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Application of H-Beta type molecular sieve in NPs detection or adsorption and method for simultaneously detecting eight NPs

A 1.h-beta, molecular sieve technology, applied in the field of analysis and detection, can solve the problem of insufficient accuracy

Active Publication Date: 2022-03-01
SHANGHAI ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, using N-propylethylenediamine powder (PSA) and acidic Al 2 o 3 High-performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) detection of samples treated as sorbents is not sufficiently precise

Method used

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  • Application of H-Beta type molecular sieve in NPs detection or adsorption and method for simultaneously detecting eight NPs
  • Application of H-Beta type molecular sieve in NPs detection or adsorption and method for simultaneously detecting eight NPs
  • Application of H-Beta type molecular sieve in NPs detection or adsorption and method for simultaneously detecting eight NPs

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preparation example Construction

[0035] In the present invention, the preparation method of the H-Beta type molecular sieve preferably comprises the following steps:

[0036] Sodium hydroxide, aluminum source, tetraethylammonium hydroxide, silicon source and water are mixed, the obtained gel is hydrothermally synthesized and then first calcined to obtain a Beta molecular sieve;

[0037] The Beta type molecular sieve is mixed with the ammonium salt aqueous solution, ion exchanged and secondly calcined to obtain the H-Beta type molecular sieve.

[0038] The invention mixes sodium hydroxide, aluminum source, tetraethylammonium hydroxide, silicon source and water, conducts hydrothermal synthesis reaction on the obtained gel, and then first calcines to obtain Beta molecular sieve.

[0039] In the present invention, unless otherwise specified, the reagents used are commercially available products well known to those skilled in the art.

[0040] In the present invention, the aluminum source preferably includes NaAl...

Embodiment 1

[0091] 0.916g NaOH, 1.808g NaAlO 2 and 33.975g tetraethylammonium hydroxide dissolved in 42.725g H 2 In O, add 23.0g of silica gel powder under stirring, transfer to a polytetrafluoroethylene-lined stainless steel autoclave after stirring for 2 hours, hydrothermally react at 145°C for 48 hours, cool to room temperature and filter, and the obtained solid product is deionized After washing with water, dry at 100° C. for 12 hours, and then calcinate at 550° C. for 6 hours to obtain a Beta molecular sieve. Put Beta type molecular sieve in 1mol / LNH 4 In aqueous Cl solution, ion-exchange at 85°C for 2h, and calcinate the obtained ion-exchange product at 550°C for 6h to obtain H-Beta molecular sieve (silicon-aluminum molar ratio is 36), wherein, Beta-type molecular sieve and NH 4 The solid-to-liquid ratio of the aqueous Cl solution is 1 g: 50 mL.

Embodiment 2

[0093] (1) Preparation of mixed standard solutions of serial reference substances

[0094] Dissolve 8 kinds of neonicotinoid pesticide reference substances in acetonitrile respectively to obtain 8 kinds of reference substance stock solutions, the concentration of the reference substance stock solutions is preferably 100mg / L, and the 8 kinds of neonicotinoid pesticide reference substances include Acetamiprid reference substance, clothianidin reference substance, dinotefuran reference substance, flonicamid reference substance, imidacloprid reference substance, chlorothiaprid reference substance, thiacloprid reference substance and thiamethoxam reference substance;

[0095] Accurately pipette 1 mL each of 8 kinds of reference substance stock solutions into the volumetric flask, and accurately dilute to 10 mL with acetonitrile to obtain the reference substance mixed standard solution; the concentrations of the 8 kinds of reference substances in the reference substance mixed standar...

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Abstract

The invention provides application of an H-Beta type molecular sieve in NPs detection or adsorption and a method for simultaneously detecting eight NPs, and relates to the technical field of analysis and detection. According to the method, the H-Beta type molecular sieve is adopted as an adsorbent of the neonicotinoid pesticide (NPs) in the sample pretreatment process, and specific adsorption of the NPs in a sample can be achieved, so that the accuracy, precision and sensitivity of detection of the NPs in water and honey are improved; the repeated utilization rate of the H-Beta type molecular sieve is high, and the requirements of rapidness, accuracy, saving and good repeatability in pretreatment and detection of eight NPs samples in a sample to be detected can be met. The detection is carried out through high performance liquid chromatography-tandem mass spectrometry detection. The method provided by the invention can realize accurate detection of eight trace NPs, the detection limit of NPs in water is less than 0.1 ng / mL, and the detection limit of NPs in honey is less than 2.0 ng / g.

Description

technical field [0001] The invention relates to the technical field of analysis and detection, in particular to the application of H-Beta molecular sieves in NPs detection or adsorption and a method for simultaneously detecting 8 kinds of NPs. Background technique [0002] Neonicotinoid pesticides (neonicotinoid pesticides, NPs) are the fourth largest class of insecticides after organophosphates, carbamates, and pyrethroids. The insecticidal mechanism is to act on the synapses of the insect nervous system Nicotinic acetylcholine receptors (nAChRs) in the posterior membrane, and the nerves surrounding them, keep the insect excited, paralyzed and then dead. This type of insecticide has chemical and biological characteristics such as wide insecticidal spectrum, low dosage, good systemic conductivity, novel mechanism of action, and high environmental compatibility, and has no cross-resistance with other traditional insecticides. Widest range of insecticides. [0003] With the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 司文帅王守英白冰吴楠黄志英
Owner SHANGHAI ACAD OF AGRI SCI
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