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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 HPLC / MS for the determination of the activity of rat and canine liver microsomes with nifedipine as a probe. Methods SHIMADZU VP-ODS (2.0mm × 150mm, 5μm) column was used. The column temperature was at room temperature. The mobile phase was methanol-water (55:45) and the flow rate was 0.2mL · min-1. Select positive ion scan (SIM) m / z345. Nifedipine was used as a probe to in vitro incubation with rat or Beagle liver microsomes. Nifedipine, a metabolite of nifedipine, was determined by liquid chromatography-tandem mass spectrometry. Results Under the established HPLC / MS conditions, the oxidation product retention time of nifedipine was about 7.15min. The lowest detection limit of oxidation nifedipine was 3μg · L-1 (S / N = 3) and the linear range was 0.01-10 mg · L-1. The recovery and precision met the detection requirements. Conclusion The HPLC / MS can accurately detect nifedipine oxidation products in rat and Beagle liver microsomes.