在线二维柱切换-高效液相色谱法测定人血清中多索茶碱浓度
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篇名: 在线二维柱切换-高效液相色谱法测定人血清中多索茶碱浓度
TITLE:
摘要: 目的:建立测定人血清中多索茶碱浓度的方法。方法:采用在线二维柱切换-高效液相色谱法测定人血清中多索茶碱浓度,一维色谱柱为Waters C18,中间柱为SC2,一维、二维柱流动相均为甲醇-水(70 ∶ 30,V/V),检测波长为273 nm,柱温为40 ℃,进样量为10 μL。结果:多索茶碱在0.5~50.00 μg/mL质量浓度范围内与峰面积线性关系良好(r=0.999 9),检测限为0.01 μg/mL,定量限为0.5 μg/mL,日内、日间精密度的RSD分别为1.51%~1.89%和1.52%~1.92%(n=5),准确度为97.91%~104.19%(n=5),提取回收率为91.63%~93.44%(RSD<2.00%,n=3),基质效应RSD≤3.01%(n=6),稳定性的RSD<5.00%(n=6)。3例患者静脉输注多索茶碱葡萄糖注射液(0.3 g/d)达稳态后,次日给药前静脉血清中多索茶碱的浓度为3.23、3.35、3.68 μg/mL,RSD为2.28%、2.34%、2.14%(n=5)。结论:该方法简便、快速、准确,适用于临床多索茶碱的血药浓度检测。
ABSTRACT: OBJECTIVE: To establish the method for the determination of doxofylline in human serum. METHODS: Online two-dimensional column switching-HPLC was adopted to determine the concentration of doxofylline in human serum. First- dimensional chromatographic column was Waters C18 column, and middle column was SC2. First-dimensional and second- dimensional column mobile phrase were methanol-water (70 ∶ 30, V/V). The detection wavelength was 273 nm, and column temperature was 40 ℃. Sample volume was 10 μL. RESULTS: The linear range of doxofylline were 0.5-50.00 μg/mL (r=0.999 9), and the detection limit was 0.01 μg/mL. The quantitative limit was 0.5 μg/mL. RSDs of intra-day and inter-day were 1.51%-1.89% and 1.52%-1.92% (n=5). The accuracy were 97.91%-104.19% (n=5). Extraction recoveries rate were 91.63%-93.44%(RSD<2.00%,n=3). RSD of matrix effect were lower than or equal to 3.01% (n=6), and RSD of stability test was lower than 5.00% (n=6). After 3 patients were given intravenous injection of Doxofylline and glucose injection(0.3 g/d) up to steady state, the serum concentrations of doxofylline were 3.23, 3.35, 3.68 μg/mL before medication on the next day (RSD=2.28%, 2.34%, 2.14%, n=5). CONCLUSIONS: The method is simple, rapid, accurate and suitable for the determination of plasma concentration of doxofylline.
期刊: 2018年第29卷第9期
作者: 郑玲利,袁明勇,蒋婷,王峰,张维,陈静
AUTHORS: ZHENG Lingli,YUAN Mingyong,JIANG Ting,WANG Feng,ZHANG Wei,CHEN Jing
关键字: 多索茶碱;血药浓度;在线二维柱切换-高效液相色谱法
KEYWORDS: Doxofylline; Plasma concentration; Online two-dimensional column switching-HPLC
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