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Method for detecting amantadine compounds and triazine herbicides in algae

A technology for the detection of amantadine and its detection method, which is applied in the field of detection of amantadine compounds and triazine herbicides in algae, and can solve the problems of simultaneous detection of two types of drugs, cumbersome operation, and high cost

Pending Publication Date: 2021-11-19
山东省海洋资源与环境研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Since amantadine drugs belong to antiviral drugs, and triazine herbicides belong to pesticide residues, and since the two drugs belong to different types of drugs, the existing detection method is for amantadine and triazine herbicides. To carry out testing separately, the operation is relatively cumbersome, and the experimenters need to carry out multiple treatments before testing on the machine separately, and the cost is high
Moreover, most of the current detection methods are aimed at amantadines in animal origin and triazine herbicides in the environment. At present, there is no method for simultaneous detection of two types of drugs in algae

Method used

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  • Method for detecting amantadine compounds and triazine herbicides in algae
  • Method for detecting amantadine compounds and triazine herbicides in algae
  • Method for detecting amantadine compounds and triazine herbicides in algae

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0126] Sample pretreatment

[0127] Weigh 3.0g (±0.01g) of the algae sample to be tested, homogenize it with a homogenizer, wash the knife head with 15mL acetonitrile, add it to the sample, vortex at 2000r / min for 30s, extract it ultrasonically for 30min, and centrifuge at 8000r / min for 10min Take 5mL supernatant in a 15mL centrifuge tube, dry it with nitrogen at 40°C, add 1mL of acetonitrile aqueous solution containing 0.1vol% formic acid (the volume ratio of acetonitrile and water in the acetonitrile aqueous solution is 6:4) 1mL, 50mg PSA adsorption (particle size: 50-75μm), vortex at 2000r / min for 1min, centrifuge at 5000r / min for 10min, take the supernatant and pass through a 0.22μm PVDF membrane to obtain the solution to be tested.

[0128] Parameters for UHPLC include:

[0129] Liquid phase model: Dionex UltiMate 3000 ultra-high performance liquid phase system

[0130] Column: Waters BEH C 18 (2.1mm×100mm 1.7μm);

[0131] Column temperature: 45°C;

[0132] Mobile phas...

Embodiment 2

[0165] Choice of extractant

[0166] The extractant acetonitrile in Example 1 was replaced with 1 vol% formic acid acetonitrile, methanol, 1 vol% formic acid methanol, ethyl acetate, 1 vol% formic acid ethyl acetate to obtain an extract.

[0167] Utilize formula 1 to calculate the extraction rate in the extract solution:

[0168]

[0169] In Formula 1:

[0170] Instrument detection value: adding standard solution to blank matrix, after pretreatment, the test result on the machine, μg / L;

[0171] Blank sample matrix addition value: the value of the standard solution added to the blank matrix sample, μg / L.

[0172] The corresponding extraction rate of each extractant obtained is as follows: figure 1 shown. From figure 1 It can be seen that the extraction efficiency of acetonitrile is close to the effect of 1vol% formic acid acetonitrile, ethyl acetate and 1vol% formic acid ethyl acetate, indicating that acetonitrile, 1vol% formic acid acetonitrile, ethyl acetate and 1vol...

Embodiment 3

[0174] Sorbent selection

[0175] The PSA adsorbent in embodiment 1 is replaced by C 18 Adsorbent, calculate recovery using Equation 2:

[0176]

[0177] In formula 2:

[0178] On-machine test results: After the blank matrix sample is pre-treated, the standard solution is used to constant volume, and the test results on the machine after the adsorbent is purified, μg / L;

[0179] The value of matrix calibration: After the blank matrix sample is pre-treated, use a certain concentration of standard solution to make up the volume, μg / L.

[0180] Effect of different adsorbents on the recovery rate of adamantane compounds and triazine herbicides figure 2 shown. From figure 2 It can be seen that: C 18 Sorbent has certain adsorption to part herbicide class medicine, causes recovery rate to reduce, therefore, the present invention mainly adopts PSA sorbent as purification means, C 18 As an auxiliary means, sorbent purification is only used when dealing with biological sampl...

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Abstract

The invention belongs to the technical field of material analysis, and provides a method for detecting amantadine compounds and triazine herbicides in algae. According to the method, acetonitrile, ethyl acetate, a formic acid-acetonitrile mixed solution with the formic acid volume concentration of 1% or a formic acid-ethyl acetate mixed solution with the formic acid volume concentration of 1% are adopted as an extracting agent, so that amantadine compounds and triazine herbicides in an algae sample can be released; a PSA adsorbent is used as an adsorbent; impurities which have great interference on amantadine compounds and triazine herbicides in an extracting solution can be adsorbed and removed to the greatest extent, qualitative detection is performed by adopting ultrahigh performance liquid chromatography, primary mass spectrometry and secondary mass spectrometry, the qualitative accuracy can be improved, false positive can be eliminated, and the detection accuracy can be improved; the amantadine compounds and the triazine herbicides can be accurately quantified by performing quantitative analysis on the amantadine compounds and the triazine herbicides by using ultrahigh liquid chromatography and primary chromatography, and the method has relatively high detection sensitivity.

Description

technical field [0001] The invention relates to the technical field of substance analysis, in particular to a method for detecting amantadine compounds and triazine herbicides in algae. Background technique [0002] Since amantadine drugs belong to antiviral drugs, and triazine herbicides belong to pesticide residues, and since the two drugs belong to different types of drugs, the existing detection method is for amantadine and triazine herbicides. It is cumbersome to carry out testing separately, and the experimenters need to carry out multiple treatments before testing on the machine separately, and the cost is high. Moreover, most of the current detection methods are aimed at amantadines in animal origin and triazine herbicides in the environment. At present, there is no method for simultaneous detection of two types of drugs in algae. Contents of the invention [0003] In view of this, the object of the present invention is to provide a method for detecting amantadine...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/72
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/72G01N2030/324
Inventor 徐英江李焕军张秀珍任传博陈玮田秀慧宫向红薛敬林张华威罗晶晶李佳蔚王景丁玉竹
Owner 山东省海洋资源与环境研究院
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