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Detection method and application of 6-chloromethyl-2-pyridinemethanol

A detection method, the technology of pyridinemethanol, which is applied in the detection field, can solve problems affecting the efficacy of anticancer drugs, etc., and achieve the effects of improved separation effect, easy preparation, and high accuracy

Active Publication Date: 2021-11-26
FOSHAN ENANTIOSIC CORP LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of synthesizing the compound shown in formula (1), the purity of 6-chloromethyl-2-pyridinemethanol will directly affect the purity of the compound shown in formula (1) and the antibody drug conjugate, thereby affecting the anticancer drug Efficacy

Method used

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  • Detection method and application of 6-chloromethyl-2-pyridinemethanol
  • Detection method and application of 6-chloromethyl-2-pyridinemethanol
  • Detection method and application of 6-chloromethyl-2-pyridinemethanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] (1) Set the liquid chromatography conditions:

[0063] Chromatographic column: WondaSil C18 Superb 5um 4.6*250mm(W);

[0064] Injection volume: 20μL;

[0065] Flow rate: 1.0mL / min;

[0066] Column temperature: 25°C;

[0067] Detection wavelength: 269nm;

[0068] Mobile phase A: 0.01% formic acid aqueous solution;

[0069] Mobile phase B: acetonitrile;

[0070] Diluent: the volume ratio of water to acetonitrile is 1:1;

[0071] Detector: UV detector;

[0072] Quantitative method: area normalization method;

[0073] The mobile phase gradient is shown in Table 1;

[0074] Table 1 Mobile phase gradient table

[0075] time (min) Mobile phase A(%) Mobile phase B(%) 0 90 10 3 90 10 13 10 90 23 10 90 24 90 10 30 90 10

[0076] (2) Blank test: Accurately measure 20 μL of the diluent, inject it into a liquid chromatograph for detection, and record the chromatogram A. Blanks must not interfere.

[0077] (3) Preparat...

Embodiment 2

[0094] The second batch of samples to be tested (batch number ILX04-210102) was detected by the same detection method as in Example 1.

[0095] The HPLC chromatogram of the sample to be tested is shown in Figure 5 ,exist Figure 5 Among them, the abscissa is time (Time), and the ordinate is the absorbance value (Absorbance / mAU). Figure 5 The information shown in Table 5 can be known. 6-Chloromethyl-2-pyridinemethanol and its known impurities (methyl 6-chloromethylpyridine-2-carboxylate) and unknown impurities can be effectively separated. The purity of 6-chloromethyl-2-pyridinemethanol in the test sample was 98.43%.

[0096] table 5

[0097]

[0098]

Embodiment 3

[0100] The third batch of samples to be tested (batch number ILX04-210104) was detected by the same detection method as in Example 1.

[0101] The HPLC chromatogram of the sample to be tested is shown in Figure 6 ,exist Figure 6 Among them, the abscissa is time (Time), and the ordinate is the absorbance value (Absorbance / mAU). Figure 6 The information shown in Table 6 can be known. 6-Chloromethyl-2-pyridinemethanol and its known impurities (methyl 6-chloromethylpyridine-2-carboxylate) and unknown impurities can be effectively separated. The purity of 6-chloromethyl-2-pyridinemethanol in the test sample is 99.77%.

[0102] Table 6

[0103]

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Abstract

The invention belongs to the technical field of detection, and discloses a detection method and application of 6-chloromethyl-2-pyridinemethanol. According to the detection method, a formic acid aqueous solution and acetonitrile are used as mobile phases, and liquid chromatography is used for detection. According to the detection method provided by the invention, the formic acid aqueous solution and acetonitrile are used as mobile phases for gradient elution, so that the separation effect can be improved, and the 6-chloromethyl-2-pyridinemethanol can be effectively separated from known impurities and unknown impurities; and the mobile phase does not contain salt and is easy to prepare, balance and wash, so that the analysis time can be shortened, and the detection efficiency can be improved. The detection method is simple, convenient, rapid, high in accuracy and good in repeatability, and industrial production and quality control of the 6-chloromethyl-2-pyridinemethanol are facilitated; the purity and the quality of the antibody drug conjugate are favorably controlled, and deeper quality research work on the antibody drug conjugate is facilitated.

Description

technical field [0001] The invention belongs to the technical field of detection, and in particular relates to a detection method and application of 6-chloromethyl-2-pyridinemethanol. Background technique [0002] Antibody Drug Conjugate (ADC) is a coupling product obtained by coupling a monoclonal antibody with a drug. Cytotoxic drugs are coupled with monoclonal antibodies through chemical bonds, and the antibody can specifically recognize the characteristics of tumor cells, and can "precisely" deliver toxic small molecules to tumor cells, increasing the concentration of drugs in tumor sites while reducing the concentration of normal tissues , organ drug concentration, to achieve high efficiency and low toxicity anti-tumor effect. [0003] Compound shown in formula (1) (wherein R 1 for (CH 2 ) n or PEG), which is an important compound to achieve site-specific coupling modification of biomolecules. When the compound is used to couple biomolecules and modifiers, the acti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/54G01N30/74
CPCG01N30/02G01N30/06G01N30/54G01N30/74
Inventor 卢彪邓伟梁徐亮周炳乾黄晓韵陈昌龙徐剑黄志豪唐道鹏蔡祥
Owner FOSHAN ENANTIOSIC CORP LTD