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Bromine residual detection method for dexamethasone epoxide

The technology of a dexamethasone epoxy compound and a detection method is applied in the field of detection of bromine residues of dexamethasone epoxide, can solve problems such as inapplicability, and achieve the effects of high accuracy, small dosage and good repeatability

Inactive Publication Date: 2014-09-03
谭桂莉
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Problems solved by technology

[0004] However, for the detection of bromine residues in the dexabromination reaction and the upper bromination reaction process, the fields described in the above methods are completely different, and the required levels are also different. Residue testing, which looks for a bromine residue detection method that works for this particular process

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  • Bromine residual detection method for dexamethasone epoxide
  • Bromine residual detection method for dexamethasone epoxide
  • Bromine residual detection method for dexamethasone epoxide

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Embodiment 1

[0027] Preparation of related reagents: prepare the following reagents in turn for later use: sodium hypochlorite solution: 1.0mol / L, sodium thiosulfate standard solution: 0.1mol / L and 0.01mol / L, hydrochloric acid solution: 6mol / L, sulfuric acid solution: 3 mol / L L, sodium hydroxide solution is a 20% aqueous solution by weight, sodium dihydrogen phosphate solution is a 30% aqueous solution by weight, sodium formate solution is a 70% aqueous solution by weight, and sodium molybdate solution is a 1% aqueous solution by weight. The potassium chloride solution is a 5% aqueous solution by weight, the potassium iodide solution is a 5% aqueous solution by weight, the starch indicator is a 0.5% aqueous solution by weight, and the methyl red indicator is a 0.1% aqueous solution by weight, ethanolamine-sodium hydroxide The ethanol-methanol solution is prepared by dissolving 15ml of ethanolamine and 3g of sodium hydroxide in 380ml of ethanol-methanol mixture.

[0028] The methyl red indi...

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Abstract

The invention discloses a bromine residual detection method used for the specific technology of bromination reaction and bromine addition reaction of dexamethasone epoxide. The method comprises: obtaining a test solution through a series of treatments of dexamethasone epoxide, adding 2-3 drops of sodium molybdate solution, 1 ml of potassium fluoride solution, 1 ml of potassium iodide solution and 25ml of sulfuric acid solution, and titrating until a starch indicator changes from blue to colorless by using 0.01 mol / L of sodium hyposulfite standard titration solution immediately upon mixing. The method is advantageous in that only small amount of sample is needed, and the analysis and detection effects can be obtained without using high-end analytical equipment, and at the same time, the method has good repeatability and high precision to satisfy the requirements of quality control for product standards.

Description

technical field [0001] The invention relates to the technical field of chemical detection, in particular to a method for detecting bromine residues of dexamethasone. Background technique [0002] The dexamethasone synthesis process uses bromine, a corrosive reagent, and the processes that use bromine in the synthesis process are the dexamethasone bromination reaction and the bromination reaction process. The synthetic route is dexabromination reaction → dexamethasone replacement and oxidation reaction → dexamethasone bromide process → dexamethasone debromination process → dexamethasone fermentation product process → dexamethasone 21 protection product → dexamethasone sulfonate → Dexamethasone elimination process → dexamethasone bromide → dexamethasone epoxy → dexamethasone fluoride (crude dexamethasone). In order to ensure the quality and safety of the product, it is necessary to choose to do bromine residue detection in dexa epoxy, to control the bromine residue in the int...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N31/16
Inventor 谭桂莉林国友赵钟兴黄慨谢美萱
Owner 谭桂莉
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