摘要
目的建立以硝苯地平为探针药物测定大鼠和犬肝微粒体活性的HPLC/MS。方法采用SHIMADZU VP-ODS(2.0mm×150mm,5μm)色谱柱;柱温为室温;以甲醇-水(55∶45)为流动相,流速:0.2mL·min-1。选择正离子扫描(SIM)m/z345。以硝苯地平为探针药物与大鼠或Beagle犬的肝微粒体进行体外孵育,以液相色谱串联质谱法测定硝苯地平的代谢产物氧化硝苯地平。结果在所建立的HPLC/MS条件下,硝苯地平的氧化产物保留时间约为7.15min。杂质峰不干扰测定;氧化硝苯地平最低检测限为3μg·L-1(S/N=3),线性范围为0.01～10mg·L-1,回收率及精密度均符合检测要求。结论该HPLC/MS能够准确的检测出在大鼠和Beagle犬肝微粒体中的硝苯地平氧化产物。
OBJECTIVE To establish a HPLC/MS method to determine microsomes activity in vitro using nifedipine as a probe drug. METHODS Nifedipine was incubated with rat or Beagle dog liver microsomes in vitro, oxidized nifedipine were determined by HPLC-MS. A SHIMADZU-ODS （2.0 mm× 150 mm） column as chromatographic column. The mobile phase consisted of methanol-water （55 ： 45） at a flow rate of 0.2 mL·min^-1. MS detector was set as positive selective ion scan mode at m/z 345. RESULTS The retention time of oxidized nifedipine was 7.15 rain. The detection limit in rat or Beagle dog liver microsomes was 3 μg·L^-1 for oxidized nifedipine （S/N=3）, and the linear range was over the range of 0.01-10 mg·L^-1. The recovery and accuracy satisfied the requirement of detection for oxidized nifedipine in rat and Beagle dog liver microsomes. CONCLUSION Oxidized nifedipine can be detected accurately and precisely by using the HPLC/MS method.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2009年第7期506-509,共4页
Chinese Pharmaceutical Journal
基金
国家自然科学基金重点资助项目(30730110)
陕西省自然科学基金资助项目(2006C221)
