Detection method for dezocine related substances

A technology for related substances and detection methods, applied in the detection field of dezocine related substances, can solve the problems of tailing, wide peak width, main peak cannot be quickly eluted, etc., and achieves the effect of enhancing elution ability and improving peak shape.

Inactive Publication Date: 2016-10-12
JINAN LIMIN PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

from spectrum picture It can be seen that the number of theoretical plates is low, mainly due to the fact that the main peak cannot be eluted quickly, resulting in a wide peak width and severe tailing, so the detection of related substances needs to be further improved; therefore, it is necessary to develop a more sensitive and durable detection method

Method used

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  • Detection method for dezocine related substances
  • Detection method for dezocine related substances
  • Detection method for dezocine related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1. YBH09172006 detection method test

[0017] Use YBH09172006 (YBH09172006 (Yangzijiang Pharmaceutical Group Co., Ltd. Dezocine Quality Standard) Dezocine raw material testing method for related substances:

[0018] Chromatographic conditions and system adaptability test use octadecylsilane bonded silica gel as filler; use acetonitrile-triethylamine solution [take 1000ml water, add 2.5ml triethylamine, adjust to pH3. 2] (200:800) is the mobile phase; the flow rate is 0.6ml per minute, the detection wavelength is 281nm, and the number of theoretical plates should not be less than 3000 based on the dezocine peak. The resolution of the dezocine peak and adjacent impurity peaks should meet the requirements.

[0019] Determination method Take about 35mg of this product, weigh it accurately, put it in a 25ml measuring bottle, add 5ml of acetonitrile, heat and shake it in a hot water bath to dissolve it, dilute it to the mark with triethylamine solution, shake it w...

Embodiment 2

[0023] Embodiment 2. Adopt the related substance detection method of dezocine raw material of the present invention:

[0024] Chromatographic conditions and system adaptability test use octadecylsilane bonded silica gel as filler; use acetonitrile-triethylamine solution [take 1000ml water, add 5ml triethylamine and 2ml tetrabutylammonium hydroxide aqueous solution, use dilute phosphoric acid (1- 5) Adjust to pH3.2] (200:800) as the mobile phase; the flow rate is 0.6ml per minute, the detection wavelength is 281nm, and the number of theoretical plates should not be less than 3000 based on the dezocine peak. The resolution of the dezocine peak and adjacent impurity peaks should meet the requirements.

[0025] Determination method Take about 35mg of this product, weigh it accurately, put it in a 25ml measuring bottle, add 5ml of acetonitrile, heat and shake it in a hot water bath to dissolve it, dilute it to the mark with triethylamine solution, shake it well, and use it as the t...

Embodiment 3

[0031] Embodiment 3. verification of the present invention's relevant substance analysis method

[0032] 1. Specific test

[0033] (1), separation test

[0034] Carry out a separation test study on the starting materials and main intermediates in the synthesis, as well as the known impurities that may be produced. The experimental results are shown in The following table ,

[0035] surface 4 Experimental results of separation of related substances of dezocine surface

[0036]

[0037]

[0038] According to the above data, in this paper bright color Under the spectral conditions, dezocine can be separated from possible intermediates and known impurities, and the resolutions are all greater than 1.5.

[0039] (2), forced degradation test

[0040] Take an appropriate amount of dezocine samples, and carry out acid, alkali, light, high temperature and oxidative damage respectively to investigate the detection and separation ability of this chromatographic conditio...

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Abstract

The invention provides a detection method for dezocine related substances. Octadecyl silane bonded silica gel is adopted as a chromatographic column of a filling agent, and an acetonitrile-triethylamine solution is adopted as a mobile phase, wherein the acetonitrile-triethylamine solution is obtained by taking 1000 ml of water, adding 5 ml of triethylamine and 2 ml of a tetrabutyl ammonium hydroxide water solution, and adjusting pH to 3.2 through diluted phosphoric acid (1-5), and the ratio of acetonitrile to triethylamine is 200:800; the flow rate is 0.6 ml per min, and the detection wavelength is 281 nanometers. According to the detection method for dezocine related substances, the concentration of buffer salts is increased, elution is enhanced, an ion-pairing agent is added, the peak shape is improved, and the problems that due to the fact that the number of theoretical plates of an original method is small and a main peak cannot be rapidly eluted, the peak width is large and trailing is serious are solved.

Description

technical field [0001] The invention relates to a method for detecting related substances of dezocine, which belongs to the technical field of medicinal chemical analysis. Background technique [0002] Dezocine belongs to a class of (Dezocine) belongs to a typical opioid alkaloid analgesics, developed by the Swedish company Astra. Dezocine is a synthetic mixed opioid receptor agonist-antagonist, which can relieve pain when the steady-state plasma concentration reaches 5-9 μg / L, and its analgesic effect is 5-9 times that of pethidine , comparable to morphine. On the one hand, it fully excites the К receptors to produce definite analgesic effects, and at the same time partially antagonizes the μ receptors, reducing the incidence of respiratory depression and addiction. Produce irritability and anxiety. Therefore, it is included in the category of non-narcotics and is widely used in clinical postoperative analgesia. It is suitable for the treatment of moderate to severe pai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 许祚芝彭丽周春红陈洪生姜洋
Owner JINAN LIMIN PHARMA
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