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Method for determining selenium forms by utilizing high performance liquid inductively coupled plasma mass spectrometry

A high-performance liquid chromatography and inductive coupling technology, which is used in measurement devices, material separation, instruments, etc., can solve the problems of not reaching the detection limit of the instrument, and achieve the effects of simple mobile phase preparation, good selectivity and strong stability.

Pending Publication Date: 2021-04-13
NANJING IFAST RES INST CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The detection method recommended in the national supply and marketing industry standard "Selenium-enriched Agricultural Products GH / T1135-2017" is LC-AFS, but agricultural products low in selenium, selenium-containing or naturally rich in selenium often fail to reach the instrument detection limit of AFS after sample pretreatment

Method used

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  • Method for determining selenium forms by utilizing high performance liquid inductively coupled plasma mass spectrometry
  • Method for determining selenium forms by utilizing high performance liquid inductively coupled plasma mass spectrometry
  • Method for determining selenium forms by utilizing high performance liquid inductively coupled plasma mass spectrometry

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The salt concentration comparison of embodiment 1 mobile phase

[0047] Table 2 The retention times of five forms under different concentrations of mobile phase salt

[0048] Configure three mobile phases with ammonium citrate contents of 2mmol / L, 6mmol / L, and 10mmol / L respectively (the three mobile phases have no other variables except the concentration of ammonium citrate), and use three mobile phases of 100μg / kg according to the instrument manual (Concentration of each form standard solution) The selenium form mixed standard solution is measured, draws the retention time of each form and analyzes.

[0049]

[0050] As can be seen from the results in Table 2, when the concentration of ammonium citrate was 2mmol / L, the retention time of selenite increased, causing it to overlap with the retention time of selenomethionine and could not be separated; and when the concentration of ammonium citrate was 10mmol / L, selenite The retention time of selenate decreased, result...

Embodiment 2

[0051] The pH value contrast of embodiment 2 mobile phases

[0052] Configure three mobile phases with pH values ​​of 5.5, 5.7, and 5.9 (the three mobile phases have no other variables except the pH value), and use three mobile phases with 100 μg / kg (concentration of each form of standard solution) respectively according to the instrument manual. The selenium form mixed standard solution was determined, and the retention time of each form was obtained and analyzed.

[0053] Table 3 Retention times of five forms of mobile phase at different pH values

[0054]

[0055] From the results in Table 3, it can be concluded that the retention time of selenite and selenate is extremely sensitive to changes in the pH value of the mobile phase, and the greater the pH, the smaller the retention time. When the pH value was 5.5, although the mobile phase could elute the form to be measured in 7 minutes, selenite and methylselenocysteine ​​could not be separated; and when the pH value was...

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Abstract

The invention discloses a method for determining selenium forms by utilizing high performance liquid inductively coupled plasma mass spectrometry. The method is characterized by comprising the steps of (1) preparing a mobile phase; (2) measuring a standard selenium form solution and an extracting solution to be measured by adopting high performance liquid chromatography-inductively coupled plasma mass spectrometry; and (3) carrying out quantitative analysis on five selenium forms of selenocystine, selenomethionine, methylselenocysteine, selenite and selenate in the sample by adopting a normalization method. By adopting the method to detect the selenium form of the plant, the form separation is complete, the mobile phase preparation is convenient, the result obtained by quantitative analysis is accurate and reliable, and five selenium forms of selenocystine (SeCys2), selenomethionine (SeMet), methyl selenocysteine (MeSeCys), selenite (SeO3<2->) and selenate (SeO4<2->) in the plant can be scientifically analyzed.

Description

technical field [0001] The invention relates to a method for measuring the form of selenium by using high-efficiency liquid-phase inductively coupled plasma mass spectrometry, and belongs to the field of analysis and testing. Background technique [0002] The current study found that selenium mainly forms as SeO in environmental media 3 2- , SeO 4 2- 、Se 0 、Se 2- in the form of SeMet, SeCysCysSe, MeSeCys, SeO in crops 3 2- , SeO 4 2- It exists in other forms, and is generally analyzed by LC-AFS, HPLC-ICP-MS and other methods. The detection method recommended in the national supply and marketing industry standard "Selenium-enriched Agricultural Products GH / T1135-2017" is LC-AFS, but agricultural products low in selenium, selenium-containing or naturally rich in selenium often fail to reach the instrument detection limit of AFS after sample pretreatment . Contents of the invention [0003] In view of this, the main purpose of the present invention is to provide a ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 张泽洲陈晓凡王张民刘志奎孙辰璐王莉莉王晓丽宋佳平林锦钰罗琴
Owner NANJING IFAST RES INST CO LTD
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