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Method for detecting 3-amino-2-azepanone through high performance liquid chromatography

A technology of high performance liquid chromatography and caprolactam, which is applied in the field of high performance liquid chromatography to detect 3-amino-2-caprolactam, can solve problems such as narrow application range, and achieve good specificity, good linear fitting and good stability Effect

Active Publication Date: 2015-11-25
SICHUAN KELUN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the scope of application of the invention is narrow

Method used

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  • Method for detecting 3-amino-2-azepanone through high performance liquid chromatography
  • Method for detecting 3-amino-2-azepanone through high performance liquid chromatography
  • Method for detecting 3-amino-2-azepanone through high performance liquid chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1: a kind of method that high performance liquid chromatography detects 3-amino-2-caprolactam, it comprises the following steps:

[0037] S1. Mobile phase preparation:

[0038] (1) Weigh 5.44 g of potassium dihydrogen phosphate, add water and dilute to 4000 ml to obtain a 0.01mol / L potassium dihydrogen phosphate solution, adjust the pH to 2 with phosphoric acid, and obtain mobile phase A after suction filtration and ultrasound;

[0039] (2) Prepare a solution with a volume ratio of methanol, acetonitrile and water of 1:5:1, shake well to obtain mobile phase B;

[0040] S2. Reference substance solution preparation:

[0041] (1) Weigh 10 mg of 3-amino-2-caprolactam and add it to a 50ml volumetric flask, dissolve it with mobile phase A and adjust the volume to the volumetric line, shake well to obtain 3-amino-2-caprolactam reference substance stock solution;

[0042] (2) Measure 1ml of 3-amino-2-caprolactam reference substance stock solution and add it to a 10...

Embodiment 2

[0045] Embodiment 2: a kind of method that high performance liquid chromatography detects 3-amino-2-caprolactam, it comprises the following steps:

[0046] S1. Mobile phase preparation:

[0047] (1) Weigh potassium dihydrogen phosphate 16.33g, add water and dilute to 4000ml to obtain 0.03mol / L potassium dihydrogen phosphate solution, adjust pH to 2.5 with phosphoric acid, obtain mobile phase A after suction filtration and ultrasonic;

[0048] (2) Prepare methanol, acetonitrile and water with a volume ratio of 2:4:1, shake well to obtain mobile phase B;

[0049] S2. Reference substance solution preparation:

[0050] (1) Weigh 20 mg of 3-amino-2-caprolactam and add it to a 50ml volumetric flask, dissolve it with mobile phase A and adjust the volume to the scale line of the volumetric flask, shake well to obtain 3-amino-2-caprolactam reference substance stock solution;

[0051] (2) Measure 1ml of 3-amino-2-caprolactam reference substance stock solution and add it to a 100ml vol...

Embodiment 3

[0054] Embodiment 3: a kind of method that high performance liquid chromatography detects 3-amino-2-caprolactam, it comprises the following steps:

[0055] S1. Mobile phase preparation:

[0056] (1) Weigh 27.22 g of potassium dihydrogen phosphate, add water and dilute to 4000 ml to obtain a 0.05 mol / L potassium dihydrogen phosphate solution, adjust the pH to 3 with phosphoric acid, obtain mobile phase A after suction filtration and ultrasound;

[0057] (2) Prepare a solution with a volume ratio of methanol, acetonitrile and water of 3:3:1, shake well to obtain mobile phase B;

[0058] S2. Reference substance solution preparation:

[0059] (1) Weigh 15 mg of 3-amino-2-caprolactam and add it to a 50ml volumetric flask, dissolve it with mobile phase A and adjust the volume to the scale line of the volumetric flask, shake well to obtain 3-amino-2-caprolactam reference substance stock solution;

[0060] (2) Measure 1ml of 3-amino-2-caprolactam reference substance stock solution a...

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Abstract

The invention discloses a method for detecting 3-amino-2-azepanone through a high performance liquid chromatography. According to the method, the following chromatographic conditions are adopted: a chromatographic column is an ODS column; a mobile phase A is a 0.01-0.09 mol / L monopotassium phosphate solution; a mobile phase B is a mixed water solution of methanol and acetonitrile in which the volume ratio of methanol, acetonitrile and water is (1-5):(1-5):1; the flow velocity is 0.4-1.2 ml / min; the detection wavelength is 100-300 nm; the column temperature is 20-60 DEG C; the sample size is 5-20 [mu]l. Through adoption of the method, the content of the impurity of 3-amino-2-azepanone degraded by lysine can be accurately measured, and the specificity is good; the quantification limit repeatability is good, the recovery rate is high, and a solution is high in stability; when the column temperature, the detection wavelength and the flow velocity change slightly, the difference between a detected recovery rate of 3-amino-2-azepanone and a result detected at a basic condition is very small, so that the durability of the method is high.

Description

technical field [0001] The invention relates to a method for detecting amino acid injections, in particular to a method for detecting 3-amino-2-caprolactam by high performance liquid chromatography. Background technique [0002] Amino acid is a general term for a class of organic compounds containing amino and carboxyl groups. It is the basic unit of biological functional macromolecular proteins, the basic substance that constitutes protein required for animal nutrition, and an organic compound containing basic amino groups and acidic carboxyl groups. . Amino Acid Injection is a sterilized aqueous solution prepared from 18 kinds of amino acids. It is used for patients with insufficient protein intake, malabsorption and other amino acids that cannot meet the metabolic needs of the body. It is also used to improve the nutritional status of patients after surgery. Intravenous infusion, 250-500ml each time, 35-50ml / kg for children. It has the functions of promoting normal prot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 邓茂林刘文军刘思川谭鸿波葛均友万阳浴聶义朱麟吴小愚王昌斌
Owner SICHUAN KELUN PHARMA CO LTD
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