摘要
目的:建立人血浆中卢帕他定浓度的液相色谱-串联质谱(LC/MS/MS)检测方法。方法:以氯雷他定为内标,血浆样本经0.1 mol/L氢氧化钠碱化后用固相小柱萃取处理;分析柱为Kromasil C18柱(150 mm×4.6 mm,5μm),保护柱为PhenomenexGemini C18柱(4 mm×3.0 mm,10μm),流动相为甲醇-10 mmol/L甲酸铵水溶液(85∶15);使用电喷雾离子源(ESI),正离子多反应监测(MRM)方式进行检测。结果:每个样本分析时间为5 min,血浆中内源性物质对测定无干扰,卢帕他定线性范围为0.011 9～15.000 0μg/L,回归方程Y=2.883X+0.009,r=0.999,定量下限为0.011 9μg/L。日内、日间精密度(RSD)均小于10%,卢帕他定与内标的平均回收率分别为102.0%和104.1%,平均基质效应为103.7%和106.2%,且均不存在浓度依赖性。结论:本方法特异性强,灵敏度高,测定结果可靠,适用于临床试验中血浆样本的高通量分析。
Objective： To establish LC-MS/MS method for the determination of rupatadine in human plasma by using a solid phase extraction technique. Methods： Loratadine was used as internal standard and plasma samples were alkalified by 0. 1 mol/L sodium hydroxide solution, and were extracted with solid phase extraction. The extractive was separated on a Kromasill C18 analytical column （150 mm×4.6 mm, 5μm） guarded by a Phemomenex Gemini C18 column （4 mm×3.0 mm, 10μm）. The mobile phase consisted of methanol-10 mmol/L ammonium formate （85 ： 15, v/v）. Electrospray ionization （ESI） source was applied and operated in the positive multiple reactions monitoring （ MRM ） mode. Results： Each analysis was completed within five minutes. Chromatogram showed no endogenous interfering peaks with blank samples. Good linearity was found within 0. 0119 - 15. 0000 p.g/L and with the regression equation of Y= 2. 883X＋0. 009, r = 0. 999. The limit of quantification was 0.0119 μg/L. The inter-and intra-day precision （RSD） were both less than 10%. The average recovery of rupatadine and loratadine were 102.0% and 104.1%, respectively. The average matrix effects of rupatadine and loratadine were 103.7% and 106.2% respectively, in which no concentration dependences were observed. Conclusions： The method is specific, sensitive and accurate, so it is suitable for the determination of rupatadine in human plasma of clinical samples.
出处
《儿科药学杂志》
CAS
2013年第3期25-28,共4页
Journal of Pediatric Pharmacy
