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Method for detecting residual solvent in pipericide

A technology of residual solvent and detection method, which is applied in the detection field of residual solvent in palbociclib, can solve the problems of difficult detection of residual solvent in palbociclib, unqualified system applicability, poor solubility of palbociclib, etc., and achieves the solution of sample dissolution. Problem and control solution instability problem, accurate and reliable data, high sensitivity effect

Pending Publication Date: 2021-07-16
SHANDONG BOYUAN PHARM CO LTD
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Problems solved by technology

However, the solubility of palbociclib is particularly poor, and it is not easy to dissolve in organic solvents and water; and using water as a solvent will cause instability of the control solution, resulting in unqualified system applicability, which causes great difficulties in the detection of palbociclib residual solvents. At present, there is no report on the detection method of palbociclib residual solvent

Method used

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  • Method for detecting residual solvent in pipericide
  • Method for detecting residual solvent in pipericide
  • Method for detecting residual solvent in pipericide

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Embodiment

[0028] 1. Instruments and materials

[0029] Instruments: Thermo Fisher trace1300 gas chromatograph, HSS 8650 headspace sampler, XS105DU electronic balance;

[0030] Material: palbociclib (batch number: 03201130GS, 03201201GS, 03201212GS);

[0031] 2. Chromatographic conditions

[0032] Chromatographic column: Agilent DB-624; specification is 30m*0.53mm*3μm;

[0033] Programmed temperature rise: keep at 40°C for 6 minutes, then raise the temperature to 200°C at a rate of 20°C / min;

[0034] Injection port temperature: 200°C;

[0035] Detector: hydrogen flame ionization detector (FID);

[0036] Detector temperature: 250°C;

[0037] Carrier gas: N 2 , the split ratio is 20:1;

[0038] Sampling method: headspace sampling method;

[0039] Equilibration time: 30 minutes;

[0040] Equilibrium temperature: 80°C; transfer line temperature: 90°C; quantitative loop temperature: 100°C.

[0041] 3. Solution preparation

[0042] Blank solution: Accurately measure 1.0ml of N,N dim...

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Abstract

The invention discloses a method for detecting a residual solvent in pipericide. According to the method, N, N-dimethylformamide is added for hydrotropy so that the pipericide can be dissolved in water, phosphoric acid is added for dispersion, the stability of a contrast solution is improved, and the problem of solution preparation is solved; and Agilent DB-624 is used as a chromatographic column, a gas chromatography external standard method is adopted for detection, and the accuracy and reliability of a result are ensured by adopting chromatographic conditions such as headspace sampling and temperature programming. The method can be used for simultaneously determining the amount of seven residual solvents, namely acetone, ethyl acetate, n-butyl alcohol, n-heptane, anisole, tetrahydrofuran and methylbenzene, in the pipericil raw material medicine, and has the characteristics of simplicity in operation, accuracy, reliability and the like.

Description

technical field [0001] The invention relates to a method for detecting residual solvents in palbociclib, belonging to the field of drug analysis and detection. Background technique [0002] Palbociclib, also known as palbociclib, is a CDK4 / 6 inhibitor developed by Pfizer. In 2015, it was approved by the FDA through the accelerated approval channel for the treatment of HER2-breast cancer. Well, compared with letrozole, it can double the progression-free survival of breast cancer; the incidence of adverse reactions is low; capsules can be taken orally, and compared with injections, they are safer, easy for patients to take, and improve patient compliance; Strong targeting, due to the increased level of Cyclin D in tumor cells, it can increase the sensitivity of cells to drugs, etc., and has attracted much attention. [0003] Various solvents such as acetone, ethyl acetate, n-butanol, n-heptane, anisole, tetrahydrofuran and toluene are used in the current synthesis process of ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/047
Inventor 陈凤牛庆娟徐汝来郑潇华
Owner SHANDONG BOYUAN PHARM CO LTD
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