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A kind of pretreatment method for detecting phenolic impurity content in samples

A detection method and impurity content technology, applied in the field of chemical analysis, can solve problems such as large deviation of results, large measurement results, and increased response value, and achieve low detection limit and quantification limit, good method durability, and the effect of inhibiting oxidation

Active Publication Date: 2021-12-14
广州国标检验检测有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

[0003] Existing determination methods usually use liquid chromatography to determine the solution in which phenols are directly dissolved and diluted. After this solution is prepared, phenolic impurities will be partially oxidized into quinone products, resulting in an increase in the response value, and the measurement results are more biased than the normal value. Larger, the longer the solution is left, the greater the deviation of the results

Method used

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  • A kind of pretreatment method for detecting phenolic impurity content in samples
  • A kind of pretreatment method for detecting phenolic impurity content in samples
  • A kind of pretreatment method for detecting phenolic impurity content in samples

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] The determination of phenolic impurity content is carried out to 5 batches of commercially available paroxetine hydrochloride raw materials, comprising the following steps:

[0077] (1) Preparation of reference solution

[0078] Accurately weigh 10 mg of 1,2,4-glucinol reference substance, place it in a 10 mL volumetric flask, first add 0.5 mL of vitamin C (content 100 μg / ml) in 50% acetonitrile solution to dissolve the reference substance, then add vitamin C (content 100 μg / ml) / ml) was diluted with 0.1% formic acid solution, and the volume was adjusted to the mark to obtain phenolic impurity reference substance stock solution Ⅰ with a concentration of 1 mg / mL. The 0.1% formic acid solution dilution is prepared into the reference substance solution of different concentrations;

[0079] (2) Sample pretreatment

[0080] Test product: Accurately weigh 0.1g of raw drug powder, place it in a 10mL volumetric flask, first add 0.5mL of vitamin C (content 100μg / ml) in 50% ace...

Embodiment 2

[0102] Investigate the stability time of phenolic impurities in the determination process, including the following steps:

[0103] (1) The preparation of the reference substance solution is the same as in Example 1;

[0104] (2) Sample pretreatment is the same as in Example 1;

[0105] (3) Liquid chromatography analysis conditions are the same as in Example 1;

[0106] (4) Result analysis

[0107] After standing for different lengths of time, detect the concentration of phenolic impurities in the reference substance solution and the standard recovery solution, and the liquid chromatography analysis results are as follows: Figure 24-Figure 39 , as shown in Table 4 and Table 5:

[0108]

[0109] The concentration of the impurity reference substance solution was 197.10ng / ml at 0h, 177.73ng / ml at 30h, and the absolute value of the concentration change rate was 9.8%, and 157.80ng / ml at 40h, and the concentration change rate was absolute The value is 19.9%, more than 15%. It...

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Abstract

The invention discloses a pretreatment method for detecting the content of phenolic impurities in a sample. The method comprises the following steps: weighing the sample, placing it in a volumetric flask, adding an acetonitrile solution of vitamin C, dissolving the sample, shaking well, and taking vitamin C dilute formic acid solution, filter, and the filtrate is used for instrumental analysis; the acetonitrile solution of vitamin C and the formic acid solution of vitamin C, wherein the content of vitamin C is 90-110 μ g / ml. By adopting the pretreatment method of the present invention, extremely low detection limits and quantitative limits can be achieved in the detection of phenolic impurities, and the repeatability is good; the stability time of the reference substance solution can also be extended to 30 hours, and the recovery of the solution after adding the standard can be achieved. The stability time is extended to 11 hours, and vitamin C and phenolic target substances can be effectively separated in the corresponding chromatographic system without interfering with the determination of target compounds.

Description

technical field [0001] The invention belongs to the field of chemical analysis, in particular to a pretreatment method for detecting the content of phenolic impurities in a sample. Background technique [0002] In the review of new drugs, phenolic genotoxic impurities are a type of impurities that must be controlled. Because phenolic substances have strong chemical activity and are easily oxidized, none of the existing methods can accurately and effectively determine trace phenolic impurities in samples. [0003] Existing determination methods usually use liquid chromatography to determine the solution in which phenols are directly dissolved and diluted. After this solution is prepared, phenolic impurities will be partially oxidized into quinone products, resulting in an increase in the response value, and the measurement results are more biased than the normal value. Larger, the longer the solution is left, the greater the deviation of the results. Contents of the invent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679
Inventor 郑传奇邱全玉陈亿展陈新国麦丽谊邵广志蒋杰
Owner 广州国标检验检测有限公司
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