HPLC-MS/MS法测定人尿液中戊乙奎醚的浓度  

Determination of penehyclidine in human urine by HPLC-MS/MS

作　　者：黄娟[1,2] 雍小兰[1,2] 冯仕银[2] 王蓝天[2] 李楠[2] 杜晓琳[2] 

机构地区：[1]四川大学化学工程学院,成都610065 [2]中国人民解放军成都军区总医院临床药学科,成都610083

出　　处：《实用药物与临床》2015年第11期1355-1358,共4页Practical Pharmacy and Clinical Remedies

摘　　要：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,5μm）,流动相：5 m M醋酸铵（甲酸调pH 5.5）-甲醇（35∶65,v/v）,流速：1.0 m L/min,柱温：30℃,进样量10μL。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/m L（r=0.997 7）,最低定量限为1 ng/m L,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。Objective To develop an HPLC-MS /MS method for determination of penehyclidine in human urine. 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 BonusRP column（ 4. 6 mm × 150 mm,5 μm）,the mobile phase compositing with 5 m Mammonium acetate（ pH was adjusted to 5. 5 by formic acid） ： methanol（ 35∶ 65,v / v）,with a rate of 1. 0 m L / min,column temperature at 30 ℃,and injected sample volume of 10 μL. The results of positive ion MRMdetection 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 of1 ~ 100 ng / m L（ r = 0. 997 7） with the lower limit of quantitation（ LLOQ） 1 ng / m L. The intra-day RSD and inter-dayRSD were all below7. 9%. Conclusion The method is simple,rapid,specific and sensitive,it can be used for the pharmacokinetic study of penehyclidinein human urine.

关 键 词：戊乙奎醚 HPLC-MS/MS 尿液浓度 药动学 

分 类 号：R446.12[医药卫生—诊断学] O657.63[医药卫生—临床医学]