Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of reversed-phase liquid chromatography detects the method for raltitrexed enantiomer

A technology of reversed-phase liquid chromatography and enantiomers, which can be used in measuring devices, instruments, scientific instruments, etc. Volatility and other issues

Active Publication Date: 2020-02-04
南京和曦生物科技有限公司
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] (1) Normal phase liquid chromatography: This method uses n-hexane and isopropanol as eluting solvents, because n-hexane is extremely volatile, causing the laboratory to be filled with the smell of n-hexane, which is very unpleasant; The peak retention time is greatly affected by temperature, especially in summer, if there is an air-conditioning outlet above the mobile phase bottle, it will often cause the retention time to drift significantly;
[0009] (2) Capillary electrophoresis: as we all know, capillary electrophoresis has poor reproducibility and is not suitable for drug quality control

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
  • A kind of reversed-phase liquid chromatography detects the method for raltitrexed enantiomer
  • A kind of reversed-phase liquid chromatography detects the method for raltitrexed enantiomer
  • A kind of reversed-phase liquid chromatography detects the method for raltitrexed enantiomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The detection of enantiomer in embodiment 1 raltitrexed

[0032] 1. Instruments and reagents

[0033] Shimadzu LC-20A high performance liquid chromatography;

[0034] CPA225D electronic balance (Beijing Sartorius Instrument System Co., Ltd.);

[0035] Chromatographic column: Waters XBridge C18 column;

[0036] The raw material of raltitrexed was purchased from Wuhan Dahua Weiye Pharmaceutical Chemical Co., Ltd., and the reference substance of raltitrexed and enantiomer was purchased from EP;

[0037] Methanol was chromatographically pure, triethanolamine was analytically pure, water was deionized water, and the mobile phase was prepared and filtered through a 0.45 μm membrane.

[0038] 2. Experimental methods and results

[0039] 1. Solution preparation

[0040] Diluent: 42% methanol aqueous solution, add 5mL triethanolamine to 1L methanol aqueous solution.

[0041] Reference substance solution: Accurately weigh approximately 10 mg of raltitrexed and its enantiome...

Embodiment 2

[0065] Example 2 failure case

[0066]The applicant has tried a variety of mobile phases of common composition, such as methanol aqueous solution and acetonitrile aqueous solution of different concentrations, but no obvious effect has been seen. Taking the 42% methanol aqueous solution (compared with Example 1 without adding triethanolamine, and other chromatographic parameters are consistent) as an example, the chromatographic peaks of raltitrexed and enantiomers are always co-eluted together, cannot be separated. Usually, when encountering this situation, technicians will consider whether the proportion of methanol is too high, and try to separate the two by reducing the proportion of methanol. After many attempts by the applicant, when using 36% methanol aqueous solution for elution, although there is a certain sign of separation between the two, the peak spread is very serious, the retention time is also significantly prolonged, and the number of theoretical plates and ta...

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
particle diameteraaaaaaaaaa
wavelengthaaaaaaaaaa
Login to View More

Abstract

The invention discloses a method for detecting Raltitrexed enantiomer with reversed phase liquid chromatography. Octadecyl silane bonded silica gel is taken as a solid phase, a methanol water solution in the volume percentage of 40%-44% is taken as a mobile phase, and 4-6 mL of triethanolamine is added to 1 L of the mobile phase to serve as a chiral selector. With the adoption of the method, Raltitrexed and enantiomer thereof can be separated effectively, and the separation degree is larger than 1.5. The method based on the reversed phase liquid chromatography is mature and universal and does not have the defects of normal phase liquid chromatography and capillary electrophoresis in the prior art.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for detecting enantiomers of raltitrexed by reversed-phase liquid chromatography. Background technique [0002] Raltitrexed, chemical name N-[5-[N-methyl-N-[(2-methyl-3,4-dihydro-4-oxo-6-quinazolinyl)-methyl] Amino]-2-thiophenoyl]-L-glutamic acid, trade name Tomudex, is a specific inhibitor of thymidylate synthase, used for the treatment of advanced colorectal cancer. Clinical trials have shown that this product is less toxic than the conventional first-line treatment drug 5-fluorouracil, has higher activity, and is more convenient to use. It has become the first-line treatment drug for advanced colorectal cancer in Western European countries such as the United Kingdom. [0003] The chemical structural formula of raltitrexed is as follows: [0004] [0005] Raltitrexed raw materials and their preparations often have a certain amount of enantiomers, and the chemical stru...

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 Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 陈云张鑫宇王斌
Owner 南京和曦生物科技有限公司