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A kind of assay method of residual solvent in decitabine intermediate

A residual solvent and determination method technology, applied in the field of pharmaceutical analysis, can solve the problems of poor stability of raw glycosides, solvent peak interference, low recovery rate, etc., and achieve the effects of good method recovery rate, high accuracy and high recovery rate.

Active Publication Date: 2018-03-20
HANGZHOU HUADONG MEDICINE GRP PHARMA RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It solves the problems that the raw material glycoside for the preparation of decitabine has poor stability, is not easy to dissolve, the recovery rate of the existing detection method is seriously low when detecting pyridine in the glycoside, and it is easily interfered by solvent peaks

Method used

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  • A kind of assay method of residual solvent in decitabine intermediate
  • A kind of assay method of residual solvent in decitabine intermediate
  • A kind of assay method of residual solvent in decitabine intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Chromatographic conditions:

[0073] Column temperature: programmed temperature rise: the initial temperature was 40°C and kept for 8 minutes, then the temperature was raised to 220°C at a rate of 20°C per minute and kept for 19 minutes.

[0074] Injection port temperature: 250°C;

[0075] Flame ionization detector temperature: 300°C;

[0076] Carrier gas: nitrogen;

[0077] Carrier gas flow rate: 3.0ml / min;

[0078] Split ratio: 20:1.

[0079] 1. Detection

[0080] A. Preparation of the test solution:

[0081] First, prepare a mixed solution of methanol-N-methylpyrrolidone-triethylamine in a volume ratio of 47.5:47.5:5 and set aside;

[0082] Again, accurately weigh 1.0 g of glucoside, put it in a 10 ml volumetric flask, dissolve and dilute it into a 0.1 g / ml solution with the prepared mixed solution of methanol-N-methylpyrrolidone-triethylamine, mix well, and set aside;

[0083] B. Preparation of reference substance solution: Accurately weigh 200 μg of pyridine...

Embodiment 2

[0127] The difference between this embodiment and embodiment 1 is that the volume ratio of methanol-N-methylpyrrolidone-triethylamine is

[0128] 45:45:10.

[0129] Chromatographic conditions:

[0130] Column temperature: programmed temperature rise: the initial temperature was 40°C and kept for 8 minutes, then the temperature was raised to 220°C at a rate of 20°C per minute and kept for 19 minutes.

[0131] Injection port temperature: 230°C;

[0132] Flame ionization detector temperature: 280°C;

[0133] Carrier gas: nitrogen;

[0134] Carrier gas flow rate: 2.0ml / min;

[0135] Split ratio: 10:1.

[0136] According to the above conditions, three batches of test solution were detected, and no pyridine peak was detected in the chromatograms. After calculation, the residual amount of pyridine in the glycoside was 0%.

Embodiment 3

[0138] The difference between this embodiment and embodiment 1 is that the volume ratio of methanol-N-methylpyrrolidone-triethylamine is

[0139] 48:48:4.

[0140] Chromatographic conditions:

[0141] Column temperature: programmed temperature rise: the initial temperature was 40°C and kept for 8 minutes, then the temperature was raised to 220°C at a rate of 20°C per minute and kept for 19 minutes.

[0142] Injection port temperature: 270°C;

[0143] Flame ionization detector temperature: 320°C;

[0144] Carrier gas: nitrogen;

[0145] Carrier gas flow rate: 4.0ml / min;

[0146] Split ratio: 30:1.

[0147] According to the above conditions, three batches of test solution were detected, and no pyridine peak was detected in the chromatograms. After calculation, the residual amount of pyridine in the glycoside was 0%.

[0148] In addition, other residual solvents in the test product can also be detected according to the methods provided in the above-mentioned Examples 1 to 3...

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Abstract

The invention discloses a method for measuring the content of pyridine in decitabine impurities. A methyl alcohol-N-methyl-pyrrolidone-triethylamine mixed solution is used as a solvent, and a direct injection gas chromatographic method is adopted for measurement. The problems that decitabine raw material glucoside stability is poor, dissolution is not easily achieved, the recycling rate of an existing detection method is seriously low and interference is likely to be caused by solvent peaks are solved. According to the method, it is tested that a blank solvent has no interference peaks for residual solvent pyridine measurement, the precision is good, the relative standard deviation (RSD) is only 0.46%, the reproducibility is good, the linear relation is good, the average recycling rate is high, and pyridine possibly remaining in glucoside can be accurately and quantitatively detected. Effective quality control is achieved for preparing second-class solvent pyridine in the decitabine raw material glucoside, and the quality of decitabine and drug use safety are ensured at the same time.

Description

technical field [0001] The invention belongs to the technical field of medical analysis, in particular to a method for determining the content of pyridine in decitabine impurities. Background technique [0002] Decitabine, known as Decitabine in English, is a cytosine nucleoside drug developed by SuperGen and marketed by MGIPHARMA. It was approved in the United States in May 2006 for the treatment of myelodysplastic syndrome. [0003] Glycoside is the raw material used in the docking reaction step when decitabine is synthesized, and the structural formula of the glycoside is as follows: [0004] [0005] The second-class solvent pyridine is used in the process of synthesizing glycosides. Pyridine is a health hazard: it is strongly irritating; it can anesthetize the central nervous system; it has an irritating effect on the eyes and upper respiratory tract; after inhalation of high concentrations, mild cases may have a feeling of euphoria or suffocation , followed by depr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor 雍春
Owner HANGZHOU HUADONG MEDICINE GRP PHARMA RES INST
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