摘要
目的：建立了一种灵敏、准确的全血中痕量雷公藤红素的液相色谱／质谱联用测定方法。方法：全血样品经醋酸乙酯提取后，在XDB C18反相色谱柱（150mm×4．6mm i．d．，5μm）上，以0．05％醋酸-醋酸铵（5mmol／L）溶液/甲醇（2s：75，v／v）为流动相，以氢化可的松为内标，采用大气压化学电离源（APCI）在选择离子监测（SIM）模式下进行检测，定量离子为m／z[M-H]^-1 449．4。结果：雷公藤红素在1．0～200．0ng／ml范围具有良好的线性，检出限为1．0ng/ml，其日内和日间RSD分别小于9．1％和10．5％。结论：本方法可用于全血中痕量雷公藤红素的测定。
Objective：To establish a sensitive and accurate method for the analysis of celastrol in whole blood samples by high - performance liquid chromatography coupled with mass spectrometry （ HPLC - MS）. Methods：The separation was carried out on a XDB C18 reserved - phase column （ 150 mm×4. 6 mm i. d. , 5 μm） using 0. 05% （v/v） acetic acid - acetic acid ammonium （5 mmol/L）/methanol （25：75, v/v） as mobile phase in isocratic mode after blood samples were extracted by ethyl acetate. Detection was performed by an atmospheric pressure chemical ionization mass spectrometry （ APCI - MS） in the negative mode using hydrocortisone as an internal standard （IS）. The quasi - molecular ion m/z 449.4 [ M - H ]^- was selected for the quantification in selected ion monitoring （SIM） mode. Results： Within - day and day - to - day relative standard deviations were less than 9. 1% and 10. 5%, respectively： The linear range was 1.0 - 200. 0 ng/ml for celastrol. The limit of quantification （LOQ） in whole blood samples was 1.0 ng/ml. Conclusion, The method can be applied to determination of trace celastrol in whole blood samples.
出处
《中国卫生检验杂志》
CAS
2008年第7期1242-1244,共3页
Chinese Journal of Health Laboratory Technology
基金
宁波市医学科技计划资助项目(200543)
