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目的:建立高效液相色谱-串联质谱(HPLC-MS/MS)方法测定人血浆及尿样中盐酸戊乙奎醚的浓度。方法:采用AB SCIEX QTRAP 5500三重四极杆复合线性离子阱串联质谱仪及Agilent 1200高效液相色谱仪进行检测。样品经甲基叔丁基醚提取处理,以维拉帕米为内标。色谱柱为Thermo Hypersil GOLD柱(30mm×2.1mm,3μm),流动相为乙腈:水(80∶20,V/V)(含10mmol/L的乙酸铵及0.01‰的甲酸);流速为0.3mL/min。盐酸戊乙奎醚和维拉帕米的MRM扫描离子通道m/z分别为316.2→128.3,454.6→303.4。进样量:5μL。结果:盐酸戊乙奎醚和维拉帕米分离良好,保留时间分别为1.25min、0.84min。盐酸戊乙奎醚血浆及尿液样品在0.05~10ng/mL范围内线性关系良好,定量下限为0.05ng/mL,批内、批间RSD均低于11.69%,准确度均低于-2.81%。结论:本法样品预处理简便快捷,检测结果专属性强,灵敏度好,准确度高,适用盐酸戊乙奎醚药代动力学的研究。
Objective: 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 samples. Methods: AB SCIEX QTRAP 5500 triple quadrupole linear ion trap tandem mass spectrometer and Agilent 1200 high performance liquid chromatography were used for detection. Samples were extracted with methyl tert-butyl ether and verapamil as internal standard. The column was a Thermo Hypersil GOLD column (30 mm × 2.1 mm, 3 μm) with a mobile phase of acetonitrile: water (80:20, V / V) containing 10 mmol / L ammonium acetate and 0.01 ‰ formic acid; / min. The m / z of MRM scanning ion channels of penehyclidine hydrochloride and verapamil were respectively 316.2 → 128.3 and 454.6 → 303.4. Injection volume: 5μL. Results: Penehyclidine hydrochloride and verapamil were separated well with retention times of 1.25 min and 0.84 min, respectively. The plasma and urine samples of penehyclidine hydrochloride showed good linearity in the range of 0.05 ~ 10ng / mL with the lower limit of quantitation of 0.05ng / mL, the intra-assay and post-assay RSD of less than 11.69% and the accuracy of less than -2.81% . Conclusion: The method of sample pretreatment is quick and easy, the test results are specific, sensitive and accurate. The pharmacokinetics of penehyclidine hydrochloride is suitable.