Method for detecting 6-chloropicolinic acid in vegetables and fruits

A technology for the detection of clopicolinic acid and its detection method, which is applied in the field of detection of 6-chloropicolinic acid in fruits and vegetables, and can solve the problems of complex detection methods, inaccurate detection results, time-consuming and labor-consuming problems of 6-chloropicolinic acid, and achieve good separation , effective detection method, and the effect of improving the recovery rate

Pending Publication Date: 2021-09-24
TECH CENT OF GUANGZHOU CUSTOMS +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Through the above analysis, the existing problems and defects of the prior art are: the existing detection method of 6-chloropicolinic acid is complex, cumbersome, time-consuming and labor-intensive, and the recovery rate is low, and the detection result is inaccurate

Method used

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  • Method for detecting 6-chloropicolinic acid in vegetables and fruits
  • Method for detecting 6-chloropicolinic acid in vegetables and fruits
  • Method for detecting 6-chloropicolinic acid in vegetables and fruits

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preparation example Construction

[0045] In step S101, the method for preparing a vegetable and fruit sample provided by the embodiment of the present invention includes: selecting a vegetable or fruit sample, chopping the selected sample, fully mixing it, sampling by quartering or directly putting it into a tissue masher for mashing into a homogenate and put into a polyethylene bottle.

[0046] In step S101, the selected vegetable or fruit samples provided by the embodiment of the present invention include:

[0047]For samples with smaller individuals, all samples shall be processed after sampling;

[0048] For a substantially uniform sample with a large individual, it is processed after being divided or cut into small pieces on the axis of symmetry or on the plane of symmetry;

[0049] For samples that are slender, flat or have different component contents in different parts, cut small pieces or cut into small pieces at different parts for post-processing.

[0050] In step S104, the use of liquid chromatog...

Embodiment 1

[0059] 1 Scope

[0060] The invention is applicable to a liquid chromatography-mass spectrometry method for determining the residual amount of 6-chloropicolinic acid in vegetables and fruits.

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Abstract

The invention belongs to the technical field of food detection, and discloses a method for detecting 6-chloropicolinic acid in vegetables and fruits, which comprises the following steps: preparing a vegetable and fruit sample, extracting with an acetonitrile-formic acid solution, and centrifuging; purifying supernate obtained through centrifugation; detecting the purified supernate by using a liquid chromatograph-mass spectrometer (LC-MS); and comparing the retention time of the detected target pesticide chromatographic peak with the retention time of the corresponding standard chromatographic peak, and carrying out qualitative and quantitative analysis. The invention provides a method for detecting and analyzing 6-chloropicolinic acid in vegetables and fruits by using LC-MS/MS. The method is suitable for liquid chromatography-mass spectrometry determination of residual quantity of 6-chloropicolinic acid in vegetables and fruits. According to the method, a T3 chromatographic column is adopted for separation, detection is carried out in a positive ion mode, a selected mobile phase is acetonitrile + 10 mmol/L ammonium acetate solution, isocratic elution is adopted for the mobile phase, the column residual effect can be eliminated, and good reproducibility is obtained.

Description

technical field [0001] The invention belongs to the technical field of food detection, in particular to a method for detecting 6-chloropicolinic acid in fruits and vegetables. Background technique [0002] At present, trichloromethylpyridine can be used as a nitrogen oxide inhibitor and a soil nitrogen fertilizer synergist due to its selective activity against nitrogen-fixing bacteria, commonly known as azopyridine. When applied together with urea and nitrogen fertilizer, it can delay the oxidation of ammonium ions in the soil, and it is also an important pesticide and pharmaceutical intermediate. It is rapidly degraded to 6-chloropicolinate in plants, animals and soil, and is the only significant chemical residue resulting from the application of azapyridine. [0003] The detection method of trichloromethylpyridine metabolite 6-chloropicolinic acid in plant-derived foods in my country is relatively complex, tedious, time-consuming and labor-intensive. The detection of 6-c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/72G01N2030/047G01N2030/146
Inventor 孙灵慧陈捷徐娟王岚廖满生廖延海
Owner TECH CENT OF GUANGZHOU CUSTOMS
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