摘要
目的:建立高效液相色谱/质谱联用测定人血浆中雷公藤甲素浓度的方法.方法:应用Thermo-keystone Hypurity G18柱(150 mm× 2.1 mm,5μm);流动相为甲醇-水(30:70);流速为0.2 mL·min-1;柱温为40℃,自动进样瓶温10℃;进样量为10μL.采用LCQ Deca XP TM液质联用仪,离子源为APCI源,源电压4.0 kV;加热毛细管温度200℃;氮气(N2)流速50 mL·min-1;辅助气流速15 mL·min-1;正离子方式检测;扫描方式为选择反应监测(SRM),用于定量分析的离子质荷比(m/z)分别为343和246.结果:雷公藤甲素的线性范围为4.1～262.0μg·L-1,最低检测浓度为2.0 μg·L-1.日内、日间精密度分别为1.5%～5.6%和4.1%～7.8%.结论:液质联用方法适用于临床人体血浆雷公藤甲素浓度监测.
OBJECTIVE To establish a method for the determination of triptolide in human plasma by HPLC/MS. METHODS Use Thermo-keystone Hypurity C18 column （150 × 2. 1 mm, 5μm） ;the mobile phase was methanol-water （30：70） with a flow rate of 0. 2 mL：min^-1 ; column temperature 40 ℃. A Finnigan LCQ Deca XP TM with an atmospheric pressure chemical ionization （APCI） source was used as detector and was operated in positive ion mode. Selected reaction monitoring （SRM） was used and transitions selected for quantization were： 343 and 246（m/z）, the mass spectrometric conditions were as follows： the temperatures of the heated capillary was 200 ＊C. Nitrogen was used as sheath and auxiliary gas with a flow rate of 50 and 15 mL. min^-1. RESULTS The calibration curve was linear over the concentration range of 4. 1 to 262. 0 μg：L^-1, the limit of quantization was 2. 0μg： L^-1 Within-day and between- day precision expressed by relative standard deviation （RSD） was 1.5% to 5. 6% and 4. 1% to 7. 8%, respectively. CONCLUSION This method is proved to be specific, accurate and sensitive enough to be applied to the determination of triptolide in human plasma
出处
《中国医院药学杂志》
CAS
CSCD
北大核心
2005年第9期802-804,共3页
Chinese Journal of Hospital Pharmacy
基金
国家自然科学基金资助项目(编号:90209049)
