Method for detecting contents of tert-butylamine, sec-butylamine and triethylamine in artificial bear gall powder

Abstract

The invention discloses a method for detecting the content of tert-butylamine, sec-butylamine and triethylamine in artificial bear gall powder. The method is carried out according to the following steps: 1) selecting chromatographic conditions: a chromatographic column is a phemomenex ZB-1 capillary column (or a capillary column with efficacy equivalent to that of the phemomenex ZB-1 capillary column), and the specification is 60m * 0.53 mm, 3.0 [mu] m; the carrier gas is nitrogen, and the flow velocity is 3.0 ml / min; the temperature of a sample inlet is 200 DEG C; the split ratio is 20: 1; the detector is a hydrogen flame ionization detector; the temperature of the detector is 220 DEG C; the headspace sampling amount is 5ml; the heating procedure comprises the following steps: keeping for 10 minutes from 50 DEG C, raising the temperature to 70 DEG C at the rate of raising 1 DEG C per minute, keeping for 5 minutes, raising the temperature to 220 DEG C at the rate of raising 40 DEG C per minute, and keeping for 10 minutes; the headspace temperature is set as follows: the box body temperature is 80 DEG C, the flow path temperature is 85 DEG C, the transmission line temperature is 90 DEG C, the circulation time is 65 minutes, and the sample preheating time is 60 minutes; 2) preparing a reference substance solution and a to-be-tested sample solution; and 3) carrying out headspace treatment, carrying out chromatographic determination, and calculating the contents of tert-butylamine, sec-butylamine and triethylamine in the artificial bear gall powder sample.

Description

Technical field [0001] The present invention relates to a method for detecting tert-butamine, sec-butamine and triethylamine content in artificial bear bile flour. Background technique [0002] The bear bile powder is a powder product of a bear, a black bear or a brown bear capsule, has an efficacy of heat, flat liver, gallbladder, antispasmodal, and olite. Clinically used in children of children, epilepsy, convulsions, jaundice. The use of artificial synthetic methods to convert a wide range of poultry bile products into an alternative resource artificial bear with natural bear bile powder, which protects both the ecological environment and facilitates promoting the modernization of Chinese medicine technology. [0003] The existing three amine content detection methods in artificial xero flour mainly include the following patents and literature: [0004] 1.202010611542.8: Method for detecting triethylamine in cefotaxime sodium [0005] 2. "Top Air Coride Color Spectroscopy Defi...

AI Technical Summary

Problems solved by technology

Different from the detection of amine content by traditional gas chromatography, the buffer solution described in this method is N,N-dimethylformamide (DMF) and a concentration of 8.0mol / L Tris aqueous solution at a volume ratio of 9:1. The mixed solution can quickly and effectively dissociate various bound amines in the artificial bear bile powder sample, which greatly reduces the detection limit and quantification limit of t-butylamine, sec-butylamine and triethylamine in the sample, and at the same time screens the non-polar The gas chromatographic column packing solves the problems of peak tailing and poor separation effect of the three amines under gas chromatographic conditions

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