Unlock instant, AI-driven research and patent intelligence for your innovation.

Methods for separating and measuring 1-fluoronaphthalene and related impurities

A technology for fluoronaphthalene and impurities, which is applied in the field of separation and determination of 1-fluoronaphthalene and related impurities, can solve the problems of inaccurate determination of 1-fluoronaphthalene and related impurities, and ineffective separation of impurities, achieving high accuracy and effective Separation, the effect of improving accuracy

Active Publication Date: 2018-12-28
HUBEI HONGYUAN PHARMA
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since 1-fluoronaphthalene, naphthalene, and 2-fluoronaphthalene have similar boiling points (1-fluoronaphthalene 215°C, naphthalene 218°C, 2-fluoronaphthalene 226°C), conventional gas chromatography cannot effectively separate impurities, let alone accurately determine 1 - Content of fluoronaphthalene and related impurities

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
  • Methods for separating and measuring 1-fluoronaphthalene and related impurities
  • Methods for separating and measuring 1-fluoronaphthalene and related impurities
  • Methods for separating and measuring 1-fluoronaphthalene and related impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 11

[0082] The positioning of embodiment 11-fluoronaphthalene and related impurity naphthalene, 2-fluoronaphthalene and 1-chloronaphthalene

[0083] (1) Preparation of positioning solutions for 1-fluoronaphthalene and related impurities naphthalene, 2-fluoronaphthalene and 1-chloronaphthalene

[0084] Preparation of 1-fluoronaphthalene positioning solution: Accurately weigh 30.79 mg of 1-fluoronaphthalene reference substance, place it in a 50mL volumetric flask, add diluent to dissolve and dilute to the mark, shake well to obtain 1-fluoronaphthalene positioning solution, concentration It is 0.6152mg / mL.

[0085] Preparation of naphthalene positioning solution: Accurately weigh 30.12 mg of naphthalene reference substance, place in a 50 mL volumetric flask, add diluent to dissolve and dilute to the mark, shake well, and obtain naphthalene positioning solution with a concentration of 0.6108 mg / mL.

[0086] Preparation of 2-fluoronaphthalene positioning solution: Accurately weigh 30....

Embodiment 21

[0090] The separation of embodiment 21-fluoronaphthalene and related impurity naphthalene, 2-fluoronaphthalene and 1-chloronaphthalene

[0091] (1) Preparation of mixed solution of 1-fluoronaphthalene and related impurities naphthalene, 2-fluoronaphthalene and 1-chloronaphthalene

[0092] Preparation of naphthalene stock solution: same as the naphthalene positioning solution in Example 1, the concentration is 0.6108mg / mL.

[0093] Preparation of 2-fluoronaphthalene stock solution: Precisely pipette 1.0mL of the 2-fluoronaphthalene positioning solution in Example 1, place it in a 20mL volumetric flask, add diluent to dissolve and dilute to the mark, shake well to obtain 2-fluoronaphthalene Stock solution, the concentration is 0.0304mg / mL.

[0094] Preparation of 1-chloronaphthalene stock solution: same as the 1-chloronaphthalene positioning solution in Example 1, the concentration is 0.6162 mg / mL.

[0095] Preparation of mixed solution: Accurately weigh 30.24mg of 1-fluoronap...

Embodiment 3

[0097] The separation and detection of 1-fluoronaphthalene and related impurity naphthalene, 2-fluoronaphthalene and 1-chloronaphthalene in the test sample of embodiment 3

[0098] Preparation of the test solution: Accurately weigh about 30 mg of the test product, place it in a 50 mL volumetric flask, add a diluent to dissolve and dilute to the mark, and shake well to obtain the test solution with a concentration of 0.6 mg / mL.

[0099] Self-contrast solution preparation: Precisely pipette 1.0mL of the test solution, place it in a 100mL volumetric flask, add diluent to dissolve and dilute to the mark, and shake well to obtain the test solution with a concentration of 0.006mg / mL.

[0100] Get above-mentioned need testing solution and self contrast solution respectively and analyze according to above-mentioned chromatographic condition, record chromatogram as follows: Figure 7 , Figure 8 As shown, the content of 1-fluoronaphthalene and related impurities in the test product is...

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
wavelengthaaaaaaaaaa
concentrationaaaaaaaaaa
Login to View More

Abstract

The invention belongs to the field of analytic chemistry, and particularly relates to methods for separating and measuring 1-fluoronaphthalene and related impurities. According to the separation method, separation is carried out by using octadecylsilane chemically bonded silica as a stationary phase and using acetonitrile and alkali buffer salt solution as mobile phases, and aqueous solution of acetonitrile is used as a diluent; and the method can implement effective separation of 1-fluoronaphthalene and related impurities. The measurement method adopts high performance liquid chromatography and comprises the steps of: taking a test sample to add a diluent to prepare test sample solution; then taking the test sample solution to add the diluent to dilute according to a certain times to obtain self-contrasted solution; respectively taking the test sample solution and the self-contrasted solution to carry out analysis by adopting the stationary phase and the mobile phases; recording a chromatogram; and calculating content of 1-fluoronaphthalene and related impurities in the test sample according to a self-contrasted method added with a correction factor. Not only can effective separation of 1-fluoronaphthalene and related impurities be implemented, but also the content of 1-fluoronaphthalene and related impurities can be accurately measured, and the separation method and the measurement method are simple and convenient to operate, rapid and high in accuracy.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a method for separating and measuring 1-fluoronaphthalene and related impurities. Background technique [0002] Duloxetine Hydrochloride (Duloxetine Hydrochloride) chemical name is (S)-(+)-N-methyl-3-(1-naphthyloxy)-3-(2-thienyl)propylamine hydrochloride, is a An antidepressant with dual inhibitory effects on the reabsorption of serotonin and norepinephrine, has the characteristics of good chemical stability, safety and effectiveness, few side effects, and low affinity to other nervous systems, and has become the preferred choice in modern clinical research Antidepressants. [0003] Dapoxetine Hydrochloride (Dapoxetine Hydrochloride) chemical name is (S)-(+)-N,N-dimethyl-1-phenyl-3-(1-naphthyloxy)-propylamine hydrochloride, is a Selective serotonin reuptake inhibitors have the characteristics of fast drug effect, short half-life and low side effects, and become the first on-...

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
Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88G01N2030/884G01N2030/8872G01N2030/065
Inventor 肖伟平蔡泽宇王正雄孟宪华胡伟张阳玲孙向阳纪瑞雪
Owner HUBEI HONGYUAN PHARMA