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

A detection method and technology for tert-butylamine are applied in the field of content detection of tert-butylamine, sec-butylamine and triethylamine in artificial bear bile powder, which can solve the problem of reducing detection limit and quantification limit, tailing of three amine peak shapes, and poor separation effect. and other problems, to achieve the effect of lowering the detection limit and quantification limit, lowering the detection cost, and improving the sensitivity

CN114235997AActive Publication Date: 2022-03-25中山百盛生物技术有限公司
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2022-03-25

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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.
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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...

Examples

Embodiment

[0044] The present invention employs a gas chromatographic analysis method, and the content of tert-butamine, sec-butamine, and triethylamine in artificial xero flour is detected, and the detection steps are as follows:

[0045] Step 1, select the chromatographic condition

[0046] Columns: Phenomenex ZB-1 capillary column (or a fairly capillary column), the column specification is 60m × 0.53 mm, 3.0 um;

[0047] Carrying gas: nitrogen;

[0048] Car gas flow rate: 3.0ml / min;

[0049] The inlet temperature is 200 ° C;

[0050] Distortion ratio: 20: 1;

[0051] Detector: hydrogen flame ionization detector;

[0052] The detector temperature is 220 ° C;

[0053] Top spoof injection: 5ml;

[0054] The heating program is: 10 min from 50 ° C, raised at a rate of 1 ° C per minute to 70 ° C, reserved 5 min, and then raised at a rate of 40 ° C per minute to 220 ° C, retained 10 min;

[0055] Top air temperature setting: box temperature 80 ° C, flow path temperature 85 ° C, transmission li...