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UPLC-MS/MS (Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry) method for rapidly detecting fruquintinib in rat plasma

A fruquintinib and plasma technology, applied in the field of UPLC-MS/MS for rapid detection of fruquintinib in rat plasma, can solve problems such as inability to repeat

Inactive Publication Date: 2019-08-27
THE FIRST AFFILIATED HOSPITAL OF WENZHOU MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, other laboratories cannot replicate these two assays

Method used

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  • UPLC-MS/MS (Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry) method for rapidly detecting fruquintinib in rat plasma
  • UPLC-MS/MS (Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry) method for rapidly detecting fruquintinib in rat plasma
  • UPLC-MS/MS (Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry) method for rapidly detecting fruquintinib in rat plasma

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1) Specimen collection: Fruquintinib was dissolved in a 0.4% sodium carboxymethyl cellulose solution at a concentration of 0.8 mg / kg and administered orally to a group of young male rats. For h, 1h, 1.5h, 2h, 3h, 4h, 6h, 9h, 12h, 24h and 48h, blood samples of 0.25ml were collected from the tail vein of rats, respectively. After centrifugation at 3000 rpm for 4min, 90µL of supernatant plasma was taken and stored in -20 ℃ refrigerator for testing.

[0020] 2) Plasma sample processing: 0.08 mL of plasma sample was directly precipitated with 180 µL of acetonitrile, in which the internal standard substance diazepam was directly dissolved in acetonitrile, and the diazepam concentration was 90 ng / mL; after vortexing for 0.8 min, 12000 Centrifuge at rpm for 8 min, and take 5 µL of the supernatant for mass spectrometry detection.

[0021] 3) Mass spectrometry detection: Detection by Acquity UPLC BEH C18 chromatographic column, the column temperature is 39 °C, the mobile phase c...

Embodiment 2

[0024] 1) Specimen collection: Fruquintinib was dissolved in a 0.5% sodium carboxymethyl cellulose solution at a concentration of 1.0 mg / kg and administered orally to a group of young male rats. After h, 1h, 1.5h, 2h, 3h, 4h, 6h, 9h, 12h, 24h and 48h, 0.3ml blood samples were collected from the tail vein of rats, respectively. After centrifugation at 1000 rpm for 5min, 100µL of supernatant plasma was taken and stored in -20℃ refrigerator for testing;

[0025] 2) Plasma sample processing: 0.1 mL of plasma sample was directly precipitated with 200 µL of acetonitrile. The internal standard substance, diazepam, was directly dissolved in acetonitrile, and the concentration of diazepam was 100 ng / mL; Centrifuge for 10 min, and take 6 µL of the supernatant for mass spectrometry detection;

[0026] 3) Mass spectrometry detection: detected by Acquity UPLC BEH C18 chromatographic column, the column temperature was 40 °C, the mobile phase consisting of acetonitrile and 0.1% formic acid ...

Embodiment 3

[0029] 1) Specimen collection: Fruquintinib was dissolved in a 0.6% sodium carboxymethyl cellulose solution at a concentration of 1.2 mg / kg and administered orally to a group of young male rats. After h, 1h, 1.5h, 2h, 3h, 4h, 6h, 9h, 12h, 24h and 48h, blood samples of 0.35ml were collected from the tail vein of rats, respectively. After centrifugation at 5000 rpm for 6min, 110µL of supernatant plasma was taken and stored in -25℃ refrigerator for testing;

[0030] 2) Plasma sample processing: 0.11mL plasma sample was directly precipitated with 220µL acetonitrile, in which the internal standard substance diazepam was directly dissolved in acetonitrile, and the diazepam concentration was 110 ng / mL; after vortexing for 1.2min, 14000 Centrifuge at rpm for 12 min, and take 7 µL of the supernatant for mass spectrometry detection;

[0031]3) Mass spectrometry detection: detection by Acquity UPLC BEH C18 chromatographic column, the column temperature is 41 °C, the mobile phase consist...

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Abstract

The invention discloses a UPLC-MS / MS (Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry) method for rapidly detecting fruquintinib in rat plasma, and belongs to the technical fieldof pharmacokinetics. The method comprises the following steps: 1) collecting a specimen; 2) treating a plasma sample; 3) performing mass spectrometric detection; and 4) reading and recording data. Through adoption of the UPLC-MS / MS method for rapidly detecting fruquintinib in rat plasma, the concentration of the fruquintinib in the rat plasma can be detected rapidly, easily and accurately. Through the method, the pharmacokinetics of the fruquintinib in the rat plasma can be investigated; the blood concentration and clinical pharmacokinetics of the fruquintinib in human plasma can be monitored; and the preclinical application and post-clinical application of the fruquintinib are facilitated.

Description

technical field [0001] The invention belongs to the technical field of pharmacokinetics, in particular to a UPLC-MS / MS method for rapidly detecting fruquintinib in rat plasma. Background technique [0002] Fruquintinib is the first anticancer drug independently invented by Chinese, researched by Chinese doctors, and developed by Chinese companies. It can bring hope to patients with metastatic colorectal cancer who have received at least two chemotherapy regimens but still have disease progression. , which has been confirmed in clinical studies to significantly prolong the survival of patients. So far, there are only two reported methods for detecting fruquintinib concentration in plasma, but these two methods are too simple and do not describe the plasma extraction process, chromatographic conditions, method parameters, etc. Therefore, other laboratories cannot replicate these two assays. SUMMARY OF THE INVENTION [0003] In view of the above-mentioned problems in the pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 徐仁爱谢赛丽郑明华
Owner THE FIRST AFFILIATED HOSPITAL OF WENZHOU MEDICAL UNIV
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