Method for detecting residual quantity of morpholine in bulk drug and application of method

A detection method and a technology of raw materials, which are applied in the directions of measuring devices, material separation, and analysis of materials, etc., can solve the problems of detection of morpholine content tailing and low sensitivity, and achieve the effects of easy purchase, high sensitivity, and strong specificity

Pending Publication Date: 2021-06-04
上海金不换兰考制药有限公司
View PDF6 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to: provide a kind of high-sensitivity detection method of morpholine residue,...

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 detecting residual quantity of morpholine in bulk drug and application of method
  • Method for detecting residual quantity of morpholine in bulk drug and application of method
  • Method for detecting residual quantity of morpholine in bulk drug and application of method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Determination of UV wavelength of morpholine derivatives:

[0045] Instruments and conditions: Shimadzu LC-20A liquid chromatograph (DAD detector), ZORBAX SB-C18 column, 250mm×4.6mm, 5μm, column temperature 30°C, flow rate 1.0ml per minute, injection The volume is 10 μl, the mobile phase A is water, and the mobile phase B is acetonitrile.

[0046] Using gradient elution, the elution program is shown in Table 1:

[0047] time / min Mobile phase A / % Mobile phase B / % 0-15 55 45 15-22 45 55 22-30 55 45

[0048] The specific implementation steps are as follows:

[0049] ①Preparation of derivatization reagent: just before use, weigh 158mg of 2,4-dinitrofluorobenzene, put it in a 10ml measuring bottle, dissolve it with methanol ultrasonically and dilute to the mark, shake well to get it;

[0050] ②Preparation of 2mg / ml sodium hydroxide / methanol solution: Weigh 0.1g of sodium hydroxide, put it in a 50ml volumetric flask, add methanol to ultr...

Embodiment 2

[0057] Investigation of different diluents:

[0058] Instruments and conditions: use Agilent 1260II liquid chromatograph, chromatographic column: Agilent EC-C18, 150mm×4.6mm, 4μm, detection wavelength is 374nm, column temperature is 30°C, flow rate is 1.0ml per minute, injection volume is 10μl , mobile phase A was 0.1% phosphoric acid solution, and mobile phase B was acetonitrile.

[0059] The gradient elution program is shown in Table 2.

[0060] time / min Mobile phase A / % Mobile phase B / % 0-10 60 40 10-11 45 55 11-15 25 75 15-25 60 40

[0061] The derivatization conditions are shown in Table 3.

[0062] Thinner Amount of derivatization reagent / ml Reaction temperature / ℃ Reaction time / min Acid Binder methanol, ethanol 1 60 30 sodium hydroxide

[0063] The specific implementation steps are with reference to embodiment 1, the results are as attached image 3 As shown, the derivatization reaction can be co...

Embodiment 3

[0065] Investigation of different acid-binding agents:

[0066] Apparatus and conditions: with embodiment 2.

[0067] The derivatization conditions are shown in Table 4.

[0068] Acid Binder Amount of derivatization reagent / ml Reaction temperature / ℃ Reaction time / min Thinner Sodium Hydroxide, Triethylamine 1ml 60℃ 30 minutes Methanol

[0069] The results are attached Figure 4 As shown, the two different acid-binding agents of sodium hydroxide and triethylamine can all react completely.

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 discloses a method for detecting the residual quantity of morpholine in a bulk drug and application of the method, and relates to the technical field of medicine analysis and detection. The bulk drug is moroxydine or moroxydine hydrochloride. The detection method detects the residual quantity of morpholine in the bulk drug through pre-column derivatization and high performance liquid chromatography. The method comprises the following steps: dissolving a bulk drug sample by use of a diluent to obtain a diluted solution, adding an acid-binding agent and a derivatization reagent into the diluted solution, carrying out a derivatization reaction to obtain the morpholine derivative, analyzing the content of the morpholine derivative by using a high performance liquid chromatograph, and carrying out simple conversion to obtain the content of morpholine in a sample. The method is high in sensitivity and accurate in detection data. The problems of serious trailing and low sensitivity when the morpholine content is detected by the existing gas chromatography are solved.

Description

technical field [0001] The invention relates to the technical field of drug analysis and detection, in particular to a method for detecting residual morpholine in raw materials. Background technique [0002] Morpholine, also known as morphine, is a colorless oily liquid at room temperature. It is mainly used to make rubber vulcanization accelerators. It can also be used for the synthesis of active agents, textile printing and dyeing auxiliaries, medicines and pesticides. It can also be used as Metal corrosion inhibitors and antirust agents are also solvents for dyes, resins, waxes, shellac, etc., and are usually used in the pharmaceutical field to produce morpholine guanidine, morpholine guanidine hydrochloride, morpholine guanidine hydrochloride is a commonly used broad-spectrum anti Virus medicine can be used to treat diseases such as influenza, mumps, viral bronchitis, chickenpox, herpes, and epidemic pink eye. [0003] On October 27, 2017, in the preliminary compilation...

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): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/067
Inventor 祖晓燕闫亚星康建党刘胜杰李尚刘建辉
Owner 上海金不换兰考制药有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap