关键词: 盐酸戊乙奎醚, 维拉帕米, HPLC-MS/MS, 血浆, 尿样

Abstract: AIM: To establish a high performance liquid chromatography- tandem mass spectrometry (HPLC-MS/MS) method for the determination of penehyclidine hydrochloride in human plasma and urine. METHODS: Penehyclidine hydrochloride was determinated by AB SCIEX QTRAP 5500 three triple quadrupole hybrid linear ion trap tandem mass spectrometer and Agilent 1200 high performance liquid chromatography. The samples were extracted with methyl tert-butyl ether, and verapamil is the internal standard (IS). The analytical column was a Thermo Hypersil GOLD column (30 mm×2.1 mm,3 μm).The mobile phase, acetonitrile- water (80∶20,which contains 10 mmol/L of ammonium acetate and 0.01 ‰ formic acid),was used at a flow rate of 0.3 mL/min. Penehyclidine hydrochloride and verapamil were detected on multiple reaction monitoring (MRM) by the transitions from the recursor to the production (m/z 316. 2→128.3 and m/z 454.6→303.4).The injection vpolume was 5 μL and the total run time was 4.0 min. RESULTS: Penehyclidine hydrochloride and verapamil concentrations in plasma and urine were detected well by HPLC-MS/MS method.The retention time of these analytes were 1.25 min and 0.84 min. Penehyclidine hydrochloride curve in plasma and urine had good linearity in the range of 0.05-10 ng/mL.Lower limit of quantification (LLOQ) was 0.05 ng/mL.The intra-batch and inter-batch precision (RSD) in plasma and urine were all less than 11.69% and the accuracy were all less than -2.81%. CONCLUSION: In this experiment,plasma and urine concentrations of penehyclidine hydrochloride were detected by the specificity,accuracy,sensitivity and reliability technical HPLC-MS/MS,reliable the study on the pharmacokinetics of penehyclidine hydrochloride.

Key words: penehyclidine hydrochloride, verapamil, HPLC-MS/MS, plasma, urine