儿科药学杂志2013,Vol.19Issue(3):25-28,4.
固相萃取-液相色谱-串联质谱法测定人血浆中卢帕他定的浓度
Determination of Rupatadine in Human Plasma by Solid Phase Extraction and LC-MS/MS
摘要
Abstract
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 mmx4.6 mm, 5 u.m) guarded by a Phemomenex Gemini Cl8 column (4 mmx3.0 mm, 10 u.m). 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 u.g/L and with the regression equation of Y=2. 883x+0.009,r = 0.999. The limit of quantification was 0.0119 u,g/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. 关键词
卢帕他定/血药浓度/液相色谱-串联质谱/固相萃取Key words
Rupatadine/ Plasma drug concentration/ LC-MS/MS/ Solid phase extraction分类
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曹靖,曾欣,周小琳..固相萃取-液相色谱-串联质谱法测定人血浆中卢帕他定的浓度[J].儿科药学杂志,2013,19(3):25-28,4.