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Selenium detection method

A detection method and morphology technology, applied in the direction of measuring devices, instruments, fluorescence/phosphorescence, etc., can solve the problems such as the lack of standards, and achieve the effects of avoiding interference, strong portability, and accurate measurement results

Active Publication Date: 2014-06-25
恩施硒谷科技股份有限公司
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Problems solved by technology

[0002] At present, the speciation analysis method of selenium is an inevitable trend in the development of selenium detection technology. Based on HPLC-ICP-MS, HPLC-MS-MS, GC-MS and other combined techniques, researchers at home and abroad have analyzed the selenoamino acids and inorganic selenium. A lot of research work has been done on the morphological analysis method, but there is no standard

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Embodiment 1

[0021] Embodiment 1: the detection method of a kind of selenium of the present invention comprises the following steps: a. Analytical instrument system configuration: chromatographic separation system, atomic fluorescence spectrophotometer and selenium form pretreatment device are combined into HPLC-HG-AFS combined system ; The chromatographic column should be able to SeO 3 4+ , SeO 4 6+ C 18 column or anion exchange column; the described selenium form pretreatment device is a selenium form pretreatment device that can be connected to the chromatographic separation system and converts the selenium-containing components in the sample to be tested separated by the chromatographic system into hydrides;

[0022] b. Instrument analysis method: the mobile phase is different concentrations (NH 4 ) 2 HPO 4 Buffer solution or solution with organic reagent added; the elution method adopts 30mM-150mM pH3-9 diammonium hydrogen phosphate buffer solution to prepare a kind of mobile eq...

Embodiment 2

[0027] Embodiment 2: a kind of detection method of selenium of the present invention,

[0028] 1. Instruments and reagents

[0029] Selenium speciation separation system adopts high performance liquid chromatography (US Waters2695 separation unit), hydride generation adopts SAP-10 speciation analysis pretreatment system, detection system and data acquisition and processing system adopts AFS-913d atomic fluorescence spectrophotometer and related software (Beijing Jitian Instrument Co., Ltd.), the sample was digested by Haineng SH230 graphite digestion instrument, and the selenium form was extracted by TMS-200 super constant temperature mixer (Hangzhou Aosheng Instrument Co., Ltd.).

[0030] Hydrochloric acid (GR), nitric acid (GR) are of superior grade, perchloric acid (AR), sodium hydroxide and methanol are of analytical purity.

[0031] Pepsin K (Merck), selenomethionine (SeMet, Sigma), selenocystine (SeCys, Sigma), selenomethylselenocysteine ​​(MeSeCys, Sigma) were prepared...

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Abstract

The invention relates to a method for detecting a selenium form, elemental selenium and total selenium. Chromatographic separation systems and atomic fluorescence spectrophotometers in different instrument manufacturers are combined into a HPLC-HG-AFS system, and a method for analyzing the selenium form and measuring elemental selenium and inorganic selenium and total selenium in a sample can be performed. The measurement result is accurate; by measurement on the total selenium and inorganic selenium, the content of organic selenium can be indirectly obtained by adopting a method of subtracting the inorganic selenium from the total selenium, and a new technology for measuring the total selenium, inorganic selenium and organic selenium through a form analysis method can be formed. The method is high in portability and convenient and flexible to use and has high popularization and application values.

Description

technical field [0001] The invention relates to a method for detecting selenium. Background technique [0002] At present, the speciation analysis method of selenium is an inevitable trend in the development of selenium detection technology. Based on HPLC-ICP-MS, HPLC-MS-MS, GC-MS and other combined techniques, researchers at home and abroad have analyzed the selenoamino acids and inorganic selenium. A lot of research work has been done on the morphological analysis method, but no standard has been formed. In recent years, the HPLC-HG-AFS combined technology developed in my country uses high-performance liquid chromatography separation-on-line hydride generation-atomic fluorescence detection method for speciation analysis, combining the advantages of high-efficiency separation of HPLC and high sensitivity of AFS, The analysis of the element forms that can form hydrides is the main direction of the development of element forms at this stage. Contents of the invention [00...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N21/64
Inventor 陈永波李红英胡百顺孙杨柳朱云芬郭光耀
Owner 恩施硒谷科技股份有限公司
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