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2-methoxymethyl-4-aminophenol and its impurity highly effective liquid phase chromatography analytical method

A high-performance liquid chromatography, methoxymethyl technology, applied in the direction of analysis of materials, material separation, measurement devices, etc., to achieve the effect of simple and reliable analysis methods

Inactive Publication Date: 2008-07-09
SHANGHAI CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no report on the method for measuring 2-methoxymethyl-4-aminophenol and its impurity content

Method used

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  • 2-methoxymethyl-4-aminophenol and its impurity highly effective liquid phase chromatography analytical method
  • 2-methoxymethyl-4-aminophenol and its impurity highly effective liquid phase chromatography analytical method
  • 2-methoxymethyl-4-aminophenol and its impurity highly effective liquid phase chromatography analytical method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: the selection of high performance liquid chromatography condition

[0031] 1.1 Selection of mobile phase

[0032] In the experiment, acetonitrile: water = 45: 5 5 was used for elution with equal flow ratio, and the separation of 2-methoxymethyl-4-aminophenol and impurities was good. However, due to the interaction between the amino and hydroxyl groups in 2-methoxymethyl-4-aminophenol and the residual silanol in the chromatographic column, the chromatographic peaks of 2-methoxymethyl-4-aminophenol have tailings. Phenomenon (Figure 1-a), affecting the accuracy of quantitative analysis of 2-methoxymethyl-4-aminophenol. Add phosphate 20mmol / l (NH 4 ) 2 HPO 4 The method of adjusting the pH value to 7.0 with phosphoric acid can eliminate the tailing phenomenon of chromatographic peaks (Fig. 1-b).

[0033] 1.2 Selection of detection wavelength

[0034] Continuously scan at 200-400nm with a diode array detector, 2-methoxymethyl-4-aminophenol has characterist...

Embodiment 2

[0037] Embodiment 2: the preparation of standard solution and sample solution

[0038] Accurately weigh 50.00mg of 2-methoxymethyl-4-aminophenol reference substance, place it in a 50ml volumetric flask, dissolve and dilute to the mark with mobile phase, shake well, and prepare 2-methoxymethyl-4-aminophenol with a concentration of 1.0mg / ml The standard stock solution of oxymethyl-4-aminophenol is gradually diluted to the required concentration when used.

[0039] Accurately weigh 25.00mg of 2-methoxymethyl-4-nitrophenol reference substance, place it in a 50ml volumetric flask, dissolve and dilute to the mark with mobile phase, shake well, and obtain 2-methoxymethyl-4-nitrophenol with a concentration of 0.5mg / ml The standard stock solution of oxymethyl-4-nitrophenol should be diluted step by step to the required concentration when used.

Embodiment 3

[0040] Embodiment 3: the making of standard curve

[0041] High performance liquid chromatography conditions: the chromatographic column is C 18 , 5 μ m, 150 × 4.6mm (I.D); The volume ratio of mobile phase composition: acetonitrile: phosphoric acid-phosphate buffered saline solution (PH7.0)=45: 55; Flow velocity 0.8ml / min; Column temperature 30 ℃; Detection wavelength 232nm . Take 10 μl of 2-methoxymethyl-4-aminophenol standard solution for injection, and plot the peak area against the concentration (Figure 3). 2-methoxymethyl-4-aminophenol is linear in the range of solution concentration 0.0001~1.0mg / ml, and the regression equation is:

[0042] A 2-甲氧甲基-4-氨基苯酚 =193754.33232+3.31341E7C, r=0.99997

[0043] Take 10 μl of 2-methoxymethyl-4-nitrophenol standard solution for injection, and plot the peak area against the concentration (Figure 4). 2-methoxymethyl-4-nitrophenol is linear in the range of solution concentration of 0.0001~0.10mg / ml, and the regression equation is: ...

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Abstract

The invention discloses a high-performance liquid chromatographic analysis method of 2-methoxymethyl-4-aminophenol and impurities thereof. The method comprises the following steps of: selecting reverse high-performance liquid chromatography; setting chromatographic conditions, wherein the chromatographic column is C18, 5 mum, 150*4.6 mm (I.D.), the mobile phase includes acetonitrile: phosphoric acid -phosphate buffer solution (pH 7.0) at a volume ratio of 45:55 with a flow rate of 0.8 ml / min, the column temperature is 30 DEG C, the detection wavelength is 232 nm, the injection dose is 5 to 10 mul, and (NH4)2HPO4 20 mmol / l is added into the mobile phase; adding phosphoric acid to adjust pH to 7.0; diluting the concentration of the injection sample to 1 / 50; and determining the contents of 2-methoxymethyl-4-aminophenol and the impurities thereof. The invention provides a simple and reliable method for quality control and analysis of 2-methoxymethyl-4-aminophenol.

Description

technical field [0001] The invention relates to a high performance liquid chromatography analysis method for 2-methoxymethyl-4-aminophenol and its impurities. Background technique [0002] 2-Methoxymethyl-4-aminophenol is a dye intermediate, especially as a color developer in oxidative hair dyes, and is widely used in the fields of dyes and hair dyes. The starting material 2-methoxymethyl-4-nitrophenol is reduced by hydrogen under the catalytic conditions of metal catalyst palladium, and 2-methoxymethyl-4-aminophenol can be prepared: [0003] [0004] 2-methoxymethyl-4-aminophenol may contain raw material 2-methoxymethyl-4-nitrophenol and other impurities, the content of which will directly affect the quality of the final product, and even cause great harm to the human body Therefore, it is very important to monitor the content of impurities such as raw material 2-methoxymethyl-4-nitrophenol when analyzing the content of 2-methoxymethyl-4-aminophenol. There is no report...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
Inventor 刘慧青黄莹
Owner SHANGHAI CHEM REAGENT RES INST
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