HPLC-MS/MS法测定人血浆中西洛他唑浓度

目的建立灵敏快速检测人血浆中西洛他唑浓度的HPLC-MS/MS方法。方法采用色谱柱为Thermo Hy-purity C18（150 mm×2.1 mm,5μm,USA）,流动相为乙腈（含0.1%甲酸）-甲醇=25∶75（v/v）;流速为0.2mL.min-1;ESI＋离子源,MRM进行离子方式监测。质谱参数：源电压3 500V,源温度100℃,去溶剂化温度350℃,锥孔气流速50 L.h^-1,去溶剂化气流速350 L.h^-1;血浆处理采用乙腈直接沉淀萃取方法。结果血浆中西洛他唑检测方法的线性范围为4.90-2 510 ng.mL-1,最低检出浓度为4.90 ng.mL-1,血浆中西洛他唑的方法回收率在80%-120%,日内RSD〈10%,日间RSD〈15%。结论本方法用于测定人血浆中西洛他唑的浓度,简单、快速、灵敏。

HPLC-MS/MS method for the determination of cilostazol in human plasma

Objective To develop a sensitive and quick high performance liquid chromatography（HPLC）-mass spectrometry（MS）/MS method for the determination of cilostazol.Methods The separation was performed on a Thermo Hypurity C18（150 mm×2.1 mm,5 μm,USA）.The mobile phase was acetonitrile（containing 0.1% formic acid）-methanol（25∶75,v/v）,and the flow rate 0.2 mL· min-1.The analytes were detected by the electronic-spry ionization（ESI）-multiple reaction monitoring（MRM） mode.The MS detection parameters were as follows： the capillary voltage was 3 500 V,source temperature was 100 ℃,desolation temperature was 350 ℃,cone gas flow was 50 L·h-1 and desolation flow was 350 L·h-1.The plasma proteins were precipitated by acetonitrile directly.Results The linearity of the plasma concentration of cilostazol was 4.90～2 510 ng·mL-1 and detection limit was 4.90 ng·mL-1.The relative recovery of cilostazol was 80%-120%.The intra-day and inter-day RSD was less than 10% and 15%,respectively.Conclusion The method is simple,quick,and sensitive and can be used to determine cilostazol in human plasma.