高效液相色谱-电喷雾离子阱质谱联用测定人血浆中伊曲康唑浓度

HPLC-ESI/MS determination of itraconazole in human plasma

目的:建立高效液相色谱-电喷雾离子阱质谱联用(HPLC-ESI/MS)测定人血浆中伊曲康唑浓度方法。方法:以地西泮为内标,用甲基叔丁基醚提取,色谱柱为 Kromasil 100 C_(18)(5 μm,10 mm×0.21 mm),流动相为0.1%甲酸-乙腈(30:70),流速为0.3 mL·min^(-1);质谱条件采用电喷雾正离子源(ESI^+),以二级质谱选择反应监测(SRM)方式进行检测。结果:测定伊曲康唑的线性范围为5.0～400.0 ng·mL^(-1),最低检测限约为1.0 ng·mL^(-1)。日内、日间精密度 RSD<15%。方法回收率范围为90.0%～110.0%。结论:方法精密、准确,能有效地检测人血浆中伊曲康唑浓度。

Objective：To establish a method of liquid chromatography electrospray ion trap mass spectrometry to determine itraconazole in human plasma. Method： Diazepam as internal standard ; After extraction with methylt - butyl ether,plasma sample was separated on a Kromasil 100 C18 colum（5 μm, 10 mm ×0. 21 mm） ,with mobile phase 0. 1% formic acid - acetonitrile （30： 70） , at a flow rate of 0. 3 mL · min^-1 . The electrospray ion trap mass spectrum in the positive mode and selected reaction monitor（SRM）were adopted to detect the coneentration of itraconazole. Results： The standard curves were linear over the range 5.0 - 400. 0 ng · mL ^- 1 for itraconazole in human plasma,the lower limits of assay was 1.0 ng · mL ^- 1 ; The mean inter - and intra - day variation coefficients were less than 15% ;The relative recovery averaged between 90% - 110%. Conclusion：The method is simple, sensitive and reproducible, and the results are reliable and accurate for determination of itraconazole.