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

Method for determining related substances in carteolol hydrochloride and eye drops thereof by ultra-high performance liquid chromatography

A technique for ultra-high performance liquid phase and related substances, which is applied in the field of ultra-high performance liquid chromatography for the determination of carteolol hydrochloride and related substances in eye drops, and can solve the problems of not being able to separate and detect 11 impurities at the same time.

Active Publication Date: 2022-03-25
SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the analysis and detection methods for related substances of catenolol hydrochloride are all recorded in the Chinese Pharmacopoeia, the United States Pharmacopoeia, the European Pharmacopoeia, and the British Pharmacopoeia, wherein the Chinese Pharmacopoeia and the United States Pharmacopoeia all use thin-layer chromatography to detect related substances; The Pharmacopoeia is the same as the British Pharmacopoeia, both use octadecylsilane bonded silica gel as filler, and use methanol: acetonitrile: 2.82g / L sodium hexanesulfonate solution (1:20:79) as mobile phase for isocratic elution , the flow rate is 1ml / min, the detection wavelength is 252nm, the injection volume is 20μl, and the self-control method without correction factor is used for the detection of impurities; but the above methods cannot simultaneously separate and detect the 11 impurities described above

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
  • Method for determining related substances in carteolol hydrochloride and eye drops thereof by ultra-high performance liquid chromatography
  • Method for determining related substances in carteolol hydrochloride and eye drops thereof by ultra-high performance liquid chromatography
  • Method for determining related substances in carteolol hydrochloride and eye drops thereof by ultra-high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The instrument and chromatographic conditions adopted are as follows:

[0029] (1) Ultra-high performance liquid chromatography: Waters UPLC H-class; detector: PDA;

[0030] (2) Chromatographic column: WatersACQUITY BEH C18 column (1.7μm, 2.1mm×100mm)

[0031] (3) mobile phase A phase: acetonitrile; mobile phase B phase: 0.282% sodium hexanesulfonate solution (10% phosphoric acid to adjust the pH value to 3.0);

[0032] (4) Detection conditions: flow rate: 0.3ml / min; column temperature: 35°C; detection wavelength: 252nm; injection volume: 2μl; gradient elution of mobile phase A and B according to the gradient in Table 1;

[0033] Table 1 Gradient elution program table

[0034]

[0035] Sample preparation:

[0036] Applicable solution for the system: take about 5 mg of the above-mentioned 11 impurity reference substances, weigh them accurately, put them in a 50ml measuring bottle, add an appropriate amount of solvent to dissolve and set the volume to the mark, sh...

Embodiment 2

[0049] The instrument and chromatographic conditions adopted are as follows:

[0050] (1) Ultra-high performance liquid chromatography: Waters UPLC H-class; detector: PDA;

[0051] (2) Chromatographic column: WatersACQUITY BEH C18 column (1.7μm, 2.1mm×100mm)

[0052] (3) mobile phase A phase: acetonitrile; mobile phase B phase: 0.254% sodium hexanesulfonate solution (10% phosphoric acid to adjust the pH value to 2.8);

[0053] (4) Detection conditions: flow rate: 0.28ml / min; column temperature: 30°C; detection wavelength: 250nm; injection volume: 1 μl; gradient elution of mobile phase A and B according to the gradient in Table 2;

[0054] Table 2 Gradient elution program table

[0055]

[0056] Sample preparation is the same as in Example 1

[0057] Operation steps are with embodiment 1

Embodiment 3

[0059] The instrument and chromatographic conditions adopted are as follows:

[0060] (1) Ultra-high performance liquid chromatography: Waters UPLC H-class; detector: PDA;

[0061] (2) Chromatographic column: WatersACQUITY BEH C18 column (1.7μm, 2.1mm×100mm)

[0062] (3) mobile phase A phase: acetonitrile; mobile phase B phase: 0.310% sodium hexanesulfonate solution (10% phosphoric acid to adjust the pH value to 3.2);

[0063] (4) Detection conditions: flow rate: 0.32ml / min; column temperature: 40°C; detection wavelength: 254nm; injection volume: 3μl; gradient elution of mobile phase A and B according to the gradient in Table 3;

[0064] Table 3 Gradient elution program table

[0065]

[0066] Sample preparation is the same as in Example 1

[0067] Operation steps are with embodiment 1

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
particle diameteraaaaaaaaaa
lengthaaaaaaaaaa
Login to View More

Abstract

The invention belongs to the field of analytical chemistry, and particularly relates to a method for determining related substances in carteolol hydrochloride and eye drops thereof by ultra-high performance liquid chromatography, which adopts a Waters ultra-high performance liquid chromatograph, adopts a chromatographic column with octadecylsilane chemically bonded silica as a filler, adopts acetonitrile as a mobile phase A and adopts a 0.282% sodium hexanesulfonate solution as a mobile phase B, and adopts an ultra-high performance liquid chromatography method for determining the related substances in carteolol hydrochloride and eye drops thereof. And carrying out gradient elution. The method not only can completely separate and detect nine known impurities contained in each pharmacopeia at the same time, but also can separate and detect initial raw materials and intermediates, especially 1, 3-cyclohexanedione and 3-amino-2-cyclohexenone, in the synthesis process of carteolol hydrochloride, can more simply, conveniently, efficiently and accurately ensure controllable quality of carteolol hydrochloride and eye drops thereof, and is suitable for industrial production. And finally, the safety of the product is determined.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for determining related substances in carteolol hydrochloride and eye drops thereof by ultra-high performance liquid chromatography. Background technique [0002] Carteolol Hydrochloride (Carteolol Hydrochloride), the chemical name is 5-(3-tert-butylamino-2-hydroxypropoxy)-3,4-dihydro-2(1H)-quinolone hydrochloride, and its molecular formula is C 16 h 24 N 2 o 3 ·HCl, the molecular weight is 328.84, the CAS number is 51781-21-6, and its structural formula is shown in the following formula (a). [0003] [0004] Carteolol hydrochloride is a β-adrenergic receptor blocker with intrinsic sympathomimetic activity and membrane stabilizing effect, and is effective in the treatment of arrhythmia, angina pectoris, hypertension, glaucoma, cardiac neurosis and tetralogy of Fallot Significant curative effect on other diseases. Carteolol hydrochloride is widely ...

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): G01N30/02G01N30/06G01N30/34G01N30/89
CPCG01N30/02G01N30/06G01N30/34G01N30/89
Inventor 王静刘燕刘亚方张治云杨琪刘彩霞姜鹰雁国璐路曹煜杰
Owner SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES
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