Check patentability & draft patents in minutes with Patsnap Eureka AI!

Detection method for PHBA process impurities

A detection method and detector technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve high sensitivity and specificity, good industrial applicability, fast and efficient detection method

Active Publication Date: 2017-08-29
CHENGDU LIKAI CHIRAL TECH
View PDF1 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the separation and analysis of PHBA-related process impurities.

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
  • Detection method for PHBA process impurities
  • Detection method for PHBA process impurities
  • Detection method for PHBA process impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The choice of solvent and the choice of solution concentration

[0047] The choice of solvent for dissolving the sample, we use acetonitrile and mobile phase to dissolve the sample, both of which can be dissolved. In order to reduce the appearance of solvent peaks, we use the mobile phase to dissolve the sample.

Embodiment 2

[0049] Instruments and testing conditions

[0050] U.S. Agilent 1200 high-performance liquid chromatograph, autosampler; Phenomenex C18 column (4.6 * 250mm, 5 μ m); Mobile phase is aqueous phase (pure water): acetonitrile=50:50 (V / V); 20 μl; the detection wavelength is 280nm; the flow rate is 0.8ml / min; the column temperature is 30°C.

[0051] Experimental procedure

[0052] Take an appropriate amount of PHBA and its impurities, dissolve and dilute it with mobile phase to make a solution containing 0.5mg of PHBA, 0.5mg of impurity A and 0.5mg of impurity B per 1ml, shake well, and use it as the test solution to inject and measure according to the above conditions, record Chromatogram, see the results figure 1 .

[0053] figure 1 It shows that PHBA, impurity A and impurity B merge into one peak and fail to achieve separation.

Embodiment 3

[0055] Instruments and testing conditions

[0056] U.S. Agilent 1200 high-performance liquid chromatograph, autosampler; Phenomenex C18 post (4.6 * 250mm, 5 μ m); Mobile phase is aqueous phase (0.1% trifluoroacetic acid-water:):acetonitrile=50:50 (V / V ); the injection volume is 20μl; the detection wavelength is 280nm; the flow rate is 0.8ml / min; the column temperature is 30°C.

[0057] Experimental procedure

[0058] Take an appropriate amount of PHBA and its impurities, dissolve and dilute it with mobile phase to make a solution containing 0.5mg of PHBA, 0.5mg of impurity A and 0.5mg of impurity B per 1ml, shake well, and use it as the test solution to inject and measure according to the above conditions, record Chromatogram, see the results figure 2 .

[0059] figure 2 It shows that the separation degree of PHBA and impurity A is less than 1.5, and the separation degree of PHBA and impurity B meets the requirements of the 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
wavelengthaaaaaaaaaa
Login to View More

Abstract

The invention discloses a detection method for PHBA process impurities. According to the detection method, normal-phase high-performance liquid chromatography is employed. Chromatographic conditions are that a C18 column or C8 column is used as a chromatographic column; a mobile phase is composed of a water phase and acetonitrile in a ratio of 70: 30 to 40: 60; the flow velocity of the mobile phase is 0.7 to 1.0 mL / min; detection wavelength is 220 to 280 nm; column temperature is 20 to 40 DEG C; and an ultraviolet detector or diode array detector is used as a detector. The detection method provided by the invention realizes separation of PHBA from the process impurity A and process impurity B of PHBA, has high sensitivity and specificity and is simple to operate; the degree of separation is greater than 1.50, which accords with regulations prescribed in Chinese Pharmacopoeia; the detection method can be used for quality control separation of PHBA, and peak appearance time of the method is within 10 min; and the detection method is fast and highly efficient and has good industrial practicality.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for detecting impurities in a PHBA process. Background technique [0002] PHBA, namely (S)-α-hydroxy-γ-N-phthalimidobutyric acid, is an important intermediate for the synthesis of amikacin. Amikacin, commonly known as amikacin and amikacin, is a third-generation semi-synthetic aminoglycoside antibiotic that is effective against Escherichia coli, Klebsiella, Enterobacter, Proteus, Chi Shigella, Salmonella, Pseudomonas aeruginosa and other Pseudomonas, Acinetobacter, Alcaligenes, etc. have strong pharmacological effects; against Neisseria meningitidis, Neisseria gonorrhoeae, influenza Haemophilus, Yersinia, Campylobacter fetalis, Mycobacterium tuberculosis and certain non-tuberculous mycobacteria have strong pharmacological effects. Amikacin has the advantages of low ototoxicity and nephrotoxicity, and its share in aminoglycoside antibiotics has risen from 5% in 19...

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
Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 袁伟成葛真真周鸣强徐小英刘斌
Owner CHENGDU LIKAI CHIRAL TECH
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com