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A kind of uplc-ms/ms method for detecting p-aminophenols

A technology for p-aminophenol and aminophenol, applied in the field of analytical chemistry, can solve problems such as inability to separate 4-aminophenol, affect detection accuracy, and inability to achieve, and achieve the effects of improving retention time, easy control, and easy operation.

Active Publication Date: 2021-09-21
SHANGHAI SCIENPHARM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Zhang Liqing et al. mentioned in the article "Reversed Phase High Performance Liquid Chromatography Simultaneously Determination of the Content of 5 Components including Paracetamol" in "Analytical Chemistry", Volume 31, Issue 1, January 2003, that the separation of paracetamol was carried out by liquid phase detection. Aminophenol, chlorpheniramine, caffeine, guaiacol glyceryl ether and p-aminophenol are five substances, but this liquid phase method cannot separate 4-amino-3-fluorophenol and 4-aminophenol, and the detection limit Unable to meet the requirement that genotoxic impurities 4-amino-3-fluorophenol and 4-aminophenol need to be controlled below 9ppm
[0004] Moreover, the retention of 4-amino-3-fluorophenol and 4-aminophenol compounds is weak, and it is easy to produce solvent effect and cause peak bifurcation, thus affecting the accuracy of detection

Method used

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  • A kind of uplc-ms/ms method for detecting p-aminophenols
  • A kind of uplc-ms/ms method for detecting p-aminophenols
  • A kind of uplc-ms/ms method for detecting p-aminophenols

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Embodiment 1

[0059] Embodiment 1, the present invention detects the UPLC-MS / MS method of p-aminophenol impurities

[0060] Chromatographic column: Platinum C18-EPS (150mm×2.1mm, 3.0μm)

[0061] Mobile phase A: water-formic acid (volume ratio 100:0.1)

[0062] Mobile phase B: acetonitrile-methanol (volume ratio 90:10)

[0063] Flow rate: 0.3ml / min

[0064] Column temperature: 35°C

[0065] Autosampler temperature: 5°C

[0066] Injection volume: 2μl

[0067] Elution procedure:

[0068]

[0069] Detector: Mass spectrometer detector

[0070] Ion source: atmospheric pressure electrospray ion source (ESI)

[0071] Mass Spectrometry Parameters:

[0072] Drying gas temperature: 300°C

[0073] Drying gas flow rate: 8L / min

[0074] Sheath gas temperature: 300°C

[0075] Sheath gas flow rate: 11L / min

[0076] Atomizing gas pressure: 45psi

[0077] Capillary voltage: 4000V

[0078] Nozzle voltage: 500V

[0079] MRM mode positive ion mode Delta EMV(+): 400

[0080] 0~4min, to MS; 4mi...

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Abstract

The invention provides a method for detecting p-aminophenols by UPLC-MS / MS; comprising the following steps: a, determining UPLC-MS / MS conditions; b, adopting ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS / MS) detects respectively reference substance solution, need testing solution; c, obtain the impurity content in the sample with peak area calculation by external standard method. The present invention provides a new detection method for detecting p-aminophenol substances, each object to be tested has no interference with each other, has high sensitivity, and can realize accurate detection of 4-amino-3-fluorophenol and 4-aminophenol at the same time , providing an effective detection method for monitoring the content of p-aminophenols.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for detecting p-aminophenols by UPLC-MS / MS. Background technique [0002] 4-[4-({[4-Chloro-3-(trifluoromethyl)phenyl]carbamoyl}amino)-3-fluorophenoxy]-N-methylpyridine-2-carboxamide monohydrate The drug is a novel oral multikinase inhibitor for the treatment of patients with metastatic colorectal cancer (CRC), gastrointestinal stromal tumor (GIST) and hepatocellular carcinoma (HCC). The drug has been approved for use in more than 90 countries and regions including the United States, the European Union, and Japan, and was approved for marketing by the CFDA on March 24, 2017, for the treatment of patients with metastatic colorectal cancer and gastrointestinal stromal tumors. The maximum daily dose of the drug is 160mg, and the genotoxic impurities 4-amino-3-fluorophenol and 4-aminophenol need to be controlled below 9ppm. [0003] In "Analytical Chemistry",...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 李惠姜春阳谢军马迪周小群许全胜彭典金
Owner SHANGHAI SCIENPHARM CO LTD
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