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高效液相色谱法测定血清茶碱
HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC ASSAY OF THEOPHYLLINE IN SERUM
【摘要】 介绍高效液相色谱测定血清茶碱浓度的方法。血清内茶碱用氯仿/异丙醇(95/5,含内标剂β—羟乙基茶碱)提取,蒸干,用甲醇重溶后在Shim—pack CLC-ODS柱(6mm×15cm)上,以醋酸盐缓冲液(10mmol/L,pH4.0)/乙腈/甲醇(83/9/8)作流动相,流速1ml/分进行分析。从茶碱和内标剂峰面积比定量。本法的分析回收率平均为100.1%(范围95,8%~106.8%)。批内CV分别为2.6%(x=4.125mg/L)、1.7%(x=8.73mg/L)和1.0%(x=19.967mg/L),批间CV2.8%(x=8.91mg/L)。血清茶碱浓度在0~40mg/L范围内呈线性,回归方程y=0.0483x-0.0053。检测下限为0.3mg/L(信号/噪声=3)。常用解热镇痛药和常用镇静药无干扰。
【Abstract】 A method for measuring concentration of theophylline in serum by high-performanceliquid chromatography (HPLC) is described. Theophylline was extracted from serum by a mixture ofchroloform /iso-propyl alcohol (95/5, by vol) containing β-hydroxyethyl-theophylline as an internalstandard, and analyzed isocratically on a Shim-pack CLC-ODS column (6mm I. D.×15cm) with a mobilephase of acetate buffer (10mmol/L, PH4.0) /acetonitrile /methanol (83/9/8, by vol), at a flow rate of1.0 ml/L. Theophylline was quantiated by peak area ratio of theophylline and internal standard. Theaverage analytical recovery was 100.1% with a range from 95.8% to 106.8%. Interassay CVs were2.6% (X=4.125 mg/L), 1.7% (X=8.73 mg/L) and 10.% (X=19.967mg/L) respectively,andintraassay CV was 2.8% (8.91mg/L). Concentrations (X) and peak area ratios(Y) lineraily relatedover 0 to 40 mg/L range with a linear regression equation of y=0.0448x-0.0053 (r=0.9999). Thedetection limit (defined as a signal-to-noise ratio of 3) was 0.3 mg/L. Other drug possibleinterference were studied.
- 【文献出处】 承德医学院学报 ,Journal of Chengde Medical College , 编辑部邮箱 ,1993年03期
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