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High performance liquid chromatography for efficiently separating and detecting p-benzoquinone in hydroquinone and application thereof

A high-performance liquid chromatography and p-benzoquinone technology, applied in the field of drug analysis, to achieve the effects of high sensitivity, efficient separation and detection, and controllable drug quality

Active Publication Date: 2020-12-25
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 for efficiently separating and detecting p-benzoquinone in hydroquinone and application thereof
  • High performance liquid chromatography for efficiently separating and detecting p-benzoquinone in hydroquinone and application thereof
  • High performance liquid chromatography for efficiently separating and detecting p-benzoquinone in hydroquinone and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0141] Example 1 The preparation of hydroquinone of the present invention

[0142] The preparation method of hydroquinone, comprises the steps:

[0143] 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;

[0144] 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;

[0145] 3) Add 550mg of sodium metabisulfite, 2.2g of activated carbon, and 330mg of zinc powder to the concentrated solution, heat to ...

Embodiment 2

[0146] Example 2 The preparation of hydroquinone of the present invention

[0147] The preparation method of hydroquinone, comprises the steps:

[0148] 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;

[0149] 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%;

[0150] 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

[0151] Example 3 The preparation of hydroquinone of the present invention

[0152] The preparation method of hydroquinone, comprises the steps:

[0153] 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;

[0154] 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%;

[0155] 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

The invention relates to a high performance liquid chromatography for efficiently separating and detecting p-benzoquinone in hydroquinone. A chromatographic column in the method is selected from any one of a reversed phase column or a normal phase column 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 any one of water,a methanol water solution and an acetonitrile water solution; the phase B is selected from any one of methanol and acetonitrile; the detection wavelength is 200 to 400nm, the sample feeding amount is1 to 100 microliters and the column temperature is 10 to 45 DEG C according to the detection method provided by the invention, effective separation and detection of the hydroquinone and related substances are realized and the drug safety of the hydroquinone is remarkably improved; and the high performance liquid chromatography has the advantages of simplicity and convenience for 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, in particular to a high-performance liquid chromatography for efficiently separating and detecting the content of p-benzoquinone in hydroquinone and its application. Background technique [0002] Hydroquinone (also known as hydroquinone) is a tyrosinase inhibitor, which mainly inhibits tyrosinase activity through complexation, regulates the metabolic process of melanocytes, significantly reduces the number of dopa-positive melanocytes in the epidermis, and produces Reversible 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 susceptible to oxi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74
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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