UFLC-MS/MS法测定胎盘灌流液中艾司西酞普兰浓度

Determination of Escitalopram in Placental Perfusate by UFLC-MS/MS

目的:建立超快速液相色谱-串联质谱(UFLC-MS/MS)法测定人胎盘灌流液中艾司西酞普兰浓度。方法:以格列苯脲为内标,色谱柱为SynergiTM Hydro-RP 80?分析柱(50 mm×2.0 mm,4.0μm),样品前处理采用甲醇沉淀蛋白法,流动相A为0.1%甲酸-水,流动相B为0.1%甲酸-乙腈,流速为0.5 ml·min^(-1),梯度洗脱。质谱采用电喷雾离子源(ESI)正离子模式,多离子反应监测(MRM),艾司西酞普兰和格列苯脲的定量离子对分别为m/z 325.119/262.100和494.200/369.100。结果:胎盘灌流液中艾司西酞普兰浓度在2.25~250 ng·ml^(-1)范围内线性关系良好(r=0.9974),平均回收率97.81%~107.56%,基质效应81.15%~87.10%,批内及批间精密度RSD均小于15%,稳定性考察结果良好。结论:所建方法快速、灵敏且特异性强,适用于胎盘灌流液中艾司西酞普兰浓度的测定。

Objective:To establish an ultra-fast liquid chromatography-tandem mass spectrometry(UFLC-MS/MS)method for determining the concentration of escitalopram(ETP)in placental perfusate.Methods:Glibenclamide was used as the internal standard,and the samples were precipitated with methanol.Analysis of escitalopram was carried out on a SynergiTM Hydro-RP 80?column(50 mm×2.0 mm,4.0μm).Gradient elution was used with 0.1%formic acid-H2O as mobile phase A and acetonitrile containing 0.1%formic acid as mobile phase B at a flow rate of 0.5 ml·min^(-1).Detection was performed with multiple reactions monitoring using positive electrospray ionization,and the quantitative ion pairs were m/z 325.119/262.100 and 494.200/369.100 for escitalopram and glibenclamid,respectively.Results:Linearities were good from 2.25 to 250 ng·ml^(-1)for escitalopram(r=0.9974).The mean recoveries and matrix effect were 97.81%^(-1)07.56%and 81.15%-87.10%,respectively.The intra-and inter-day RSDs were all less than 15%and the stability of analytes were acceptable.Conclusion:The results showed that the method was rapid,sensitive and specific,which was successfully applied in the determination of ETP in placenta perfusate.