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High performance liquid chromatography method for efficiently separating and detecting related substances in hydroquinone and application thereof

A high-performance liquid chromatography and related substance technology, applied in the field of drug analysis, to achieve the effects of high sensitivity, good specificity, high-efficiency separation and detection

Active Publication Date: 2021-03-05
广东人人康药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the dosage of hydroquinone must be strictly controlled

Method used

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  • High performance liquid chromatography method for efficiently separating and detecting related substances in hydroquinone and application thereof
  • High performance liquid chromatography method for efficiently separating and detecting related substances in hydroquinone and application thereof
  • High performance liquid chromatography method for efficiently separating and detecting related substances in hydroquinone and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0158] Example 1 The preparation of hydroquinone of the present invention

[0159] The preparation method of hydroquinone, comprises the steps:

[0160] 1) MnO 2 Add 280g, 430g of 98% sulfuric acid, and 2.0L of water into the reaction flask, slowly add 100g of aniline dropwise at 5-10°C, stir, and gradually raise the temperature to about 25°C until the reaction is complete. The reaction liquid is steam distilled at 60-90°C, and the collected p-benzoquinone condensate is introduced into another reaction flask;

[0161] 2) Under the condition of shading and nitrogen protection, add 42g of iron powder to the collected p-benzoquinone condensate, stir and react for 3-4 hours at 90-100°C, until the reaction is complete, filter, and depressurize the collected filtrate Concentrating to a hydroquinone content of 35% in the concentrated solution;

[0162] 3) Add 550mg of sodium metabisulfite, 2.2g of activated carbon, and 330mg of zinc powder to the concentrated solution, heat to ...

Embodiment 2

[0163] Example 2 The preparation of hydroquinone of the present invention

[0164] The preparation method of hydroquinone, comprises the steps:

[0165] 1) MnO 2 Add 350g, 500g of 98% sulfuric acid, and 2.0L of water into the reaction flask, slowly add 100g of aniline dropwise at 5°C-8°C, stir, and gradually raise the temperature to about 25°C until the reaction is complete. The reaction liquid is steam distilled at 60-90°C, and the collected p-benzoquinone condensate is introduced into another reaction flask;

[0166] 2) Under the conditions of shading and nitrogen protection, add 60g of iron powder to the collected p-benzoquinone condensate, stir and react for 2-3 hours at 90-100°C, until the reaction is complete, filter, collect the filtrate and concentrate under reduced pressure To the hydroquinone content in the concentrated solution is 25%;

[0167] 3) Add 750 mg of sodium pyrosulfite, 3.1 g of activated carbon, and 500 mg of iron powder to the concentrated solutio...

Embodiment 3

[0168] Example 3 The preparation of hydroquinone of the present invention

[0169] The preparation method of hydroquinone, comprises the steps:

[0170] 1) MnO 2 Add 250g, 370g of 98% sulfuric acid, and 2.5L of water into the reaction flask, slowly add 100g of aniline dropwise at 6-10°C, stir, and gradually raise the temperature to about 25°C until the reaction is complete. The reaction liquid is steam distilled at 70-95°C, and the collected p-benzoquinone condensate is introduced into another reaction flask;

[0171] 2) Under the conditions of shading and nitrogen protection, add 31g of iron powder to the collected p-benzoquinone condensate, stir and react at 90-100°C for 2-3 hours, until the reaction is complete, filter, collect the filtrate and concentrate it under reduced pressure to The content of hydroquinone in the concentrated solution is 30%;

[0172] 3) Add 550 mg of sodium pyrosulfite, 2.20 g of activated carbon, and 350 mg of zinc powder to the concentrated s...

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Abstract

A high performance liquid chromatography for efficiently separating and detecting related substances in hydroquinone is characterized in that a chromatographic column in the method is selected from any one of a reversed-phase column or a normal-phase column capable of adopting a reversed-phase solvent; a mobile phase is composed of a phase A and a phase B, wherein the phase A is selected from anyone of water, a methanol aqueous solution and an acetonitrile aqueous solution; and the phase B is selected from any one of methanol and acetonitrile, the detection wavelength is 200-400 nm, the sample size is 1-100 [mu]l, and the column temperature is 10-45 DEG C. The detection method provided by the invention realizes effective separation of hydroquinone and related substances, significantly improves the medication safety of hydroquinone, and has the advantages of simple operation, high separation degree, good specificity, high sensitivity and the like.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to a high-performance liquid chromatography for efficiently separating and detecting related substances in hydroquinone and an application thereof. Background technique [0002] As a tyrosinase inhibitor, hydroquinone (also known as hydroquinone) mainly inhibits tyrosinase activity through complexation, regulates the metabolic process of melanocytes, and significantly reduces the number of dopa-positive melanocytes in the epidermis, resulting in reversible Sexual skin discoloration. Oettel first proposed in 1936 that hydroquinone has the effect of whitening the skin. Since the 1960s, many countries have used hydroquinone as a whitening agent in cosmetics and in dermatology for the treatment of pigmentation, freckles and other external preparations. But the amount of hydroquinone must be strictly controlled. [0003] [0004] Hydroquinone is unstable and susce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06A61K8/34A61Q19/02C07C39/08C07C37/84C07C37/86C07C37/00A61K31/05A61P17/00
CPCG01N30/02G01N30/06A61K8/347A61Q19/02C07C37/84C07C37/86C07C37/002A61K31/05C07C46/00A61P17/00G01N2030/065G01N2030/027A61K2800/782C07C39/08C07C50/04
Inventor 苏冠荣尹贝立
Owner 广东人人康药业有限公司
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