摘要
目的 建立测定骨髓移植患者血浆伏立康唑浓度的HPLC-MS/MS法,并应用于临床药物监测.方法 HPLC色谱柱为Ultimate XB-C18.柱温50℃,流速0.8 ml/min,流动相为含0.1%甲酸和2 mmol/L乙酸铵的水和含0.1%甲酸的甲醇,梯度洗脱.质谱检测方式为ESI正离子模式,多反应检测(MRM)扫描监测伏立康唑,用于定量分析的离子反应为:质荷比(m/z)350.1~281.2,用于定性分析的离子反应为:m/z 350.1~127.1;内标伏立康唑-d3 m/z 353.2~284.2.结果 伏立康唑浓度在0.1~10.0μg/ml时与峰面积线性关系良好(r=0.9991),日内及日间相对标准差(RSD)〈5%,平均回收率为88% ~103%.结论 本方法简便、准确、快速,适用于伏立康唑的血药浓度测定.
Objective To establish the HPLC-MS/MS method for determination of voriconazole in bone marrow transplant patients, and use it in clinic trial. Methods Chromatographic column of HPLC was Ultimate XB-C18. The gradient elution separation was performed on a Ultimate XB-C18 col-umn with a mobile phase of water (containing 2 mmol/L ammonium acetate and 0. 1% formic acid) and methanol (containing 0. 1% formic acid), and temperature of column was 50 ℃, at a speed of 0. 8 mL/min. The way of eluting was gradient. Mass spectrum detection method was ESI positive ion mode, and multiple reaction monitoring (MRM) was used to detect voriconazole ; ionic reaction in quati-tative analysis: mass-to-charge ratio (m/z) 350. 1-281.2, ionic reaction in qualitive analysis: m/z 350. 1-127. 1. Substance Voriconazole-d3 m/z 353.2-284. 2 was used as quantitative ion for Internal standard. Results The standard curve of voriconazole was linear over the range of O. 1-10. 0 μg/ml (r = 0. 9991). The average recovery was among the range of 88%-103% ; intra-day and inter-day vali-dation relative standard deviation (RSDs) were less than 5%. Conclusions This method is convenient, accurate and rapid, and can be used for the determination of voriconazole in clinic test.
作者
王磊
刘红星
Wang Lei;Liu Hongxing(Hebei Yanda Ludaopei Hospital, Sanhe 065201, China)
出处
《中国实用医刊》
2018年第9期30-33,共4页
Chinese Journal of Practical Medicine
关键词
伏立康唑
液质联用
治疗药物监测
Voriconazole
HPLC-MS/MS
Therapeutic drug monitoring