Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

High-performance liquid chromatography analytical method for N1,N1-diisopropyl ethylenediamine

A high-performance liquid chromatography, propyl ethylenediamine technology, applied in the field of high-performance liquid chromatography analysis, can solve the problems of poor method reproducibility, poor accuracy and sensitivity, poor accuracy, etc., and achieves accurate method, high sensitivity, good reproducibility

Pending Publication Date: 2015-11-04
HANGZHOU XINBOSI BIOMEDICAL CO LTD
View PDF5 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Currently detected N 1 ,N 1 -The analytical methods of diisopropylethylenediamine include: acid-base titration, chromatography, due to N 1 ,N 1 -Diisopropylethylenediamine is an organic amine, which can be determined by acid direct titration 1 ,N 1 - the content of diisopropylethylenediamine, but if it is necessary to determine N in other samples 1 ,N 1 -residue of diisopropylethylenediamine, the accuracy and sensitivity of the method are relatively poor; due to N 1 ,N 1 -Diisopropylethylenediamine has a small boiling point and can be determined by gas chromatography 1 ,N 1 -Residue of diisopropylethylenediamine, but if there are insoluble substances in the sample, it will easily adsorb the sample, and the accuracy is relatively poor; N 1 ,N 1 - Diisopropylethylenediamine itself has no UV-absorbing groups, so it cannot be detected by conventional liquid-phase methods. If unconventional detectors such as differential detectors are used, the method will have poor reproducibility
In addition, there are no relevant reports on liquid phase analysis, which limits the choice of methods for analysts.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • High-performance liquid chromatography analytical method for N1,N1-diisopropyl ethylenediamine
  • High-performance liquid chromatography analytical method for N1,N1-diisopropyl ethylenediamine
  • High-performance liquid chromatography analytical method for N1,N1-diisopropyl ethylenediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1: N 1 ,N 1 - Diisopropylethylenediamine standard curve drawing

[0046] Take N 1 ,N 1- About 20mg of diisopropylethylenediamine, accurately weighed, put in a 25ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well; accurately measure 1ml of the above solution, put it in a 20ml measuring bottle, and dilute with diluent To the mark, as N1,N1-diisopropylethylenediamine standard stock solution; take the appropriate amount of the above-mentioned standard stock solution precisely, and quantitatively dilute with the above-mentioned diluent to make each 1ml contain about 0.4μg, 0.8μg, 4μg, 8μg, 12μg linear solution;

[0047] Measure 1ml of each of the above linear solutions, put them in 5ml measuring bottles, add 2ml of 0.05mol / L sodium carbonate solution, add 1ml of derivatization reagent, place in a 50oC water bath for 30 minutes, cool, and then dilute to the mark with diluent. Precisely measure 10 μl each of the derivatized linear solu...

Embodiment 2

[0048] Example 2: N 1 ,N 1 - Determination of detection limit and limit of quantification of diisopropylethylenediamine.

[0049] Take N 1 ,N 1 - About 20mg of diisopropylethylenediamine, accurately weighed, put in a 25ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well; accurately measure 1ml of the above solution, put it in a 20ml measuring bottle, and dilute with diluent to scale, as N 1 ,N 1 -Diisopropylethylenediamine limit stock solution; measure the above limit stock solution, dilute step by step with diluent to obtain limit solution, measure each 1ml of the above limit solution, put in 5ml measuring bottle respectively, add 0.05mol / Add 2ml of L sodium carbonate solution, add 1ml of derivatization reagent 2,4-dinitrofluorophenylacetonitrile solution (1%, V / V), place in 50oC water bath for 30 minutes, cool, and then dilute to the mark with diluent. Precisely measure 10 μl each of the derivatized limiting solutions, inject them into a li...

Embodiment 3

[0050] Example 3: N 1 ,N 1 - Determination of recovery rate of diisopropylethylenediamine

[0051] Take N 1 ,N 1 - About 20mg of diisopropylethylenediamine, accurately weighed, put in a 25ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well; accurately measure 1ml of the above solution, put it in a 100ml measuring bottle, dilute with diluent to scale, as N 1 ,N 1 -Diisopropylethylenediamine standard solution.

[0052] Take an appropriate amount of the test product (equivalent to 16 mg of acotiamide hydrochloride), accurately weigh it, put it in 10 20ml measuring bottles, add diluent to dissolve, and add 1ml N to 3 of them. 1 ,N 1 - Diisopropylethylenediamine standard solution, 3 of which added 2ml N 1 ,N 1 -Diisopropylethylenediamine standard solution, 3 of which were added with 4ml N1,N1-diisopropylethylenediamine standard solution, and the last one was not added with N 1 ,N 1 -Diisopropylethylenediamine standard solution, then dilute to ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a high-performance liquid chromatography analytical method for N1,N1-diisopropyl ethylenediamine. The analytical method is characterized by including the following steps that 1, N1,N1-diisopropyl ethylenediamine standard solutions of different concentrations are prepared, excess 2,4-dinitrofluorobenzene is added into the standard solutions for a derivatization reaction, after the reaction is completed, high-performance liquid chromatography analysis is carried out on reaction solutions, and the DNB-N1,N1-diisopropyl ethylenediamine peak area corresponds to a N1,N1-diisopropyl ethylenediamine concentration drawing standard curve; 2, a test sample is prepared into a solution, excess 2,4-dinitrofluorobenzene is added into the solution to react, after the reaction is completed, high-performance liquid chromatography analysis is carried out on the reaction solution, and the content of N1,N1-diisopropyl ethylenediamine in the test sample is calculated. The analytical method is accurate, high in repeatability and sensitivity, and capable of being used for detecting N1,N1-diisopropyl ethylenediamine in the producing and placing processes of acotiamide hydrochloride and tablets thereof and detecting N1,N1-diisopropyl ethylenediamine in other samples.

Description

technical field [0001] The present invention relates to a kind of N 1 ,N 1 - High performance liquid chromatography analysis method of diisopropylethylenediamine. technical background [0002] N 1 ,N 1 -Diisopropylethylenediamine is a relatively important chemical raw material and an excellent organic solvent. It is also commonly used in organic synthesis and is an important intermediate for the synthesis of Acotiamide hydrochloride trihydrate. [0003] Currently detected N 1 ,N 1 -The analytical methods of diisopropylethylenediamine include: acid-base titration, chromatography, due to N 1 ,N 1 -Diisopropylethylenediamine is an organic amine, which can be determined by acid direct titration 1 ,N 1 - the content of diisopropylethylenediamine, but if it is necessary to determine N in other samples 1 ,N 1 -residue of diisopropylethylenediamine, the accuracy and sensitivity of the method are relatively poor; due to N 1 ,N 1 -Diisopropylethylenediamine has a small bo...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): G01N30/02
Inventor 杜焕达周卫枫郑春燕
Owner HANGZHOU XINBOSI BIOMEDICAL CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com