UPLC-MS/MS法测定血浆中新型酪氨酸酶抑制剂UP302的含量  

UPLC-MS/MS quantification of a natural novel tyrosinase inhibitor UP302 in plasma

作　　者：朱凌[1] 张双庆[1] 闻镍[1] 于敏[1] 李佐刚[1] 

机构地区：[1]中国食品药品检定研究院国家药物安全评价监测中心,北京100176

出　　处：《药物分析杂志》2012年第1期40-43,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立超高效液相色谱-串联质谱测定血浆中新型酪氨酸酶抑制剂UP302的方法,并用于研究UP302在大鼠、狗、猴和人血浆中的稳定性。方法:血浆中加入内标大豆苷元经2倍体积甲醇沉淀后进行分析。采用Hypersil Gold C18(50 mm×2.1 mm,1.9μm)色谱柱,流动相为甲醇(A)-5 mmol.L-1甲酸铵水溶液(B),梯度洗脱,梯度流速恒定为0.2 mL.min-1,柱温为30℃,整个分析时间为6 min。采用负离子电喷雾离子化电离源和选择反应监测模式进行检测。结果:在5～2000 ng.mL-1的浓度范围内,标准曲线线性关系良好(r=0.9998);血浆中UP302最低定量下限为5 ng.mL-1;本方法日内日间准确度在99.2%～107.3%,日内日间精密度均小于9.3%。结论:本方法灵敏度高,重现性好,操作简便,可用于血浆中UP302浓度的测定。Objective：To establish an ultra -performance liquid chromatography -tandem mass spectrometry （UP- LC- MS/MS） method for the determination of tyrosinase inhibitor UP302 in plasma, and study the stability of UP302 in rat, dog, monkey and human plasma. Methods：The plasma samples were precipitated by methanol using daidzein as an internal standard. On Hypersil Gold C18column （50 mm × 2. 1 mm, 1.9 μm） , separation was achieved by a gradient mobile phase of methanol and 5 mmol · L^- 1 ammonium formate solution at a flow rate of 0. 2 mL · min^ - l at 30℃. The total analysis time was 6 min. Selection - reaction monitoring mode in negative - mode electrospray ionization was used to detect UP302 in plasma. Results：Calibration curve was linear in a range from 5 - 2000 ng · mL^- 1 with a correlation coefficient of 0. 9998. The lower limit of quantification was 5 ng · mL^- 1. The intra - and inter - day accuracy was between 99.2% and 107.3% , and precision was less than 9. 3%. Conclusion ： The UPLC - MS/MS method is sensitive and reproducible. It can be used for the determination of UP302 in plasma.

关 键 词：酪氨酸酶抑制剂 UP302 大豆苷元 血浆样品 稳定性 超高效液相色谱-串联质谱 临床前研究 

分 类 号：R917[医药卫生—药物分析学]