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Method for detecting residual solvent in antiangitide by utilizing gas chromatographic method and application

A gas chromatography and residual solvent technology, applied in the field of drug detection, can solve problems such as solvent residues, affecting the safety of the final product, and achieve the effects of stable quality, great practical significance and academic value, and strong specificity.

Pending Publication Date: 2021-11-05
BEIJING SAISHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When the synthesis process adopts the solid-term synthesis method, Fmoc-Asp(Otbu)-wang resin is used as the starting material, and then dipeptide to octadecapeptide are sequentially connected with protected amino acids. During this process, there may be solvent residue problems. Thus affecting the use safety of the final product, so it is necessary to detect and monitor its quality

Method used

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  • Method for detecting residual solvent in antiangitide by utilizing gas chromatographic method and application
  • Method for detecting residual solvent in antiangitide by utilizing gas chromatographic method and application
  • Method for detecting residual solvent in antiangitide by utilizing gas chromatographic method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] This embodiment provides a gas chromatography analysis and detection method for residual DMSO in antiangitide, the specific steps are as follows:

[0040] Take the antiangitide sample to be tested, accurately weigh it, add water to dissolve and dilute to make a solution containing about 20 mg of antiangitide in each 1ml, and prepare 2 parts in parallel as the test solution; Take 50 mg of sulfone, dilute it in a 50 mL volumetric flask, adjust the volume to the mark and mix evenly, measure 1 ml, put it in a 10 ml volumetric bottle, add water to dilute to the mark, shake well, and prepare 2 copies in parallel as the control solution.

[0041] Use 6%-cyanopropylphenyl-94% dimethyl polysiloxane capillary column (DB-624, 30m×0.53mm×3μm) as the chromatographic column, the flow rate is 3mL nitrogen per minute, and the gas flow rate is 30ml / min , the flow rate of the assisted gas is 400ml / min. The temperature of the detector is 250°C, the temperature of the injection port is 28...

Embodiment 2 Embodiment 1

[0042] The specificity test of embodiment 2 embodiment 1 method

[0043] (1) Scheme design

[0044] To investigate whether the organic solvents introduced in the production process of antiangitide and the volatile components of the main component interfere with the detection of dimethyl sulfoxide. Test method is the same as embodiment 1.

[0045] Antiangitide production process includes: Wang resin as carrier, Fmoc protected amino acid as raw material, DIC, HOBt as condensation agent and catalyst, DMF, DMSO, DCM as solvent, piperidine / DMF solution as deprotection reagent, anhydrous methanol As a shrinking solvent, solid-phase synthesis was performed to obtain a peptide resin. Cleavage the peptide from the resin with TFA-based lysate, settle the peptide with methyl tert-butyl ether and dry it to obtain the crude peptide. The crude peptide is purified by preparative HPLC with acetonitrile and salt solution as the mobile phase. Refined peptides were obtained by lyophilization....

Embodiment 3

[0068] 1. Quantitation limit and detection limit

[0069] (1) Scheme design

[0070] From the limit concentration control solution, dilute step by step, the concentration when the signal-to-noise ratio is 10:1 is the limit of quantification; the concentration when the signal-to-noise ratio is 3:1 is the limit of detection.

[0071] (2) Experimental method

[0072] Detection limit: take the dimethyl sulfoxide limit concentration solution, dilute it with water step by step to a certain concentration solution, inject samples, and the test method is the same as in Example 1. In the resulting chromatogram, the signal intensity of the main peak and the noise peak should not be less than 3, then the concentration of the solution at this time is the detection limit of the component.

[0073] Quantitative limit: take the limit concentration solution of dimethyl sulfoxide, dilute it into a solution with a certain concentration step by step with water, inject samples, and the test meth...

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Abstract

The invention relates to the technical field of drug detection, and particularly discloses a method for detecting a residual solvent in antiangitide by using a gas chromatographic method and application. According to the method for detecting the residual solvent in antiangitide by utilizing the gas chromatographic method, the residual solvent is dimethyl sulfoxide, a direct sample injection mode is adopted, and a programmed heating mode is as follows: the initial temperature is 50-60 DEG C and is kept for 1-2 minutes; and heating is performed to 210-220 DEG C at the heating rate of 20 DEG C / min, the temperature is kept for 4-6 minutes, and the process is finished after 13-16 minutes. The gas chromatographic detection method is high in sensitivity and good in specificity, stability and accuracy, the quality of antiangitide can be effectively controlled, and the quality of antiangitide is stable, controllable and safe.

Description

technical field [0001] The invention relates to the technical field of drug detection, in particular to a method and application for detecting residual solvents in antiangitide by gas chromatography. Background technique [0002] Antiangitide (HM-3) is a synthetic peptide with integrin affinity and high-efficiency blood vessel inhibitor, which consists of 18 amino acids. It can effectively inhibit the migration of endothelial cells, and can effectively inhibit the proliferation of human non-small cell lung cancer, liver cancer, and gastric cancer. Its biggest feature is remarkable activity, good safety, and is not easy to produce drug resistance (the treatment is aimed at tumor endothelial cells, and endothelial cells are not easy to mutate). When the synthesis process adopts the solid-term synthesis method, Fmoc-Asp(Otbu)-wang resin is used as the starting material, and then dipeptide to octadecapeptide are sequentially connected with protected amino acids. During this pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8818
Inventor 赵佳欣齐硕栾美丽孔双泉宋梦薇
Owner BEIJING SAISHENG PHARMA
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