Sun Chenglong, Li Qian, Pan Liping, Liu Bing, Gu Pan, Zhang Junying, Ding Li, Wu Chungyong
Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China; Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China.
Department of Pharmaceutics of Traditional Chinese Medicine, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China.
J Pharm Biomed Anal. 2015;111:163-8. doi: 10.1016/j.jpba.2015.03.025. Epub 2015 Apr 3.
An easy LC-ESI-MS/MS method was developed and validated for simultaneous determination of rupatadine (RT) and its two active metabolites, namely desloratadine (DT) and 3-hydroxydesloratadine (3-OH-DT), in human plasma. The chromatographic separation was carried out on a C18 column with gradient elution by using methanol and 10mM ammonium acetate containing 0.1% (v/v) formic acid. The lower limit of quantification (LLOQ) was 0.05, 0.035 and 0.035 ng/mL for RT, DT and 3-OH-DT, respectively. The intra- and inter-day precision of analytes were within the range of 1.0-4.7% and 2.2-12.1%, respectively. The intra- and inter-day accuracy of analytes were within the range of -7.7% to 5.2% and -4.1% to 4.8%, respectively. The method was successfully applied to a pharmacokinetic study of RT and its two metabolite DT and 3-OH-DT in healthy volunteers following single (10, 20, 40 mg) and multiple (10 mg) oral doses of rupatadine fumarate tablets.
建立并验证了一种简便的液相色谱-电喷雾串联质谱（LC-ESI-MS/MS）方法，用于同时测定人血浆中卢帕他定（RT）及其两种活性代谢物，即地氯雷他定（DT）和3-羟基地氯雷他定（3-OH-DT）。采用C18柱，以甲醇和含0.1%（v/v）甲酸的10mM醋酸铵进行梯度洗脱，实现色谱分离。RT、DT和3-OH-DT的定量下限（LLOQ）分别为0.05、0.035和0.035 ng/mL。分析物的日内和日间精密度分别在1.0 - 4.7%和2.2 - 12.1%范围内。分析物的日内和日间准确度分别在-7.7%至5.2%和-4.1%至4.8%范围内。该方法成功应用于健康志愿者单次（10、20、40 mg）和多次（10 mg）口服富马酸卢帕他定片后RT及其两种代谢物DT和3-OH-DT的药代动力学研究。
