血浆中环维黄杨星D的测定方法学研究

目的建立血浆中环维黄杨星D的浓度测定方法。方法在含有环维黄杨星D的血浆中加入内标盐酸多奈哌齐,碱化后液-液萃取,采用LC-MS联用技术,以环维黄杨星D的准分子离子（M＋H]^＋,m/z403）和内标多奈哌齐的准分子离子（M＋H]^＋,m/z 380）进行测定。色谱条件：Agilent SB C18（2.1 mm×50mm,3.5μm）,甲醇：醋酸盐缓冲液（80∶20）为流动相,流速：0.4 mL/min;质谱检测参数：大气压化学源（AP-CI）接口,气化室温度：350℃,鞘气流速：65 arb,辅助气流速：20 arb,放电电流：5.00μA,毛细管温度：200℃。结果环维黄杨星D在1-500 ng.mL^-1的范围内呈线性,最低检测限为0.1 ng.mL^-1。结论该测定方法具有灵敏、专一和快速的优点,可用于血浆中环维黄杨星D的含量测定。

Determination of Cyclovirobuxine D in Plasma by HPLC-APCI-MS

Objective To establish a method for determination of cyclovirobuxine D in the plasma.Methods Agilent SB C18 column(2.1 mm×50 mm,3.5 μm) was used with the mobile phase consisted of methanol-acetate buffer(80:20),and was set at a flow rate of 0.4 mL·min-1.Detection was performed on the electrospray ion trap mass spectrometer with an APCI interface and operated in positive-ionization mode.Cyclovirobuxine D quantity was realized by computing the peak area ratio cyclovirobuxine D m/z 403/donepeziL m/z380)and comparing them with calibration curve(r=0.999 8).Vaporizer Temp:350℃,Sheath Gas Flow Rate:65arb,Aux/Sweep Gas Flow Rate:20 arb,Dischange Current: 5.00 μA,Capillarg Temp:200℃.Results Cyclovirobuxine D had a good linear within the ranges of 1～500 ng·mL-1 and the detection limit was 0.1 ng·mL-1.Conclusion The method can be successfully applied to determinate the concentrations of cyclovirobuxine D in the plasma.