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Method for detecting N-dimethyl nitrosamine in ranitidine

A technology of dimethylnitrosamine and ratintinib, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of expensive equipment and unstable detection data

Pending Publication Date: 2020-05-08
SUZHOU HOMESUN PHARMA
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  • Claims
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Problems solved by technology

[0004] The detection method published by the FDA for detecting NDMA in ranitidine hydrochloride requires the use of LC-MSMS. This equipment is very expensive, and most pharmaceutical companies do not have this equipment, and this equipment and the detection method published by the FDA are being used to detect ranitidine The detection data of NDMA in Tidine is unstable, and this method may be more suitable for detecting NDMA in Ranitidine Hydrochloride, so it is urgent to develop a simple and stable method for detecting NDMA in Ranitidine

Method used

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  • Method for detecting N-dimethyl nitrosamine in ranitidine
  • Method for detecting N-dimethyl nitrosamine in ranitidine
  • Method for detecting N-dimethyl nitrosamine in ranitidine

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Embodiment 1

[0029] (1) Solution preparation:

[0030] Diluent: Accurately measure 425ml of concentrated hydrochloric acid, put it in a 1000ml volumetric flask, dilute with water to the mark, shake well, and get ready.

[0031] Blank solution: pipette 10ml of diluent and 10ml of dichloromethane into a 100ml round bottom flask, shake at high speed for 5 minutes, transfer all the liquid to a 100ml separating funnel, let stand to separate the layers, and collect the organic layer (lower layer), namely have to.

[0032] Reference substance stock solution: take 20 mg of NDMA reference substance, weigh it accurately, put it in a 100ml volumetric flask, dissolve it with methanol and dilute to the mark, shake well, then precisely pipette 1ml into a 50ml volumetric flask, dilute to the mark with methanol, shake Mix well, then pipette 2ml precisely, put it in a 25ml volumetric flask, dilute to the mark with methanol, shake well, and set aside.

[0033] Reference substance solution: Precisely pipet...

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Abstract

The invention discloses a method for detecting N-dimethyl nitrosamine in ranitidine. The method is carried out by adopting a high performance liquid chromatography and comprises the following steps: taking concentrated hydrochloric acid diluted to 42.5% of the original concentration as a diluent; mixing a methanol solution of an NDMA reference substance with the concentration of 3.2 * 10 <-4> mg / mL with a diluent and dichloromethane with the volume being 10 times that of the NDMA reference substance, standing for layering, and taking an organic layer as a reference substance solution; dissolving an NDMA test sample into an isopyknic mixed solution of a diluent and dichloromethane at the concentration of 100mg / mL, then standing for layering, and taking an organic layer as a test sample solution; injecting the reference substance solution and the test solution into a high performance liquid chromatograph, carrying out gradient elution by using the mobile phase A and the mobile phase B asmobile phases, and recording chromatograms; wherein the chromatographic column is ODS-3V C18, 250 mm * 4.6 mm, 5 [mu]m; wherein the mobile phase A is water-methanol in a volume ratio of 65: 35, and the mobile phase B is water-methanol in a volume ratio of 25: 75. Compared with a method published by FDA, the method is more stable in detection data.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a method for detecting N-dimethylnitrosamine in ratintinib. Background technique [0002] N-Nitrosodimethylamine is referred to as NDMA for short, and its English name is N-Nitrosodimethylamine, which is considered to be a suspected carcinogenic chemical substance. FDA issued a related warning letter on September 13, 2019, warning that NDMA was detected in ranitidine hydrochloride, and then FDA announced the method for detecting NDMA in ranitidine hydrochloride and announced the The limit for NDMA is 0.32ppm. [0003] There are two main sources of NDMA in ranitidine hydrochloride, one is brought in during the early synthesis, and the other is self-degradation. The self-degrading NDMA is due to the structure of the compound that determines that the impurity will be produced during storage, which is basically uncontrollable. Therefore, if you want to control the content of ND...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 樊超田会明
Owner SUZHOU HOMESUN PHARMA
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