A rapid,specific and sensitive HPLC-MS/MS method was developed and validated for the determination of 20(S)-protopanaxadiol(PPD)in human plasma.PPD and the internal standard PD were extracted from plasma by liquid-liq...A rapid,specific and sensitive HPLC-MS/MS method was developed and validated for the determination of 20(S)-protopanaxadiol(PPD)in human plasma.PPD and the internal standard PD were extracted from plasma by liquid-liquid extraction with cyclohexane-methylene dichloride(2:1,v/v).The separation was performed on a HyPURIYTY C18 column using methanol-5 mM ammonium formate(90:10,v/v)as mobile phase at a flow rate of 0.35 mL/min.Mass spectrometric detection was carried out by electrospray ionization(ESI)in the positive ion mode using multiple reaction monitoring(MRM).The monitored transitions were m/z 425.4-217.2 for PPD and at m/z 461.4-425.5 for PD.The method was linear over the range 0.512-100 ng/mL with a lower limit of quantification(LLOQ)of 0.512 ng/mL.The mean extraction recovery of PPD was greater than 78.2%and no significant matrix effect was detected.The intra-and inter-day precisions were less than 10%and the biases below 4%for PPD.The validated method was applied to a three-level single-dose clinical pharmacokinetics study of 12 healthy Chinese volunteers and the main pharmacokinetic parameters of PPD were obtained.展开更多
基金supported by the National Natural Science Foundation of China(No.81102499)Hunan Science and Technology Project(No.2011SK3261)a grant from the Open-End Fund for the Valuable and Precision Instruments of Central South University(Changsha,China).
文摘A rapid,specific and sensitive HPLC-MS/MS method was developed and validated for the determination of 20(S)-protopanaxadiol(PPD)in human plasma.PPD and the internal standard PD were extracted from plasma by liquid-liquid extraction with cyclohexane-methylene dichloride(2:1,v/v).The separation was performed on a HyPURIYTY C18 column using methanol-5 mM ammonium formate(90:10,v/v)as mobile phase at a flow rate of 0.35 mL/min.Mass spectrometric detection was carried out by electrospray ionization(ESI)in the positive ion mode using multiple reaction monitoring(MRM).The monitored transitions were m/z 425.4-217.2 for PPD and at m/z 461.4-425.5 for PD.The method was linear over the range 0.512-100 ng/mL with a lower limit of quantification(LLOQ)of 0.512 ng/mL.The mean extraction recovery of PPD was greater than 78.2%and no significant matrix effect was detected.The intra-and inter-day precisions were less than 10%and the biases below 4%for PPD.The validated method was applied to a three-level single-dose clinical pharmacokinetics study of 12 healthy Chinese volunteers and the main pharmacokinetic parameters of PPD were obtained.
