsorbent, the steps are as follows:

[0046] 1. Fe 3 o 4 Preparation of nanoparticles

[0047] 1.35g FeCl 3 ·6H 2 O, 3.85 g NH 4 OAC and 0.40 g of sodium citrate were dispersed in 70 mL of ethylene glycol and mixed by magnetic stirring for 1 h at room temperature to generate a homogeneous solution. The resulting solution was transferred to a 100 mL reaction kettle, and then heated to 200 °C for 16 h. After cooling to room temperature, the product was collected with an external magnet and washed several times with ethanol and water until the supernatant was clear. Finally, the product was vacuum-dried at 60°C to obtain Fe 3 o 4 Nanoparticles.

[0048] 2. Fe 3 o 4 Preparation of @COF(TpDA)

[0049] 63.0mg Tp, 107.2mg DA and 80mg Fe 3 o 4 Nanoparticles were dispersed in 3 mL of dioxane. Transfer the mixture to a pressure-resistant tube, then quickly freeze the pressure-resistant tube in a liquid nitrogen bath, evacuate t...

Embodiment 2

[0056] With the Fe prepared in Example 1 3 o 4 @COF(TpDA) is an adsorbent, and the process conditions for detecting PGRs are screened, and the steps are as follows:

[0057] 1. Standard solution preparation

[0058] Weigh 10mg of IAA, IPA, IBA, 1-NAA, 2-NAA, 1-NOA and 2-NOA respectively, dissolve them in 10mL of acetonitrile respectively, and make PGRs standard solution with a concentration of 1mg / mL, put Store in a refrigerator at 4°C, protected from light, for later use.

[0059] 2. Chromatographic conditions

[0060] Chromatographic analysis was performed on an Agilent 1260 HPLC (Agilent Corporation) equipped with a diode array detector. Separation of PGRs was performed on a Hypersil GOLD C18 column (150 x 4.6 mm, 3 μm). 5% aqueous acetonitrile (A) and pure acetonitrile (B) were selected as mobile phases. Gradient elution was used for elution, and the program was (volume fraction): starting from 30% B, increasing to 34% B within 2 minutes, and maintaining for 11 minut...

Embodiment 3

[0073] The optimization method step that above-mentioned embodiment 2 screens obtains is as follows:

[0074] 1. Preparation of standard solution or sample solution

[0075] Weigh 10mg of IAA, IPA, IBA, 1-NAA, 2-NAA, 1-NOA and 2-NOA respectively, dissolve them in 10mL of acetonitrile respectively, and make PGRs standard solution with a concentration of 1mg / mL, put Store in a refrigerator at 4°C, protected from light, for later use.

[0076] Cut the fruit or vegetable samples into small pieces and crush them, weigh 5g of the samples and 6mL of methanol and transfer them to a 10mL centrifuge tube, sonicate it for 40min, then centrifuge the centrifuge tube at 4000rpm for 10min, and collect the supernatant. The sample was extracted three more times using the same procedure, and the combined extracts were dried with nitrogen to remove most of the methanol (because PGRs have low solubility in water, a small amount of solvent should be kept to ensure complete dissolution of the anal...

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Abstract

The invention discloses a magnetic solid-phase extraction method of detecting ethoxyquine in fruits and vegetables. The method uses a magnetic covalent organic skeleton material Fe3O4@COF(TpDA) as anadsorbent for magnetic solid-phase extraction, so as to extract ethoxyquine in fruits and vegetables. The method detects PGRs in fruits and vegetables by using an MSPE technology, and selects Fe3O4@COF(TpDA) as the adsorbent. The adsorbent is convenient to use, has multiple carbonyl and aromatic rings on the surface, can enrich and extract PGRs through hydrophobic interaction, pi-pi interaction and hydrogen bonds, has good extraction effect and high structure stability, can be reused, and can detect multiple trace PGRs in fruits and vegetables sensitively. In the method, MSPE of Fe3O4@COF(TpDA) and HPLC-DAD are combined for the first time for measuring PGRs, providing a new concept for detection of PGRs.

Description

technical field [0001] The invention relates to a method for detecting plant growth regulators in fruits and vegetables, in particular to a method for detecting plant growth regulators in fruits and vegetables by using a magnetic solid-phase extraction method. Background technique [0002] Plant growth regulators (PGRs) are a class of synthetic compounds that have similar effects to natural plant hormones and natural plant hormones extracted from organisms. They are widely used to accelerate the growth of plants and increase the yield of crops. However, excessive use of PGRs has brought some potential threats to humans, such as premature puberty, reproductive organ damage, carcinogenicity, acute toxicity, and neurotoxicity. Humans are mainly exposed to plant growth regulators through fruits and vegetables. At present, how to effectively detect PGRs at trace concentrations in plants is still a challenge in the field of analytical chemistry. Therefore, it is very necessary to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/08B01J20/22B01J20/30B01J20/28B01D15/08
CPCG01N30/02G01N30/06G01N30/08B01J20/226B01J20/06B01J20/28009B01D15/08G01N2030/062
Inventor 李国梁吴頔吴永宁李宁
Owner QUFU NORMAL UNIV
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