CAJ | 학술논문

目的建立测定人尿液中戊乙奎醚浓度的HPLC-MS/MS法. 方法尿样经稀释,离心后取上清液进行HPLC-MS/MS测定. 色谱柱:Agilent ZORBAX Bonus-RP (4. 6 mm × 150 mm,5 μm),流动相:5 mM醋酸铵(甲酸调pH 5. 5) -甲醇(35:65,v/v),流速:1. 0 mL/min,柱温:30 ℃,进样量10 μL. 采用电喷雾离子源( ESI) ,正离子模式多重反应选择离子检测( MRM). 戊乙奎醚和内标的定量离子对分别为m/z 316. 2→128. 1和m/z 256. 2→167. 1. 结果线性范围为1~100 ng/mL(r=0. 997 7),最低定量限为1 ng/mL,日内和日间精密度( RSD)均<7. 9%. 结论本方法简单、快速、灵敏、专属性高,适用于人尿液中戊乙奎醚药动学的研究.
목적 건립측정인뇨액중무을규미농도적HPLC-MS/MS법. 방법 뇨양경희석,리심후취상청액진행HPLC-MS/MS측정. 색보주:Agilent ZORBAX Bonus-RP (4. 6 mm × 150 mm,5 μm),류동상:5 mM작산안(갑산조pH 5. 5) -갑순(35:65,v/v),류속:1. 0 mL/min,주온:30 ℃,진양량10 μL. 채용전분무리자원( ESI) ,정리자모식다중반응선택리자검측( MRM). 무을규미화내표적정량리자대분별위m/z 316. 2→128. 1화m/z 256. 2→167. 1. 결과 선성범위위1~100 ng/mL(r=0. 997 7),최저정량한위1 ng/mL,일내화일간정밀도( RSD)균<7. 9%. 결론 본방법간단、쾌속、령민、전속성고,괄용우인뇨액중무을규미약동학적연구.
Objective To develop an HPLC-MS/MS method for determination of penehyclidine in human u-rine. Methods The supernatant liquid obtained from the diluted urine centrifugate was subjected to sample introduction and was analyzed by the HPLC-MS/MS method under flowing chromatographic conditions:Agilent ZORBAX Bonus-RP column (4. 6 mm × 150 mm,5 μm),the mobile phase compositing with 5 mM ammonium acetate (pH was adjus-ted to 5. 5 by formic acid):methanol (35:65,v/v),with a rate of 1. 0 mL/min,column temperature at 30 ℃,and in-jected sample volume of 10 μL. The results of positive ion MRM detection of penehyclidine and internal standards were m/z 316. 2→128. 1 and m/z 256. 2→167. 1. Results The calibration curve was linear over the concentration range of 1~100 ng/mL(r=0. 997 7)with the lower limit of quantitation (LLOQ) 1 ng/mL. The intra-day RSD and inter-day RSD were all below 7. 9%. Conclusion The method is simple, rapid, specific and sensitive, it can be used for the pharmacokinetic study of penehyclidinein human urine.