Huo Jiping, Wang Hongyun, Hu Pei, Li Pingya, Liu Jinping, Jiang Ji
Clinical Pharmacology Research Center, Peking Union Medical College Hospital, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing, 100730, China.
Biomed Chromatogr. 2013 Dec;27(12):1701-7. doi: 10.1002/bmc.2982. Epub 2013 Jul 15.
A specific, sensitive and rapid method based on high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) was developed for the determination of pseudo-ginsenoside GQ in human plasma. Liquid-liquid extraction was used to isolate the analyte from biological matrix followed by injection of the extracts onto a C8 column with isocratic elution. Detection was carried out on a triple quadrupole tandem mass spectrometer (API-4000 system) in multiple reaction monitoring mode using negative electrospray ionization. The mobile phase consisted of methanol-10 mM ammonium acetate (90:10, v/v) and the flow rate was 0.3 mL/min. The method was validated over the concentration range of 5.0-5000.0 ng/mL for plasma. Inter- and intra-day precisions (relative standard deviation) were all within 15% and the accuracy (relative error) was ≤ 9.4%. The lower limit of quantitation was 5.0 ng/mL. The pseudo-ginsenoside GQ was stable after 8 h at room temperature, 24 h at autosampler and three freeze-thaw cycles (from -30 to 25 °C). The method was successfully applied to the pharmacokinetic study of pseudo-ginsenoside GQ in healthy Chinese volunteers.
建立了一种基于高效液相色谱-串联质谱（HPLC-MS/MS）的特异性强、灵敏度高且快速的方法，用于测定人血浆中的拟人参皂苷GQ。采用液-液萃取法从生物基质中分离分析物，然后将萃取物注入C8柱进行等度洗脱。在三重四极杆串联质谱仪（API-4000系统）上采用负电喷雾电离，以多反应监测模式进行检测。流动相由甲醇-10 mM醋酸铵（90:10，v/v）组成，流速为0.3 mL/min。该方法在血浆浓度范围为5.0-5000.0 ng/mL内进行了验证。日间和日内精密度（相对标准偏差）均在15%以内，准确度（相对误差）≤9.4%。定量下限为5.0 ng/mL。拟人参皂苷GQ在室温下8小时、自动进样器中24小时以及三个冻融循环（从-30至25°C）后均稳定。该方法成功应用于健康中国志愿者体内拟人参皂苷GQ的药代动力学研究。
