Method for detecting chloroacetone compounds in folic acid

A detection method, the technology of chloroacetone, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problem of low accuracy of detection results, and achieve the effects of accurately determining chloroacetone compounds, improving solubility, and increasing concentration

Active Publication Date: 2021-06-11
杭州仟源保灵药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The main purpose of the present invention is to provide a detection method of chloroacetone compounds in folic acid, to solve the problem that there is no method for detecting all chloroacetone compounds (9 kinds) in folic acid in the art. The detection method has the problem of low accuracy of detection results

Method used

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  • Method for detecting chloroacetone compounds in folic acid
  • Method for detecting chloroacetone compounds in folic acid
  • Method for detecting chloroacetone compounds in folic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Solution preparation.

[0041] Same method as in method verification step.

[0042] (2) Chromatographic detection.

[0043] Using a Thermo TRACE 1300 chromatograph, test the blank solution, the test solution and the reference solution in sequence, and the test working conditions are as follows:

[0044] Chromatographic column: Agilent DB-624, with a length of 30m, a diameter of 0.32mm, a film thickness of 1.8μm, and an operating temperature range of -20°C to 260°C.

[0045] Injection volume: 1 μL, inlet temperature: 200°C, split ratio 5:1, column temperature 70°C, temperature was raised to 180°C at 20°C / min, and then to 240°C at 10°C / min.

[0046] Carrier gas: high-purity nitrogen; hydrogen flow: 35mL / min; air flow: 350mL / min; make-up gas: 40mL / min

[0047] Detector: FID; Detector temperature: 250°C.

[0048] see test results figure 1 , monochloroacetone peaks at position 3 with a retention time of 4.003 min; 1,1-dichloroacetone peaks at position 5 with a reten...

Embodiment 2

[0050] (1) Solution preparation.

[0051] Same method as in method verification step.

[0052] (2) Chromatographic detection.

[0053] Using a Thermo TRACE 1300 chromatograph, test the blank solution, the test solution and the reference solution in sequence, and the test working conditions are as follows:

[0054] Chromatographic column: Agilent DB-624, with a length of 30m, a diameter of 0.32mm, a film thickness of 1.8μm, and an operating temperature range of -20°C to 260°C.

[0055] Injection volume: 1 μL, inlet temperature: 200°C, split ratio 5:1, column temperature 70°C, temperature was raised to 180°C at 20°C / min, and then to 240°C at 10°C / min.

[0056] Carrier gas: high-purity nitrogen; hydrogen flow: 35mL / min; air flow: 350mL / min; make-up gas: 40mL / min

[0057] Detector: ECD; Detector temperature: 250°C.

[0058] see test results figure 2 , when the test sample is 100μg / ml, monochloroacetone peaks at position 1 with a retention time of 3.179min; 1,1-dichloroaceton...

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Abstract

The invention provides a method for detecting chloroacetone compounds in folic acid. The method for detecting the chloroacetone compounds in the folic acid comprises the following steps: mixing the folic acid with 15-25wt% sulfuric acid to obtain a mixed solution; extracting the chloroacetone compound in the mixed solution by adopting an extracting agent to obtain an extracting solution; preparing at least one sample to be detected by adopting the extract liquor; detecting a sample to be detected by adopting a gas chromatography device, wherein a flame ionization detector or an electron capture detector is adopted as a detector. By adopting the method, folic acid matrix interference can be greatly reduced or even eliminated, meanwhile, extraction separation and concentration of nine kinds of chloroacetone can be achieved, meanwhile, the problem that folic acid cannot be analyzed due to the fact that folic acid is not dissolved in a solvent and the problem that chloroacetone is easy to decompose in the analysis process can be solved, and then the accuracy of a detection result can be greatly improved.

Description

technical field [0001] The invention relates to the field of folic acid synthesis, in particular to a method for detecting chloroacetone compounds in folic acid. Background technique [0002] Folic acid is a water-soluble vitamin with the molecular formula C 19 h 19 N 7 o 6 , is an essential substance for the growth and reproduction of body cells, and is mainly used for the prevention and treatment of folic acid deficiency caused by megaloblastic anemia and chronic hemolytic anemia. Traditional synthetic method of folic acid: use N-(4-aminobenzoyl)-L-glutamic acid, trichloroacetone and 2,4,5-triamino-6-hydroxypyrimidine sulfate as raw materials, and use water as solvent , the crude product of folic acid was prepared by a one-pot method, and the pure product of folic acid was obtained through acid refining and alkali refining. The purity level of trichloroacetone is directly related to the purity and the yield of folic acid, and the price of trichloroacetone with higher ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/54G01N30/68G01N30/70
CPCG01N30/02G01N30/06G01N30/54G01N30/68G01N30/70G01N2030/025G01N2030/062
Inventor 沈杞容周淑丰丁常英刘玲宋存珍刘东华朱金梁
Owner 杭州仟源保灵药业有限公司
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