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Method for concurrently determining butylphthalide and relates substances thereof

A related substance, butylphthalide technology, applied in the field of drug analysis, can solve problems such as separation difficulties, and achieve the effects of good specificity, good accuracy and low cost

Active Publication Date: 2016-11-09
NANJING YOKO PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when this method is applied to the detection of samples containing the above 6 impurities, the separation is difficult

Method used

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  • Method for concurrently determining butylphthalide and relates substances thereof
  • Method for concurrently determining butylphthalide and relates substances thereof
  • Method for concurrently determining butylphthalide and relates substances thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] The determination of embodiment 1 detection wavelength

[0078] Preparation of diluent: Measure 400mL of acetonitrile and 600mL of water, stir and mix evenly, the obtained solution is also a blank solution, use a UV spectrophotometer to measure the maximum absorption wavelength of each impurity and butylphthalide reference substance, see the results in Figure 1-7 .

[0079] Scan the spectrum by full wavelength Figure 1-7 , Butylphthalide and its various impurities have relatively large absorption at a wavelength of about 226-230nm, and the preferred wavelength is 228nm, so the detection wavelength is determined to be 228nm.

Embodiment 2

[0080] Embodiment 2 system suitability experiment

[0081] Chromatographic conditions: Shimadzu LC-20A or Dionne U3000 high-performance liquid chromatography system and workstation; automatic sample injection; Welch Ultimate XB C 18 (4.6mm×250mm, 5μm) is a separation column; UV detection wavelength: 228nm; mobile phase: 0.2% disodium hydrogen phosphate solution and acetonitrile (gradient elution); column temperature 25°C, injection volume 20μL, flow rate 1.0mL / min;

[0082] gradient program

[0083]

[0084]

[0085] Preparation of positioning solution:

[0086] Weigh about 25mg of phthalic acid, weigh it accurately, put it in a 50mL measuring bottle, add diluent to dissolve and dilute to the mark, shake well, weigh 200μL of the solution, put it in a 20mL volumetric flask, and obtain a concentration of 5μg / mL Phthalate positioning solution;

[0087] Weigh about 25 mg of Intermediate I, weigh it accurately, put it in a 50 mL volumetric flask, add diluent to dissolve ...

Embodiment 3

[0107] Embodiment 3 specificity test

[0108] Investigate the degradation research of butylphthalide bulk drug, the forced degradation conditions include acid, alkali, oxidation, high temperature and light, the specific degradation test is as follows:

[0109] Undamaged sample: Take about 25mg of butylphthalide raw material, weigh it accurately, put it in a 50mL measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and you get it.

[0110] Acid destruction: Take about 25mg of butylphthalide raw material, weigh it accurately, put it in a 50mL measuring bottle, add 2mL of 1mol / L hydrochloric acid solution to destroy it for 6 hours; add an equal amount of 1mol / L sodium hydroxide solution to neutralize, add dilution Dissolve the agent and dilute to the mark, shake well, and you have it.

[0111] Alkali destruction: Take about 25mg of butylphthalide raw material, weigh it accurately, put it in a 50mL measuring bottle, add 2mL of 1mol / L sodium hydroxide solu...

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Abstract

The present invention provides an analysis detection method for concurrently determining butylphthalide and relates substances thereof. According to the analysis detection method, through a high performance liquid chromatograph, an octadecylsilane bonded silica gel is adopted as a filler, a 0.2% phosphate buffer liquid and acetonitrile are adopted as a mobile phase to carry out gradient elution, and the detection wavelength is 226-230 nm. According to the present invention, the analysis method has characteristics of good specificity, high sensitivity, good accuracy and good durability, wherein the separation degrees of each absorption peak are more than or equal to 7.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for separating and measuring butylphthalide and its related substances by high performance liquid chromatography. Background technique [0002] Butylphthalide is the earliest cerebrovascular drug developed by the Chinese Academy of Sciences, and it is used to treat mild and moderate acute ischemic stroke. Its structural formula is: [0003] [0004] The related substances are mainly the starting materials, intermediates, polymers, side reaction products brought in during the production process, and degradation products during the storage process. Based on considerations of safety and actual production conditions, a certain amount of harmless or low-toxic related substances may be allowed to be contained, but related substances that are relatively toxic, harmful to human health, ineffective or affect drug stability must be strictly controlled. Therefore, the detection of ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 杨谋伟周莹朱素华薛峪泉张峰
Owner NANJING YOKO PHARMA
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