Derivatization gas chromatography for rapidly measuring dialkoxy propyl-diamidine salt

A dialkoxy propane diamidine salt and gas chromatography technology is applied in the field of derivative gas chromatography for rapid determination of dialkoxy propane diamidine salts, and can solve the problem of lack of detection ability, strong pertinence and lack of versatility and other problems to achieve the effect of overcoming poor universality and enriching analytical methods

Active Publication Date: 2013-07-03
INSIGHT FINECHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Some fluorescent amidines can be converted into strong fluorescent derivatives through thorough hydrolysis, etc., so they can be detected by fluorescence analysis. Too strong and lack of versatility (Journal of Hebei University(natural science edition)., 26(2), 175-177, 2006)
[0006] The above description shows that the existing analytical methods for amidine compounds have their own limitations. For compounds such as dialkoxymalonimidine salts, none of the above methods has the ability to detect them. Therefore, it is necessary to develop a method suitable for The new rapid detection method of this kind of compound has practical research and development value and application significance

Method used

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  • Derivatization gas chromatography for rapidly measuring dialkoxy propyl-diamidine salt
  • Derivatization gas chromatography for rapidly measuring dialkoxy propyl-diamidine salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Derivatization pretreatment of samples

[0025] Weigh ~0.2g of the sample to be tested into a 10ml sample tube, add 2.0g of derivatization reagent-1 [mixture of dilute phosphoric acid (5% by weight) and methanol (25% V / V)], shake to dissolve, and ultrasonically hydrolyze for 20 Minutes, dry with ~2g of anhydrous sodium sulfate, let stand for 5 minutes, centrifuge to get the supernatant.

[0026] (2) Setting of instruments and testing conditions

[0027] Instrument: Shimadzu GC-2010 Plus;

[0028] Chromatographic conditions: chromatographic column: PEG-20000 (30m×0.32mm×0.25μm) capillary column; inlet temperature: 200°C; FID detector temperature: 250°C; carrier gas: high-purity nitrogen, flow rate 2.0ml / min; Hydrogen: 35ml / min; Air: 450ml / min; Injection method: Split injection, split ratio: 1:30; Makeup gas flow: 20ml / min; Injection volume: 2.0μl; (No hold), raise the temperature to 280°C at 20°C / min, and hold for 10 minutes.

[0029] (3) Actual testing of sample...

Embodiment 2

[0036] (1) Derivatization pretreatment of samples

[0037] Weigh ~0.2g of the sample to be tested in a 10ml sample tube, add 2.0g of derivatization reagent-1 [mixture of dilute sulfuric acid (5% by weight) and methanol (25% V / V)], shake to dissolve, and ultrasonically hydrolyze for 20 Minutes, dry with ~2g of anhydrous sodium sulfate, let stand for 5 minutes, centrifuge to get the supernatant.

[0038] (2) Setting of instruments and testing conditions

[0039] Instrument: Shimadzu GC-2010 Plus;

[0040] Chromatographic conditions: chromatographic column: OV-17 (30m×0.32mm×0.50μm) capillary column; inlet temperature: 250°C; FID detector temperature: 250°C; carrier gas: high-purity nitrogen, flow rate 2.0ml / min; Hydrogen: 35ml / min; Air: 450ml / min; Injection method: Split injection, split ratio: 1:30; Makeup gas flow: 20ml / min; Injection volume: 2.0μl; (No hold), the temperature was raised to 250°C at 15°C / min, and held for 10 minutes.

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Abstract

The invention relates to a derivatization gas chromatography for rapidly measuring the key intermediate, namely, dialkoxy propyl-diamidine salt, of 2-amido-4,6-dimethoxypyrimidine (ADMP). In the method, a special derivatization reagent is adopted, hydrolytic treatment is performed on the dialkoxy propyl-diamidine salt in specific conditions, and then gas chromatography and quantitative treatment are performed on the derivatization product, thus obtaining the analysis result of the content of the to-be-measured product. The method disclosed by the invention has the advantages of being rapid, simple, accurate and sensitive; the defect that the dialkoxy propyl-diamidine salt cannot be analysed by the conventional detection means is greatly overcome; and moreover, the method has universality to a certain extent, and can be further popularized and applied to analysis and detection for other amidine salt compounds.

Description

technical field [0001] The invention relates to an analysis method for amidine salts, in particular to a derivation gas chromatography method for rapid determination of dialkoxymalonimidine salts. Background technique [0002] Amidines and their derivatives are a class of organic compounds with wide application prospects and good biological activities, and they are also important intermediates for the synthesis of nitrogen-containing heterocycles. Currently known detection methods for such compounds mainly include conventional gas chromatography, liquid chromatography and fluorescence spectrophotometry. [0003] The disadvantage of gas chromatography is that it cannot detect amidines that are difficult to gasify or have poor thermal stability (Food Science and Technology., 31(2), 94-95, 2006). [0004] The limitation of liquid chromatography is that the structure of the analyte must contain a chromophore and have certain stability in the corresponding mobile phase. Some hig...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 李永芳王坤凌云韦倩殷巍
Owner INSIGHT FINECHEM
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