Detection method for determining chloroacetic acid residues in cinepazide maleate intermediate through HPLC method

Abstract

The invention belongs to the technical field of chloroacetic acid detection, and particularly relates to a detection method for determining chloroacetic acid residues in a cinepazide maleate intermediate through an HPLC method. The method comprises the following steps: (1) preparing a reference solution; (2) preparing a sample solution; (3) performing sample injection detection in HPLC, wherein chromatographic detection conditions are as follows: chromatographic column: a silane bonding silica gel column is a high performance liquid chromatography column of a stationary phase, a mobile phase A: water-methanol-trifluoroacetic acid in a volume ratio of 96: 4: 0.1, a mobile phase B: methanol, the flow velocity of the mobile phase being 0.6-1ml / min, the column temperature of the chromatographic column is 33-37 DEG C, the sample size is 20mu l, and the detection wavelength is 212-216nm; and (4) calculating the content of chloroacetic acid: calculating the content of chloroacetic acid according to the peak area through an external standard method. The method has the beneficial effects that the chloroacetic acid is detected by using the HPLC method, the operation is simple, and the problems in the prior art are solved.

Description

technical field [0001] The invention belongs to the technical field of chloroacetic acid detection, in particular to a method for detecting residual chloroacetic acid in an intermediate of cinepazide maleate by HPLC. Background technique [0002] Cinepazide maleate chemical name: (E)-1-{4-[(3',4',5'-trimethoxycinnamoyl)]1-1piperazine}acetylpyrrolidine maleic butene Diacid salts, which can be used to treat cerebrovascular diseases and cardiovascular diseases, often contain chloroacetic acid as an impurity, which is one of the genotoxic impurities. Genotoxic impurities refer to positions that can directly or indirectly damage DNA, cause gene mutation or have a tendency to cause cancer. Chloroacetic acid is one of the raw materials used in the synthesis process of the cinepazide maleate intermediate, and the present invention further ensures the safety of the drug by strictly controlling the content of chloroacetic acid in the cinepazide maleate intermediate . [0003] In re...

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Problems solved by technology

The derivatization method is also commonly used in the detection of halogenated hydrocarbons, but its operation is relatively cumbersome

[0004] Chinese patent CN 110988151A pointed out in the background technology that due to the low boiling point of chloroacetic acid, small molecular weight, weak ultraviolet absorption and small proportion of hydrocarbons, it is difficult to use the commonly used detection methods GC-FID, HPLC-UV, GC-MS detection test Low concentration limit of chloroacetic acid in samples

However, this detection method has high requirements for instruments, and requires the combination of liquid chromatography and mass spectrometry, and the operation process is cumbersome and complicated.

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