HPLC-ESI/MS测定血浆中9-羟基利培酮异构体

HPLC-ESI/MS determination of 9-hydroxyrisperidone enantiomers

目的建立血浆中9-羟基利培酮（9-OH-RSP）异构体的测定方法。方法样品经液-液萃取后，采用ChiralAGP柱（100mm×4．0mm，5μm）进行分离，柱温为25℃，以50mmol·L^-1醋酸铵（pH6．5）-异丙醇（95：5）为流动相，流速为0．9mL·min。采用电喷雾电离源正离子模式（ESI^＋），选择性离子监测（SIR）9-OH-RSP和内标安定的质荷比（m／z）分别为428和285的分子离子峰。结果9-羟基利培酮异构体在1．47～275．30μg·L^-1线性良好。左右旋异构体萃取回收率均〉80％，日内、日间RSD均〈15％。结论该方法准确、重现性好、灵敏度高，可用于测定血浆中9-羟基利培酮异构体的浓度。

Objective To develop a method for the determination of 9-hydroxyrisperidone enantiomers in the plasma. Methods After being pretreated by liquid-liquid extraction, the samples were separated by Chiral-AGP column at 25 ℃. The mobile phase was 50 mmol · L^-1 ammonium acetate （pH 6. 5） -isoprotanol （95 ： 5, w/v） with the flow rate of 0. 9 mL · min^-1. The compound was ionized in the electrospray ionization （ESF-） ion source of the mass spectrometer and detected in the selected ion recording （SIR） mode with the m/z of 9-OH-RSP and I. S. of 428 and 285 respectively. Results The assay was linear from 1.47 to 275.30μg · L^-1 for each enantiomer of 9-hydroxyrisperidone. The absolute recovery for each enantiomer was larger than 80%. The intra day and inter-day variations were less than 15%. Conclusion The method is accurate, sensitive, reliable and suitable for the determination of 9-hydroxyrisperidone enantiomers in the human plasma.