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The alkaloids from P.longum L showed protective effects on ParkinsonS diseasemodels in our previous study and piperine and piperlonguminine were the two main constituentsin the alkaloids．The present study aimed at developing a rapid，sensitive，and accurateUFLC-ESI-MS／MS method and validating it for the simultaneous determination of piperine andpiperIonguminine in rat plasma using terfenadine as the internal standard．The analytes andinternal standard(IS)were extracted from rat plasma using a simple protein precipitation byadding methanol／acetonitrile(1：1，v/v)．A Phenomenex Gemini 3 U C 1 8 column(20 mm×2.00mm,3 pm)Was used to separate the analytes and IS using a gradient mode system with a mobilephase consisting of water with O.1％formic acid(mobile phase A)and acetonitrile with O.1％formic acid(mobile phase B)at a flow rate ofO.4 mL／min and an operating column temperature of25℃．The total analytical run time was 4 min．The detection was performed using the positive ionelectrospray ionization(ESI)in multiple reaction monitoring(MRM)mode with transitions at m／z286.1-201.1 for piperine，m／z 274.0-201.1 for piperionguminine，and m／z 472.4—436.4 for the IS·The calibration cur、，es were both linear(r>0．995)over a concention range of 1.0 to 1,000ng／mL;the lower limit of quantification(LLOQs)was 1.0 ng／mL for both piperine andpiperlonguminine．The intra-day and inter-day precisiom(RSD％)were<12.1％，accuraciesranged from 86.6 to 120％,and recoveries ranged from 90.4 to 108％．The analytes were provenstable in the short-term，long-term，and after three freeze-thaw cycles．The method Wassuccessfully applied to pharmacokinetic studies of piperine and piperlonguminine in rats after oraladministration of alkaloids from Piper longum L．