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Method for detecting alpha-phenylethylamine impurity in ubenimex bulk drug

A detection method, the technology of Ubenex, is applied in measurement devices, material separation, and analysis of materials, etc., which can solve the problems of poor stability, high reactivity of genotoxic impurities, and low concentration limit, achieving good repeatability and reducing correlation. Side effects, the effect of improving product quality

Active Publication Date: 2021-10-01
深圳万乐药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This concentration limit is extremely low, and genotoxic impurities are highly reactive and poorly stable, so the analysis of such trace impurities in pharmaceuticals is extremely challenging and requires analytical methods with high sensitivity and specificity
There is no literature report on the detection and analysis method of α-phenylethylamine impurity in Ubenimex API. In order to ensure the drug safety of Ubenimex, it is necessary to develop a detection method with high sensitivity and good specificity for Ubenimex Content control of α-phenylethylamine impurity in raw materials of the company

Method used

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  • Method for detecting alpha-phenylethylamine impurity in ubenimex bulk drug
  • Method for detecting alpha-phenylethylamine impurity in ubenimex bulk drug
  • Method for detecting alpha-phenylethylamine impurity in ubenimex bulk drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1 Determination of Ubenimex Samples

[0028] Instrument: Agilent7890B-5977 gas chromatography mass spectrometry

[0029] Reagents: 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU, chromatographically pure), acetonitrile (chromatographically pure)

[0030] Sample: Ubenimex (Shenzhen Wanle Pharmaceutical Co., Ltd.), α-phenylethylamine (1-PEA, Shenzhen Lijing Biotechnology Co., Ltd., standard product with a purity of 99%)

[0031] Solvent: Acetonitrile:DBU(99:1);

[0032] Test solution: Weigh 30mg of ubenimex sample, put it in a 10ml measuring bottle, dissolve it with a solvent and set the volume to the mark, shake well for testing;

[0033] 1-PEA stock solution 1 (1.644mg / ml): Weigh 16.95mg of 1-PEA standard substance, put it in a 10ml measuring bottle, dissolve it with a solvent and set the volume to the mark, and set aside;

[0034] 1-PEA stock solution 2 (15μg / ml): Accurately pipette 0.91ml of stock solution 1, put it in a 10ml measuring bottle, dissolve it with a s...

Embodiment 2

[0045] Embodiment 2 method verification experiment

[0046] Instrument: Agilent7890B-5977 GC / MS

[0047] Reagent: 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU), acetonitrile (chromatographically pure)

[0048] Sample: Ubenimex (Shenzhen Wanle Pharmaceutical Co., Ltd.), α-phenylethylamine (1-PEA, Shenzhen Lijing Biotechnology Co., Ltd., standard product with a purity of 99%)

[0049] Chromatographic conditions:

[0050] Capillary column: CP Volamine, 30m×0.32mm, 5μm; Injection port temperature: 265°C; Injection method: Split injection, split ratio: 5:1; Constant flow mode, flow rate: 2ml / min; Carrier gas: Helium Gas (He); oven temperature: 50°C (maintain for 2min) -10°C / min (heating) -265°C (maintain for 10min); injection volume: 1μl; auxiliary heating zone: 265°C.

[0051] Mass Spectrometry Conditions:

[0052] Solvent delay: 12min; acquisition mode: SIM mode; selected ion parameters (mass number m / z, residence time ms) (106.00,50), (79.00,50), (120.00,50); trace ion detection ...

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Abstract

The invention provides a method for detecting a genotoxic impurity alpha-phenylethylamine in an ubenimex bulk drug, the method is high in detection sensitivity, the detection limit concentration is about 0.015 [mu]g / ml (5ppm), and the quantitation limit concentration is about 0.045 [mu]g / ml (15ppm) which is far lower than the limit concentration 0.15 [mu]g / ml (50ppm) of alpha-phenylethylamine; the method has the advantages of good detection specificity, good repeatability, and accurate and credible detection method, can realize effective control of the genotoxic alpha-phenylethylamine in the ubenimex bulk drug, can reduce the related side effects of medication of a preparation product prepared from the ubenimex bulk drug, and can improve the product quality.

Description

technical field [0001] The invention relates to the field of drug analysis, in particular to a method for detecting α-phenethylamine impurities in ubenimex raw materials. Background technique [0002] Ubenimex (Ubenimex; Bestatin) is a low-molecular-weight dipeptide compound isolated from the culture medium of Streptomyces olivine reticulum, which has the ability to inhibit tumor cell surface aminopeptidase B, N and leucine aminopeptide Enzyme action, inducing tumor cell apoptosis, promoting host cell immune function, and enhancing anti-cancer effect. It was launched in Japan in 1987. Ubenimex is often used in combination with other chemotherapy drugs in the treatment of acute myeloid leukemia, chronic myelogenous leukemia, lung squamous cell carcinoma, malignant melanoma, gastric tumor, etc.; combined with radiotherapy, it is used for nasopharyngeal carcinoma It is also used for the treatment of tumor diseases such as tumors, and it is also used for those with low immune f...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/8634G01N30/06Y02A50/30
Inventor 钟剑吴子强刘东华陈博翟丽平罗唐
Owner 深圳万乐药业有限公司