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High performance liquid chromatographic analysis method for antioxidant 1076 content

A technology of high performance liquid chromatography and analysis method, which is applied in the field of high performance liquid chromatography analysis of antioxidant 1076 content

Active Publication Date: 2010-05-19
SHANGHAI CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, there is no published report on the method for accurately measuring the content of antioxidant 1076 with the HPLC analysis method

Method used

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  • High performance liquid chromatographic analysis method for antioxidant 1076 content
  • High performance liquid chromatographic analysis method for antioxidant 1076 content
  • High performance liquid chromatographic analysis method for antioxidant 1076 content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Selection of High Performance Liquid Chromatography Conditions

[0041] 1.1 Selection of mobile phase

[0042] The experimental results show that the solubility of antioxidant 1076 in water is poor, so the mobile phase with lower water content is suitable for use. When eluted isocratically with 100% methanol, the resolution of raw material, intermediate and antioxidant 1076 is good, but the resolution of raw material and intermediate is not good; when eluted isocratically with 90% methanol-10% water , the separation degree of raw materials and intermediates is good, but the peak eluting time of antioxidant 1076 is too long, taking into account the separation effect and analysis time, gradient elution is adopted.

[0043] Gradient conditions: 0 min 90% methanol-10% water, 5 min 90% methanol-10% water, 10 min 100% methanol-0% water, flow rate of mobile phase: 0.8ml / min.

[0044] 1.2 Selection of detection wavelength

[0045] Use a diode array detector to scan continuou...

Embodiment 2

[0047] Preparation of standard solution

[0048] Accurately weigh 0.5309g of antioxidant 1076 standard product, put it in a 50ml volumetric flask, add 5ml of n-hexane to dissolve it, then dilute to 50ml with methanol, shake well, and make an antioxidant with a concentration of 0.02mol / L The standard stock solution of 1076 is diluted step by step to the required concentration when used.

[0049] Accurately weigh 0.2924g of the intermediate β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid methyl ester standard product, place it in a 50ml volumetric flask, add methanol to dissolve it, and then use methanol to make it volume to 50ml, shake well, and make a standard stock solution of the intermediate product with a concentration of 0.02mol / L, and gradually dilute to the required concentration when used.

[0050] Accurately weigh 0.2063g of 2,6-di-tert-butylphenol, place it in a 50ml volumetric flask, add methanol to dissolve it, then dilute to 50ml with methanol, shake well, an...

Embodiment 3

[0052] Preparation of Standard Curve

[0053] Select the high performance liquid chromatography condition of the present invention, that is, the chromatographic column is C 18 Column, 5 μm, 150×4.6mm (I.D.); mobile phase composition (volume ratio) and gradient conditions: 0min 90% methanol-10% water, 5min 90% methanol-10% water, 10min 100% methanol-0% water; Flow rate: 0.8ml / min; Column temperature: 25°C; Detection wavelength: 220nm; Injection volume: 20μl.

[0054] Get the sample injection of antioxidant 1076 standard solution, plot the concentration with the peak area (see figure 2 ). The concentration of antioxidant 1076 in the solution is 1.5×10 -4 ~1.5×10 -3 The linear relationship is good in the range of mol / L, and the regression equation is:

[0055] A 抗氧剂1076 =-41443.2+6.66686E9C, r=0.9968

[0056] Get intermediate β-(3,5-di-tert-butyl-4-hydroxyphenyl) methyl propionate standard solution injection, plot concentration with peak area (see image 3 ). The concen...

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Abstract

The invention discloses a high performance liquid chromatographic analysis method for antioxidant 1076, which adopts a reserved phase high performance liquid chromatography method. The reserved phase high performance liquid chromatography comprises the following conditions that: the chromatographic column is a C18 column and is of 5 mu m and 150*4.6 mm (I.D.); the mobile phase comprises the following components in a volume ratio with gradient conditions: 90 percent of methanol and 10 percent of water in 0 minute, 90 percent of methanol and 10 percent of water in 5 minutes, and 100 percent of methanol and 0 percent of water in 10 minutes; and the flow rate is 0.8 milliliter per minute, the column temperature is 25 DEG C, the detection wavelength is 220 nanometers, and the sampling volume is 20 microliters. The chromatographic analysis method of the invention accurately measures the main body content of the antioxidant 1076, further measures the contents of an intermediate beta-(3,5-tertbutyl-4-hydroxyphenyl) methyl propionate and a raw material 2,6-ditertbutyl phenol at the same time, and is suitable for quality control of the antioxidant 1076 in the industrialized production process.

Description

technical field [0001] The invention relates to a high performance liquid chromatography analysis method for the content of antioxidant 1076. Background technique [0002] The chemical name of antioxidant 1076 is β-(4-hydroxyphenyl-3,5-di-tert-butyl) n-octadecyl propionate, which is a highly efficient hindered phenolic antioxidant, which is compatible with most Polymers have good compatibility, prevent discoloration caused by light and heat, and can inhibit the oxidative and thermal degradation of many organic compounds and polymers. [0003] Antioxidant 1076 has good heat resistance and water extraction resistance, and is widely used in polyethylene, polypropylene, polyoxymethylene, ABS resin, polystyrene, polyvinyl chloride, engineering plastics, synthetic rubber and petroleum products. [0004] The preparation of antioxidant 1076 uses 2,6-di-tert-butylphenol, methyl acrylate, and stearyl alcohol as the main raw materials, and potassium tert-butoxide as the catalyst, and ...

Claims

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Application Information

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