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目的建立液相色谱串联质谱法测定人血清中可的宁的含量。方法以稳定同位素化合物(氘3-可的宁)为内标,血清经直接沉淀后进样分析。以XBridge~(TM) Phenyl(2.1 mm×150 mm,5μm)为分析柱,含0.02%甲酸的水溶液-含0.02%甲酸的乙腈溶液(83:17,V/V)为流动相。电喷雾离子源,正离子MRM扫描分析,可的宁和内标离子对分别为m/z 177.0→80.0和m/z 180.5→80.2。结果可的宁在10～2 000μg·L~(-1)范围内线性关系良好,定量下限为10μg·L~(-1)。批内、批间精密度RSD均小于5%,平均提取回收率在77.9%～88.6%范围内。结论本方法灵敏度高、专一性好、操作简单,可用于人血清中可的宁的检测。
Objective To establish a liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for the determination of cortinone in human serum. Methods Stable isotope compounds (deuterium 3-cortinone) as internal standard, the serum was directly precipitated after injection analysis. The mobile phase consisted of 0.02% formic acid in water and acetonitrile (83:17, V / V) containing 0.02% formic acid on an XBridgeTM Phenyl (2.1 mm × 150 mm, 5 μm) column. Electrospray ionization, positive ion MRM scanning analysis, cortinone and internal standard ion pairs were m / z 177.0 → 80.0 and m / z 180.5 → 80.2, respectively. Results Cortinone showed good linearity in the range of 10-2 000 μg · L -1 with a lower limit of quantitation of 10 μg · L -1. The intra-batch and inter-batch precision RSDs were less than 5%, and the average extraction recovery was in the range of 77.9% -88.6%. Conclusion The method is sensitive, specific and easy to operate. It can be used for the determination of cortinone in human serum.