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

Method for determining related substances in 6-bromohexyltrimethyl ammonium bromide by ion pair chromatography

A technology of bromohexyltrimethylammonium bromide and ion pair chromatography, applied in the field of ion chromatography, can solve the problems of long analysis time, high cost, complicated operation and the like, and achieves good reproducibility, high precision, and simple and easy method. row effect

Active Publication Date: 2021-07-13
QINGDAO SHENGHAN CHROMATOGRAPH TECH CO LTD
View PDF7 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ultraviolet spectrophotometry and high performance liquid chromatography can measure quaternary ammonium salts with ultraviolet absorption, but cannot measure saturated alkyl quaternary ammonium salts such as 6-bromohexyltrimethylammonium bromide and hexamethylammonium bromide; liquid chromatography- Mass spectrometry and gas chromatography-mass spectrometry can determine saturated alkyl quaternary ammonium salts, but the operation is complicated, the analysis time is long, and the cost is expensive

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
  • Method for determining related substances in 6-bromohexyltrimethyl ammonium bromide by ion pair chromatography
  • Method for determining related substances in 6-bromohexyltrimethyl ammonium bromide by ion pair chromatography
  • Method for determining related substances in 6-bromohexyltrimethyl ammonium bromide by ion pair chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The eluent conditions of embodiment 1 6-bromohexyltrimethylammonium bromide and hexamethylamine bromide

[0046] Using ion chromatography for detection, the specific steps include:

[0047] (1) prepare 6-bromohexyltrimethylammonium bromide and hexamethylammonium bromide standard stock solution

[0048] Accurately weigh 102.04mg of 6-bromohexyltrimethylammonium bromide standard (purity 98%) in a 100mL volumetric flask, dissolve with ultrapure water, set the volume to the mark, shake well, and make 1000mg / L 6-bromohexyl Hexyltrimethylammonium bromide standard stock solution.

[0049] Accurately weigh 101.01mg of hexamethylammonium bromide standard substance (purity 99%) in a 100mL volumetric flask, dissolve with ultrapure water, set the volume to the mark, shake well, and make 1000mg / L hexamethylammonium bromide standard stock solution.

[0050] (2) preparation of 6-bromohexyltrimethylammonium bromide and hexamethylammonium bromide mixed standard solution

[0051] Accu...

Embodiment 2

[0063] Example 2 Linear parameters and detection limits of 6-bromohexyltrimethylammonium bromide and hexamethylamine bromide

[0064] Using ion chromatography for detection, the specific steps include:

[0065] (1) prepare 6-bromohexyltrimethylammonium bromide and hexamethylammonium bromide standard stock solution

[0066] The preparation of standard stock solution of 6-bromohexyltrimethylammonium bromide and hexamethylammonium bromide is the same as in Example 1.

[0067] (2) Preparation of 6-bromohexyltrimethylammonium bromide and hexamethylammonium bromide standard solution series

[0068] Accurately pipette 0.1mL, 0.5mL, 1.0mL, 2.5mL, 5.0mL 6-bromohexyltrimethylammonium bromide standard stock solution into a 10mL volumetric flask, dissolve with ultrapure water, dilute to the mark, shake Uniformly, the obtained concentration is respectively 10mg / L, 50mg / L, 100mg / L, 250mg / L, 6-bromohexyltrimethylammonium bromide standard solution series of 500mg / L.

[0069] Accurately pip...

Embodiment 3

[0081] Embodiment 3 A kind of method that utilizes ion-pair chromatography to detect the purity of 6-bromohexyltrimethylammonium bromide adopts ion chromatography to detect, and external standard method single-point quantitative analysis, and the specific steps include:

[0082] (1) prepare 6-bromohexyltrimethylammonium bromide reference substance and sample solution

[0083] Weigh about 50mg of 6-bromohexyltrimethylammonium bromide standard (purity 98%) and 1#, 2#, samples in 100mL volumetric flask, dissolve with ultrapure water, set the volume to the mark, shake well, That is, standard and sample solutions were obtained.

[0084] (2) Setting of ion-pair chromatographic conditions

[0085] The chromatographic conditions used are as in Example 1, except that gradient elution is used, and the gradient program is as in Table 2.

[0086](3) According to the above chromatographic conditions, after the baseline of the instrument is balanced, take 6-bromohexyltrimethylammonium bro...

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

PropertyMeasurementUnit
The inside diameter ofaaaaaaaaaa
Lengthaaaaaaaaaa
Login to View More

Abstract

The invention discloses a method for determining related substances in 6-bromohexyltrimethyl ammonium bromide by ion pair chromatography, which comprises the following steps: (1) preparation of standard solutions: weighing standard substances of 6-bromohexyltrimethyl ammonium bromide and hexamethylamine bromide, respectively dissolving the standard substances with ultrapure water to a certain volume, and uniformly shaking the solution to obtain the standard substance solutions of the standard substances of the two components; (2) preparation of a sample solution: weighing a 6-bromohexyltrimethyl ammonium bromide sample, dissolving the sample with ultrapure water to a certain volume, and uniformly shaking the liquid to obtain the sample solution; (3) determination of a standard substance and a sample solution: carrying out sample introduction analysis on the standard substance and the sample solution by using an ion chromatograph according to certain chromatographic conditions, and recording peak areas at the same time; and (4) calculating the content of the substance to be detected: calculating the content of 6-bromohexyltrimethyl ammonium bromide and hexamethylamine bromide according to an external standard method. Compared with mass spectrometry, the method has the advantages that the test cost is low, complicated pretreatment is avoided, a 6-bromohexyltrimethylammonium bromide sample can be directly injected and analyzed after being dissolved by adding water, and the method is simple and easy to implement.

Description

technical field [0001] The invention relates to the field of ion chromatography, and relates to a quantitative analysis method for related substances in 6-bromohexyltrimethylammonium bromide, in particular to an ion pair chromatography for determining related substances in 6-bromohexyltrimethylammonium bromide Methods. Background technique [0002] 6-Bromohexyltrimethylammonium bromide, CAS number is 191086-27-8, the structural formula is as follows, it is easily soluble in water and deliquescent. [0003] [0004] The preparation process of 6-bromohexyltrimethylammonium bromide is often accompanied by the generation of impurity hexamethylammonium bromide, the CAS number is 55-97-0, and the structural formula is as follows. Both have similar structural formulas, both have quaternary ammonium salt groups, and are excellent pharmaceutical intermediates and pharmaceutical products. 6-Bromohexyltrimethylammonium bromide is an important intermediate in the synthesis of the d...

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): G01N30/96
CPCG01N30/96
Inventor 郑秀瑾张锦梅张苗苗王晓娇王永文
Owner QINGDAO SHENGHAN CHROMATOGRAPH TECH 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