High performance liquid chromatography analysis method for 2,2-2(3-amino-4-hydroxyl radical) phenyl propane and its impurity content

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

Inactive Publication Date: 2012-10-31
SHANGHAI HUAYI GRP CO
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no report on the method for measuring 2,2-bis(3-amino-4-hydroxyl)phenylpropane and its impurity content

Method used

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  • High performance liquid chromatography analysis method for 2,2-2(3-amino-4-hydroxyl radical) phenyl propane and its impurity content
  • High performance liquid chromatography analysis method for 2,2-2(3-amino-4-hydroxyl radical) phenyl propane and its impurity content
  • High performance liquid chromatography analysis method for 2,2-2(3-amino-4-hydroxyl radical) phenyl propane and its impurity content

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Experimental program
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Effect test

Embodiment 1

[0036] Embodiment 1: the selection of high performance liquid chromatography condition

[0037] 1.1 Selection of mobile phase

[0038] Secondary quartz distilled water (containing phosphoric acid-disodium hydrogen phosphate buffer solution with pH 7.0) and acetonitrile were mixed in proportion as the mobile phase, and the samples and standard solutions were analyzed. The results show that when the acetonitrile ratio is less than 55%, 2,2-bis(3-nitro-4-hydroxyl) phenylpropane and 2,2-bis(3-amino-4-hydroxyl)phenylpropane cannot achieve complete separation. In order to take into account the separation degree and the measurement time simultaneously, the ratio of acetonitrile-water (phosphoric acid-small diammonium hydrogen phosphate buffer solution containing pH7.0) is selected to be 70:30ml / ml (volume ratio). At this time, each component can realize Baseline separation, and analysis time and reasonableness, see Figure 1-b .

[0039] 1.2 Selection of detection wavelength

[...

Embodiment 2

[0043] Embodiment 2: the preparation of standard solution and sample solution

[0044] Accurately weigh 25.00mg of 2,2-bis(4-hydroxy-3-nitro)phenylpropane reference substance, place it in a 50ml volumetric flask, dissolve and dilute to the mark with mobile phase, shake well, and obtain a concentration of 0.5mg / ml of 2,2-bis(4-hydroxy-3-nitro)phenylpropane standard stock solution, when used, gradually dilute to the required concentration.

[0045] Accurately weigh 25.00mg of 2,2-bis(3-amino-4-hydroxy)phenylpropane reference substance, place it in a 50ml volumetric flask, dissolve and dilute to the scale with mobile phase, shake well, and obtain a concentration of 0.5mg / ml of 2,2-bis(3-amino-4-hydroxyl) phenylpropane standard stock solution, when used, gradually dilute to the required concentration.

Embodiment 3

[0046] Embodiment 3: the making of standard curve

[0047] Choose the best HPLC conditions, that is, the column is C 18 , 5 μ m, 150 * 4.6mm (I.D); The volume ratio that mobile phase is made up is: acetonitrile: phosphoric acid-disodium hydrogen phosphate buffer solution (pH7.0)=70: 30, ml / ml; Flow velocity is 0.8ml / min ; The column temperature is 28°C; the detection wavelength is 285nm.

[0048] Take 2,2-bis(3-nitro-4-hydroxyl) phenylpropane standard solution 15 μl sample injection, plot the concentration with the peak area ( image 3 ), 2,2-bis(3-nitro-4-hydroxy)phenylpropane solution at a concentration of 2.2×10 -3 In the range of ~1.0mg / ml, the sample concentration has a linear relationship with the peak area, and the linear regression equation is:

[0049] A 2,2-two (3-nitro-4-hydroxyl) phenylpropane=3.6307×10 2 +3.6843×10 4 C, r=0.99807

[0050] Take 2,2-two (3-amino-4-hydroxyl) phenylpropane standard solution 15 μl sample injection, plot the concentration with the...

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Abstract

The invention discloses an efficient liquid chromatographic-analysis method of 2, 2-bis (3-azyl-4-oxhydryl) phenyl propane and the impurity content thereof, which adopts a reversed phase efficient liquid chromatographic method. The efficient liquid chromatography satisfies the conditions that a chromatographic column satisfies C18, 5 mum and 150 multiplied by 4.6mm(I.D.); mobile phase compositions have the volume ratio that acetonitrile:phosphoric acid-phosphate buffer aqueous solution (the pH value is 7.0) equals to 70:30 (ml / ml); the flow speed is 0.8 ml / min; the column temperature is 28 DEG C; the detection wavelength is 285nm; the injection volume is 15 mul; and the concentration of injection samples whose contents are measured is diluted by 100 times through the mobile phase, a phosphate that is Na2HPO4 of 20mmol / l is added in the mobile phase, and then the pH value is regulated to reach 7.0 by using a phosphoric acid. The invention provides a simple and reliable analytical method for quality control analysis of 2, 2-bis (3-azyl-4-oxhydryl) phenyl propane.

Description

technical field [0001] The invention relates to a high performance liquid chromatography analysis method for 2,2-bis(3-amino-4-hydroxy)phenylpropane and its impurity content. Background technique [0002] 2,2-bis(3-amino-4-hydroxy)phenylpropane is an intermediate of a new type of intumescent N-P flame retardant, which has a wide range of applications in the fields of chemical building materials, electronic appliances, daily furniture, interior decoration application. Bisphenol A is nitrated to obtain the intermediate product 2,2-bis(3-nitro-4-hydroxyl)phenylpropane, and then the 2 , 2-bis(3-amino-4-hydroxy)phenylpropane. [0003] The reaction equation is: [0004] [0005] Known from above equation, there may be intermediate product 2 in 2,2-bis(3-amino-4-hydroxyl) phenylpropane product, 2-bis(3-nitro-4-hydroxyl) phenylpropane impurity, its content The level directly affects the quality of the final product 2,2-bis(3-amino-4-hydroxyl)phenylpropane. Therefore, it is ...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): G01N30/02G01N30/54
Inventor廖本仁钱柯君蒋旭亮黄莹刘慧青
OwnerSHANGHAI HUAYI GRP CO