Intelligent detection method for trichloromethyl carbonate residues in clindamycin hydrochloride

Abstract

The invention relates to the technical field of intelligent measurement and control of trichloromethyl carbonate residues, in particular to an intelligent detection method for trichloromethyl carbonate residues in clindamycin hydrochloride. The method is completed by adopting a gas chromatography-mass spectrometer convenient for automatically leveling a column head of a chromatographic column in a matching manner. The detection method comprises the following steps: 1) preparing a raw material solution of a test sample; 2) preparing a test sample preparation solution; 3) preparing a reference substance solution; and 4) respectively and independently putting the prepared test sample raw material solution, the test sample preparation solution and the reference substance solution into a gas chromatography-mass spectrometer for detection. According to the invention, through the arranged cutting and leveling structure, the chromatographic column head can be automatically cut and leveled when the chromatographic column head of the chromatographic mass spectrometer body is replaced, and compared with manual leveling, the leveling efficiency and the leveling quality are greatly improved.

Description

technical field [0001] The invention relates to the technical field of intelligent measurement and control of trichloromethyl carbonate residues, in particular to an intelligent detection method for trichloromethyl carbonate residues in clindamycin hydrochloride. Background technique [0002] Clindamycin hydrochloride is an antibiotic drug, which is used for most infections caused by sensitive strains such as Streptococcus, Staphylococcus and anaerobic bacteria. The solid reagent trichloromethane carbonate is used in the synthesis process of clindamycin hydrochloride Triphosgene ester (also known as triphosgene), there may be traces of trichloromethyl carbonate residue in the final raw material drug, and trichloromethyl carbonate is stable at room temperature and has strong stability. Only a small amount of decomposition produces trichloromethyl chloroformate and phosgene. Triphosgene is insoluble in water but soluble in ether, tetrahydrofuran, benzene, cyclohexane, chlorofo...

AI Technical Summary

Problems solved by technology

[0004] The chromatographic column on the chromatographic mass spectrometer is a consumable part, which needs to be replaced during detection, and when installing a new chromatographic column, it is usually necessary to manually check whether the column head is flat, and if it is not smooth, it needs to be manually passed through the ceramic. The knife cuts. After cutting, the uneven end is pulled off by manual dialing, and then the cutting surface is checked again to see if it is smooth. If it is flat, it can be installed into the cavity of the chromatographic column. It is difficult to observe the flatness of the stigma manually, and it usually takes a long time to draw a conclusion manually, and it is difficult to level the stigma by manual cutting, and the leveling quality is poor, and it usually requires repeated cutting and leveling to be able to A flat column head is obtained, which greatly reduces the flattening efficiency, and the injection port of the existing chromatographic mass spectrometer is usually exposed outside the box, and the corresponding dust-proof measures are not aligned. Accumulated dust, during each sampling process, the dust will enter the detection part with the push of the sampling needle, which will easily affect the detection results and reduce the detection accuracy

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