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Method for detecting contents of D-ribose and 5-deoxy-D-ribofuranose in capecitabine intermediate

A technology of ribofuranose and capecitabine, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effects of improving drug safety, good separation effect, and high sensitivity

Pending Publication Date: 2022-03-25
SHANDONG BOYUAN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, after retrieval, there is currently no method for detecting the content of D-ribose and 5-deoxy-D-ribose in 1,2,3-tri-O-acetyl-5-deoxy-β-D-ribose to report

Method used

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  • Method for detecting contents of D-ribose and 5-deoxy-D-ribofuranose in capecitabine intermediate
  • Method for detecting contents of D-ribose and 5-deoxy-D-ribofuranose in capecitabine intermediate
  • Method for detecting contents of D-ribose and 5-deoxy-D-ribofuranose in capecitabine intermediate

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Embodiment 1

[0029] 1 Instruments and materials

[0030] 1.1 Instrument: triple quadrupole liquid mass spectrometer (Thermo Ultimate 3000-TSQ Quantiva);

[0031] 1.2 Reagents: Acetonitrile is chromatographic grade, and water is ultrapure water.

[0032] 2 Methods and Results

[0033] 2.1 Chromatography and mass spectrometry conditions

[0034] Chromatographic column: Acclaim RSLC120 C18 (2.0×100mm, 2.2μm), flow rate: 0.2ml / min, column temperature: 20-50℃, injection volume: 2μl, mobile phase: acetonitrile-water (35:65).

[0035] Mass spectrometry conditions are: ion source: electrospray ionization source (ESI), negative ion mode: selective quantitative (SRM) mode, spray voltage (IS): 2800V; evaporation temperature 200 ° C; sheath gas (Gas1): 35Arb; auxiliary gas (Gas2 ): 7Arb;

[0036] Ion transfer tube temperature (Ion Transfer Tube Temp): 325°C; ion pairs used for quantitative analysis are m / z184.962→m / z35.167 (D-ribose) and m / z168.912→m / z35.250 (5-deoxy-D-ribofuranose), the mass spe...

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Abstract

The invention discloses a method for detecting the content of D-ribose and 5-deoxy-D-ribofuranose in a capecitabine intermediate. According to the method, an LC-MS detection method is adopted, Acclaim RSL C120C18 is used as a chromatographic column, acetonitrile-water (35: 65) is used as a mobile phase, D-ribose and 5-deoxy-D-ribofuranose in 1, 2, 3-tri-O-acetyl-5-deoxy-beta-D-ribofuranose are detected, and the two impurities are matched with 1, 2, 3, 3-tri-O-acetyl-5-deoxy-beta-D-ribofuranose in terms of content of 1, 2, 3-tri-O-acetyl-5-deoxy-beta-D-ribofuranose and 5-deoxy-D-ribofuranose. According to the present invention, the 3, 3-tri-O-acetyl-5-deoxy-beta-D-ribofuranose can be well separated (the RT of the D-ribose is 1.39 min; the RT of the 5-deoxy-D-ribofuranose is 1.45 min; the peak RT of 1, 2, 3-tri-O-acetyl-5-deoxy-beta-D-ribofuranose is 4.33 min, and the method has the advantages of being high in specificity, rapid, sensitive, accurate and the like.

Description

technical field [0001] The invention relates to impurities D-ribose and 5-deoxy-D-ribose furanose in a capecitabine intermediate (1,2,3-tri-O-acetyl-5-deoxy-β-D-ribofuranose) detection method. Background technique [0002] Capecitabine (Capecitabine) is the first oral fluoropyrimidine carbamate antineoplastic drug on the market, and it is a new targeted drug for the treatment of breast cancer and colorectal cancer. The drug was developed by Roche with the trade name "Xeloda". It was approved for marketing in the United States in April 1998, and was subsequently launched in Switzerland and other countries. In November 1999, it began to conduct clinical trials for registration in China. The clinical trials were conducted by five national anti-tumor drug clinical trial research centers in Beijing, Shanghai, Guangzhou and other places, and it was listed under the trade name "Xeloda". Capecitabine is rapidly absorbed through the intestinal mucosa after oral administration, and ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N30/74G01N2030/065Y02P20/55
Inventor 闫玲玲张秀云钱振英
Owner SHANDONG BOYUAN PHARM CO LTD
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