LC-MS/MS法测定人粪便中匹诺塞林的浓度及在粪便排泄中的应用

目的建立LC-MS/MS测定人粪便中匹诺塞林浓度并将其应用于粪便排泄的方法。方法样品用乙腈提取处理,用LunaTMC8色谱柱,以乙腈-乙酸铵水为流动相,等度洗脱(65∶35),流速为0.25 mL.min-1,电喷雾电离源(ESI),用负离子模式检测,多反应离子监测(MRM)。结果匹诺塞林的线性范围为30～4000 ng.mL-1,定量下限为30 ng.mL-1,日间、日内准确度与精密度变异均<7%,回收率均>90%,不存在基质效应。48 h内粪便的累积排泄率为(1.9±1.4)%。结论本方法快速、灵敏、专属性强、重现性好,可用于人粪便中的匹诺塞林测定。

Determination of pinocembrin in human feces by LC-MS/MS and and its application to feces excretion

Objective To develop an LC-MS/MS method for the determination of pinocembrin in human feces and apply the method to the study of feces excretion.Methods The column was a Phenomenex LunaTM C8 column and the mobile phase consisted of acetonitrile-ammonium acetate aqueous solution(65∶35) at a flow rate of 0.25 mL·min-1.Acetonitrile was used in sample preparation.The detection was performed by multiple reaction monitoring mode via a negative eletrospray ionization source.Results The assay was linear over the range of 30-4000 ng·mL-1 with a limit of quantitation of 30 ng·mL-1,the RSD of intra-and inter-day validation were both less than 7%,the recovery was all greater than 90%,and there was no matrix effects.Feces excretory rate in 48 h was(1.9±1.4)%.Conclusion This validated assay is a rapid,sensitive,selective and reliable method for the determination of pinocembrin in human feces,which provided a base for the study on feces excretion of pinocembrin.