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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 |
| 阅读数： | 232 次 |
| 本月下载数： | 28 次 |
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