Li Lie, Pabbisetty Deepthi, Zhu Shiqian, Avery Mitchell A, Avery Bonnie A
Department of Pharmaceutics, School of Pharmacy, University of Mississippi, University, MS 38677, USA.
J Chromatogr Sci. 2008 Mar;46(3):215-9. doi: 10.1093/chromsci/46.3.215.
A method based on ultra-performance liquid chromatography mass spectrometry (UPLC-MS) applying atmospheric pressure chemical ionization in the positive ion mode is developed for the determination of coenzyme Q10 (CoQ10) in rat urine. The assay involves the extraction of crude urine, fast liquid chromatography on a Waters Acquity UPLC BEH C18 column (1.7 microm, 1.0 x 50 mm), and selected ion monitoring detection using mass transition. The calibration range is found to be 0.05-25 microg/mL, with the lower limit of quantitation of 0.05 microg/mL. Intra- and inter-day precision (relative standard deviation) for CoQ10 in rat urine range from 0.7% to 15%, and accuracy expressed in recovery rates in urine is between 83% and 118%. The recovery of this method is found to be between 80% and 95% at three concentrations. The total cumulative recovery of CoQ10 is 1.16 +/- 1.05% (percentage of dose intake, n = 4) from rat urine collected over 30 h after oral administration of the drug. The UPLC-MS method described allows the quick determination of CoQ10 in rat urine with good precision and accuracy. It is suitable for further excretion studies of CoQ10 in animals.
建立了一种基于超高效液相色谱-质谱联用(UPLC-MS)的方法,该方法采用大气压化学电离正离子模式测定大鼠尿液中的辅酶Q10(CoQ10)。该分析方法包括粗尿液提取、在Waters Acquity UPLC BEH C18柱(1.7微米,1.0×50毫米)上进行快速液相色谱分析以及使用质量跃迁进行选择离子监测检测。校准范围为0.05 - 25微克/毫升,定量下限为0.05微克/毫升。大鼠尿液中CoQ10的日内和日间精密度(相对标准偏差)范围为0.7%至15%,以尿液回收率表示的准确度在83%至118%之间。该方法在三个浓度下的回收率在80%至95%之间。口服给药后30小时收集的大鼠尿液中CoQ10的总累积回收率为1.16±1.05%(剂量摄入量的百分比,n = 4)。所描述的UPLC-MS方法能够快速、准确地测定大鼠尿液中的CoQ10,适用于CoQ10在动物体内的进一步排泄研究。