Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

HPLC detecting method for tenofovir alafenamide and isomer thereof

A technology for tenofovir alafenamide and a detection method is applied in the field of HPLC detection of tenofovir alafenamide and its isomers, and can solve the problem of long running time and inability to tenofovir alafenamide. The separation of amine and its isomers impurities, the complex mobile phase preparation and other problems, to achieve the effect of accurate results and good resolution

Active Publication Date: 2018-02-02
厦门蔚扬药业有限公司
View PDF6 Cites 10 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In Method 1, the chromatographic column adopts a chiral chromatographic column, and the price is 4 to 5 times that of ordinary C18, and the mobile phase used in the elution process is an organic phase, and the separation cost is high; in Method 2, the preparation of the mobile phase is complicated, and The running time is long, and more importantly, it has been verified that tenofovir alafenamide and its isomer impurities cannot be effectively separated. Therefore, it is necessary to detect tenofovir alafenamide and its isomer impurities. Isomer impurity method for a more in-depth study

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • HPLC detecting method for tenofovir alafenamide and isomer thereof
  • HPLC detecting method for tenofovir alafenamide and isomer thereof
  • HPLC detecting method for tenofovir alafenamide and isomer thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A method for separating and determining tenofovir alafenamide and its isomers, specifically comprising the steps of:

[0043] 1) Column: Kromstar C 18 (4.6×250 mm×5 µm);

[0044] 2) Column temperature: 30°C;

[0045] 3) Wavelength: 260nm;

[0046] 4) Injection volume: 5 µL;

[0047] 5) Flow rate: 1.0 mL / min;

[0048] 6) Isocratic elution: methanol: 0.1% phosphoric acid aqueous solution = 40:60.

[0049] see results figure 1 , figure 1 The chromatographic peak at 19.892 min is the chromatographic peak of the isomers of tenofovir alafenamide, and the chromatographic peak at 21.863 min is the chromatographic peak of tenofovir alafenamide. The separation degree of the two was 1.83, meeting the requirements of the Chinese Pharmacopoeia.

Embodiment 2

[0051] A method for separating and determining tenofovir alafenamide and its isomers, specifically comprising the steps of:

[0052] 1) Column: Kromstar C 18 (4.6×250 mm×5 µm);

[0053] 2) Column temperature: 30°C;

[0054] 3) Wavelength: 260nm;

[0055] 4) Injection volume: 5 µL;

[0056] 5) Flow rate: 1.0 mL / min;

[0057] 6) Isocratic elution: methanol: 0.1% formic acid aqueous solution = 40:60.

[0058] see results figure 2 , figure 2 The chromatographic peak at 29.038 min is the chromatographic peak of the isomers of tenofovir alafenamide, and the chromatographic peak at 31.850 min is the chromatographic peak of tenofovir alafenamide. The separation degree of the two is 2.13, meeting the requirements of the Chinese Pharmacopoeia.

Embodiment 3

[0060] A method for separating and determining tenofovir alafenamide and its isomers, specifically comprising the steps of:

[0061] 1) Column: Kromstar C 18 (4.6×250 mm×5 µm);

[0062] 2) Column temperature: 30°C;

[0063] 3) Wavelength: 260nm;

[0064] 4) Injection volume: 5 µL;

[0065] 5) Flow rate: 1.0 mL / min;

[0066] 6) Isocratic elution: Methanol: 0.1% trifluoroacetic acid aqueous solution = 40:60.

[0067] see results image 3 , image 3The chromatographic peak at 33.892 min is the chromatographic peak of the isomers of tenofovir alafenamide, and the chromatographic peak at 36.342 min is the chromatographic peak of tenofovir alafenamide. The separation degree of the two is 1.62, meeting the requirements of the Chinese Pharmacopoeia.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Column lengthaaaaaaaaaa
Wavelengthaaaaaaaaaa
Login to View More

Abstract

The invention relates to a fractionation detection method for tenofovir alafenamide and isomer thereof, and belongs to the technical field of fractionation detection. The detection method comprises the following steps: taking a chromatographic column filled with octadecylsilane chemically bonded silica; and carrying out isocratic elution by taking methanol and an acidic aqueous solution as mobilephases under certain conditions. By the method, the tenofovir alafenamide and the isomer thereof can be effectively detected in a fractionation manner, the peak pattern of chromatographic peaks is good, the appearance time is short, and the degree of fractionation is good.

Description

technical field [0001] The invention relates to an HPLC detection method for tenofovir alafenamide and its isomers, belonging to the technical field of drug detection. Background technique [0002] Tenofovir alafenamide is a novel nucleotide reverse transcriptase inhibitor and a prodrug of tenofovir. The drug is an improved version of Gilead's marketed drug Viread®, which has been approved by the United States for the treatment of adults with uncompensated chronic hepatitis B. Compared with Viread®, the clinical dosage of tenofovir alafenamide is smaller, it only needs 1 / 10 of Viread® to have equivalent antiviral efficacy, better safety, and can improve renal function and Bone safety parameters. [0003] The structure of tenofovir alafenamide is shown in the following formula (1): [0004] (1). [0005] In the preparation process of tenofovir alafenamide, the racemate is first synthesized and then transformed, so the synthesized tenofovir alafenamide may have isomer im...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 蔡惠坚顾世海
Owner 厦门蔚扬药业有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com