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Fluorescein sodium refining method

A technology of sodium fluorescein and a refining method, which is applied in the field of preparing pharmaceutical-grade high-purity sodium fluorescein, and can solve the problems of high cost, cumbersome, and many process steps

Active Publication Date: 2010-01-20
GUANGZHOU BAIYUNSHAN MINGXING PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method is feasible, diacetyl fluorescein, as a radiotoxic substance, can decompose radiotoxic substances under heating or fire conditions, which has strong hazards.
At the same time, the process steps are many and cumbersome, and the cost is high

Method used

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  • Fluorescein sodium refining method
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  • Fluorescein sodium refining method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take by weighing 100g of sodium fluorescein, (sodium fluorescein is provided by Tianjin Reagent No. 1 Factory, and the weight content is 95.0% (see attached figure 1 ), analyzed by HPLC (see attached Figure 2-5 , the impurity content is 7.1%,) add 100% ethanol 500ml, heat and reflux to dissolve, add the gac of 5g, filter after continuing to reflux for 15 minutes, get the hydrochloric acid (36.5%) that adds 56ml to the filtrate, stir, and make it cool down Let stand at room temperature for 18 hours, filter, wash the filter cake with 200ml of methanol and then wash with purified water until the chloride ions meet the requirements, put the fluorescein in 200ml of water, add sodium hydroxide solution (concentration 40%) to adjust the pH to 8.7 , the solution was concentrated to a thick thing, and dried at 105°C to obtain 75g of sodium fluorescein, the content of which was determined by high performance liquid chromatography to be 99.8% (see appendix Figure 6 ), the refin...

Embodiment 2

[0033]Weigh 100 g of sodium fluorescein (the same raw material as in Example 1), add 250 ml of 50% ethanol, heat and reflux to dissolve, add 10 g of activated carbon, continue to reflux for 30 minutes and filter, and add 56 ml of hydrochloric acid (36.5% ), stirred, and allowed to cool down to room temperature, placed for 16 hours, filtered, washed with purified water after the filter cake was washed with acetone until the chloride ion met the requirements, the fluorescein was placed in 200ml of water, and sodium hydroxide solution (concentration 40%) to adjust the pH to 8.8, the solution was concentrated to a thick substance, and dried at 105°C to obtain 70g of sodium fluorescein, the content of which was measured by high performance liquid chromatography was 99.7%, and the refined yield was 70%. 0.18%, 10% solution 600nm absorbance 0.379.

Embodiment 3

[0035] Weigh 100 g of fluorescein sodium, add 200 ml of water (same as the raw material of Example 1), stir and dissolve, add 10 g of activated carbon, heat and reflux for 30 minutes and filter, take the filtrate and add dropwise 56 ml of hydrochloric acid (36.5%), stir, and make It was cooled to room temperature, left for 20 hours, filtered, the filter cake was washed with ethanol and then washed with purified water until the chloride ion met the requirements, the fluorescein was placed in 150ml of water, and sodium hydroxide solution (concentration 40%) was added to adjust the pH to 8.75, the solution was concentrated to a thick substance, dried at 105°C to obtain 60g of sodium fluorescein, the content determined by high performance liquid chromatography was 99.6%, the refined yield was 60%, the impurity content was 0.32%, and the 10% solution 600nm absorbance 0.495.

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Abstract

A fluorescein sodium refining method relates to a method for preparing high purity fluorescein sodium by using reagent grade fluorescein sodium as raw material, comprising the following steps: taking reagent grade fluorescein sodium, adding polar solvent, then adding activated carbon, refluxing for 10-60min, filtrating, taking filtrate to add hydrochloric acid while stirring, reducing the temperature to room temperature, standing to ensure that fluorescein sodium is fully precipitated, filtrating, washing the precipitate with polar solvent, then washing with pure water, placing the fluorescein in water, adjusting the pH value to 8.5-9.0 with sodium hydroxide or sodium carbonate, and filtrating to obtain more than 99.5wt% of fluorescent sodium. The method has simple operation and is applicable to industrialized batch production; the whole process is a one-step acidic-basic refining process and the amount of wastewater is less, thus facilitating environmental protection; the method can effectively improve the purity of the product and the clarity of the solution, thus facilitating the quality control of the injection product and reducing the risk of clinical medication.

Description

technical field [0001] The invention relates to a method for refining a heterocyclic organic compound containing only oxygen atoms, in particular to a method for preparing pharmaceutical-grade high-purity fluorescein sodium by using reagent-grade fluorescein sodium as a raw material. Background technique [0002] The chemical name of sodium fluorescein is 9-(o-carboxyphenyl)-6-hydroxy-3H-xanthene-3-one disodium salt, and its English name is fluorescein sodium. It can be used for corneal injury, fundus angiography diagnosis and blood Determination of cycle time. High-purity pharmaceutical-grade sodium fluorescein is used to prepare injections for imaging. Although the fluorescein sodium raw material currently used to prepare injections meets the requirements of the Pharmacopoeia, and the weight content of fluorescein sodium can reach 98.5%, it can be found that there are still many impurities by high performance liquid chromatography analysis. Because of the interference of ...

Claims

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Application Information

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IPC IPC(8): C07D311/82
Inventor 许小春段敏丽司徒少金高建胜王莎周小琴
Owner GUANGZHOU BAIYUNSHAN MINGXING PHARM CO LTD
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