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A kind of method for ion-pair chromatography to measure related substances in 6-bromohexyltrimethylammonium bromide

A technology of bromohexyltrimethylammonium bromide and ion-pair chromatography, which is applied in the field of ion chromatography, can solve problems such as long analysis time, complicated operation, and inability to measure, and achieve good reproducibility, simple method, and low test cost. low effect

Active Publication Date: 2022-06-28
QINGDAO SHENGHAN CHROMATOGRAPH TECH CO LTD
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  • 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

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  • A kind of method for ion-pair chromatography to measure related substances in 6-bromohexyltrimethylammonium bromide
  • A kind of method for ion-pair chromatography to measure related substances in 6-bromohexyltrimethylammonium bromide
  • A kind of method for ion-pair chromatography to measure related substances in 6-bromohexyltrimethylammonium bromide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0046] The ion chromatograph is used for detection, and the specific steps include:

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

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

[0049] Precisely weigh 101.01 mg of hexamethylammonium bromide standard product (purity 99%) into a 100 mL volumetric flask, dissolve in ultrapure water, make up to the mark, shake well, and prepare a 1000 mg / L hexamethylammonium bromide standard stock solution.

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

[0051] Precisely ...

Embodiment 2

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

[0064] The ion chromatograph is used for detection, and the specific steps include:

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

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

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

[0068] Precisely pipette 0.1mL, 0.5mL, 1.0mL, 2.5mL, 5.0mL of 6-bromohexyltrimethylammonium bromide standard stock solution into a 10mL volumetric flask, dissolve with ultrapure water, make up to the mark, shake to obtain a series of 6-bromohexyltrimethylammonium bromide standard solutions with concentrations of 10mg / L, 50mg / L, 100mg / L, 250mg / L and 500mg / L respectively.

[0069...

Embodiment 3

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

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

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

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

[0085] The adopted chromatographic conditions are the same as those in Example 1, except that the gradient elution is performed, and the gradient program is shown in Table 2.

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

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Abstract

The invention discloses a method for determining related substances in 6-bromohexyltrimethylammonium bromide by ion-pair chromatography, comprising the following steps: (1) preparation of standard solution: weighing 6-bromohexyltrimethylammonium bromide Ammonium and hexamethylammonium bromide standard substance were dissolved in ultrapure water and settled to a certain volume, and shaken up to obtain the standard solution of the two; (2) preparation of sample solution: weigh 6-bromohexyltrimethyl The ammonium bromide sample is dissolved in ultrapure water to a certain volume, shakes up to obtain the sample solution; (3) determination of the standard product and sample solution: according to certain chromatographic conditions, utilize ion chromatography to standard product and sample solution Sample injection analysis, record peak area simultaneously; (4) calculate the content of analyte: calculate the content of 6-bromohexyltrimethylammonium bromide and hexamethylammonium bromide according to external standard method. Compared with mass spectrometry, the method of the present invention has low test cost and no complicated pretreatment. The 6-bromohexyltrimethylammonium bromide sample only needs to be dissolved in water, and can be directly injected for analysis. The method is simple and easy.

Description

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

Claims

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Application Information

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Patent Type & Authority Patents(China)
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
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