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Detection method for content of enantiomer in L-alanine isopropyl ester

A technology of isopropyl alanine and enantiomers, which is applied in the field of high performance liquid chromatography detection of enantiomer content, can solve the enantiomerization of L-isopropyl alanine hydrochloride No pharmacopoeia and other problems, to achieve the effect of strong specificity, high sensitivity, good accuracy and durability

Inactive Publication Date: 2020-02-28
ZHENGZHOU TAIFENG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Currently L-alanine isopropyl hydrochloride enantiomer has no pharmacopoeia and other statutory standards

Method used

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  • Detection method for content of enantiomer in L-alanine isopropyl ester
  • Detection method for content of enantiomer in L-alanine isopropyl ester
  • Detection method for content of enantiomer in L-alanine isopropyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] specificity test

[0029] Adopt the method among the present invention.

[0030] Chromatographic column: CROWNPAKCR (+) (4.0mm×150mm, 5μm)

[0031] Mobile phase: Perchloric acid aqueous solution at pH 1.0

[0032] Flow rate: 0.5ml / min

[0033] Column temperature: 20°C

[0034] Detection wavelength: 205nm

[0035] Injection volume: 20μl

[0036] Experimental steps:

[0037] Blank solvent: purified water

[0038] Preparation of system suitability solution: Take the appropriate amount of impurity TN-SM2-R2 reference substance, enantiomer reference substance and L-alanine isopropyl ester hydrochloride reference substance respectively, add purified water to dissolve and dilute to make each A mixed solution containing about 50 μg of impurity TN-SM2-R2 and 50 μg of enantiomers in 1 ml, and 2.5 mg of L-alanine isopropyl ester hydrochloride is used as a system suitability solution.

[0039] Preparation of sample solution: Take an appropriate amount of this product, weigh...

Embodiment 2

[0048] Limit of detection and limit of quantitation tests.

[0049] The chromatographic method in Example 1 was used.

[0050] Experimental steps:

[0051] Blank solvent: purified water

[0052] Limit of detection and limit of quantitation solution: Take appropriate amount of L-alanine isopropyl ester hydrochloride and enantiomer reference substance, add anhydrous purified water to prepare solutions with a series of concentrations, and measure according to the law. The quantification limit and detection limit of the substance were judged by the signal-to-noise ratio.

[0053] The results are shown in Table 1 below.

[0054]

Embodiment 3

[0056] Linearity and Range

[0057] The chromatographic method in Example 1 was used.

[0058] Experimental steps:

[0059] Blank solvent: purified water

[0060] Linear solution: Take an appropriate amount of L-alanine isopropyl ester hydrochloride and enantiomer reference substance, add purified water to prepare solutions with a series of concentrations, and measure according to the law.

[0061] Results: The enantiomer of L-alanine isopropyl ester hydrochloride had a good linear relationship in the concentration range of 0.5214 μg / ml-20.8560 μg / ml, and the concentration of L-alanine isopropyl ester hydrochloride was 0.5410 μg / ml The linear relationship is good in the concentration range of ml-21.6560μg / ml. The specific results are shown in Table 2 below, and the linear relationship diagram is shown in the appendix Figure 5 , Figure 6 .

[0062]

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Abstract

The invention belongs to the field of pharmaceutical analysis, and particularly relates to a high performance liquid chromatography detection method for the content of enantiomer in L-alanine isopropyl ester hydrochloride. According to the method, high performance liquid chromatography is used for determination, a crown ether chiral chromatographic column is used, and a perchloric acid aqueous solution with the pH value of 1.0 serves as the mobile phase. Thus, the L-alanine isopropyl ester hydrochloride can be effectively separated from the corresponding enantiomer, and the content of enantiomer can be detected more accurately. According to the method, a reversed-phase method and isocratic elution are used, operation is simple, peak shape is better, the separation degree is qualified, andvia methodological verification, the method is high in specificity, sensitivity, accuracy and durability.

Description

technical field [0001] The invention belongs to the field of drug analysis, and in particular relates to a high performance liquid chromatography detection method for enantiomer content in L-alanine isopropyl ester hydrochloride. Background technique [0002] L-alanine isopropyl ester hydrochloride: molecular formula is C 6 h 14 ClNO 2 , the molecular weight is 167.63, and its chemical structure is: [0003] [0004] L-alanine isopropyl ester hydrochloride is an important starting material in the synthesis process of tenofovir alafenamide, which has a chiral center, and the L-alanine isopropyl ester hydrochloride Enantiomer impurity is one of the sources of tenofovir alafenamide chiral impurity, and it is necessary to strictly control the enantiomer content of L-alanine isopropyl ester hydrochloride. [0005] At present, there is no legal standard such as pharmacopoeia for the enantiomer of L-alanine isopropyl ester hydrochloride. Therefore, it is necessary to develo...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 沙薇杨苗苗吕艳歌
Owner ZHENGZHOU TAIFENG PHARMA CO LTD
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