Simultaneous determination of sunitinib and its active metabolite in plasma by high performance liquid chromatography-tandem mass spectrometry
10.13699/j.cnki.1001-6821.2015.23.023
- VernacularTitle:HPLC－MS／MS法同时测定人血浆中舒尼替尼及其活性代谢产物 SU12662的浓度
- Author:
Yuan-Yuan ZHANG
1
;
Guang-Tao HAO
;
Rui-Hua DONG
;
Xue-Yi CHEN
;
Long-Mei CHENG
;
Ze-Yuan LIU
;
Heng-Yan QU
Author Information
1. 安徽医科大学 解放军307临床学院
- Keywords:
high performance liquid chromatography tandem mass spectrometry;
sunitinib;
N -desethyl sunitinib;
plasma concentration
- From:
The Chinese Journal of Clinical Pharmacology
2015;(23):2348-2351
- CountryChina
- Language:Chinese
-
Abstract:
Objective To establish a high performance liquid chroma-tography-tandam mass spectrometry ( HPLC-MS/MS) method for de-termining the concentration of sunitinib and N -desethyl sunitinib (SU12662) in human plasma.Methods Sunitinib, SU12662 and in-ternal standard sunitinib -D10 were extracted from plasma with one -step protein precipitation and the stereoselective analysis of sunitinib and SU12662 was achieved on an Agilent ZORBAX Extend C18 (2.1 mm ×75 mm ×3.5 μm) with gradient elution by a mobile phase consisting of wa-ter containing 0.1%formic acid and 95%acetonitrile.Electrospray ioni-zation source was applied, and multiple reaction monitoring mode was operated in the positive mode with the monitor ions at m/z 399.3→326.1 for sunitinib, m/z 371.3→283.1 for SU12662 and 409.3→326.2 for sunitinib-D10.Results The calibration curve for plasma sunitinib was linear in the range of 0.5-200 ng? mL-1 ( r=0.998 7) , the lower limi-tation of quantification was 0.5 ng? mL-1 , while the accuracy was ranged from 0.57% to 2.87%, the average recovery rate was ranged from 92.75%to 98.62%,and intra-and inter-day RSD were ranged from 0.91%to 1.92%and 5.40%to 7.87%, respectively.The calibration curve for plasma SU12662 was linear in the range of 0.25 -100 ng? mL-1 ( r =0.999 9 ) , while the accuracy was ranged from -2.08% to 2.80%, the average recovery rate was ranged from 96.23%to 101.12%, and intra-and inter-day RSD were ranged from 0.46%to 2.46%and 5.84%to 9.75%, respectively, the lower limitation of quantification was 0.25 ng? mL-1 .Conclusion The HPLC-MS/MS method was accurate, sensitive, specific, and could be used in the determination of sunitinib in plasma and the clinical study of its pharmacokinetics.
