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Detection method and application of impurities in synthetic raw materials of tenofovir fumarate

A technology of propofol fumarate and tenofovir, which is applied in the field of detection of impurities in raw materials for the synthesis of propofol fumarate and tenofovir, can solve the problems of low response value and low accuracy of detection results, and achieve Realize the effect of quality control

Active Publication Date: 2022-01-04
HINYE PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In the related art, the control of impurities in the raw material of L-alanine isopropyl ester is detected by the derivatization treatment of the impurities in the raw material. The derivatization process has the problem of low response value, which leads to low accuracy of the detection results.

Method used

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  • Detection method and application of impurities in synthetic raw materials of tenofovir fumarate
  • Detection method and application of impurities in synthetic raw materials of tenofovir fumarate
  • Detection method and application of impurities in synthetic raw materials of tenofovir fumarate

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Embodiment 1

[0110] The present embodiment is: a detection method of L-alanine isopropyl ester in tenofovir alafenamide fumarate, comprising the following steps:

[0111] S1, preparation solution:

[0112] Diluent: Mix acetonitrile and water at a volume ratio of 20:80 to obtain the diluent.

[0113] Blank solution: diluent.

[0114]L-alanine reference substance stock solution: take about 30 mg of L-alanine (CAS No.: 56-41-7) reference substance, weigh it accurately, put it in a 20mL measuring bottle, dissolve it with diluent and dilute to the mark, Shake well to obtain the L-alanine reference substance stock solution (concentration 1500μg / mL).

[0115] L-alanine methyl ester reference substance stock solution: Take about 5 mg of impurity L-alanine methyl ester (CAS number: 114041-77-9) reference substance, weigh it accurately, put it in a 100mL measuring bottle, and dissolve it with diluent And dilute to the mark, shake well to obtain L-alanine methyl ester reference substance stock sol...

Embodiment 2

[0219] This embodiment is: a kind of detection method of L-alanine isopropyl ester, and the difference of embodiment 1 is:

[0220] Mobile phase A is: pure water;

[0221] Mobile phase B is: acetonitrile.

Embodiment 3

[0223] This embodiment is: a kind of detection method of L-alanine isopropyl ester, and the difference of embodiment 1 is:

[0224] Gradient elution is performed as follows:

[0225] 0min~5min, the volume fraction of described mobile phase A is 60%;

[0226] 5min~15min, the volume fraction of described mobile phase A drops to 40% by 60%;

[0227] 15min~18min, the volume fraction of described mobile phase A is raised to 60% by 40%;

[0228] 18min~25min, the volume fraction of described mobile phase A is 60%.

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Abstract

The invention discloses a detection method and application of impurities in raw materials for synthesizing tenofovir alafenamide fumarate. The detection method comprises the following steps: taking the test solution and detecting it by liquid chromatography-mass spectrometry; The liquid chromatography includes the following conditions: mobile phase A: formic acid solution; mobile phase B: acetonitrile; elution method: gradient elution. The invention realizes the quality control of the impurities in the L-alanine isopropyl ester raw material by liquid chromatography-mass spectrometry. The detection method of the invention has good system applicability, good specificity, low detection limit, high sensitivity, good linear relationship, high accuracy, good repeatability and good stability.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for detecting impurities in synthetic raw materials of tenofovir alafenamide fumarate and its application. Background technique [0002] Hepatitis B virus infection is a worldwide infectious disease. The development of tenofovir alafenamide fumarate provides a new option for the clinical treatment of hepatitis B infection. [0003] The production process of tenofovir alafenamide fumarate raw material may introduce impurities such as starting materials, and at the same time, during the production, storage and transportation of the raw material, by-products or other degradation products may also be produced. The quality control of its starting materials is extremely important. [0004] L-alanine isopropyl ester is a kind of important starting material in the synthetic process of tenofovir alafenamide fumarate, and its molecular formula is C 6 h 13 NO 2 , the mol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/72
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/72G01N2030/324
Inventor 刘栋华尚金凤马晓宁李承龙
Owner HINYE PHARM CO LTD