高效液相色谱法测定卡马西平血药的浓度

Determination of Plasma Carbamazepine Concentrations by HPLC

目的对高效液相色谱法(HPLC)测定人血浆中卡马西平(CBZ)血药浓度进行探讨。方法血清样品经甲醇沉淀后,以甲醇水=5446为流动相,流速为1.0mL.min-1,色谱柱为Agilent HC-C18(4.6mm×150mm,5μm),柱温为30℃,紫外检测波长为285nm。结果该法专属性较好,血浆中杂质不干扰样品峰的测定;CBZ在1.0～40.0μg.mL-1质量浓度范围内线性关系良好,定量下限为1.0μg.mL-1;批内、批间精密度RSD均小于15%,准确度RE均小于15%;血浆样品室温放置6h、-20℃冷冻2周反复冻融3次,其处理后样品在自动进样器中放置6h稳定性均较好;方法学质控测定亦符合相关规定。结论 HPLC灵敏、快速、准确,操作简便、线性范围宽,可用于CBZ的血药浓度监测。

Objective To determine the plasma concentrations of carbamazepine using HPLC.Methods Serum samples were precipitated with methanol and separation was carried out on Agilent HC-C18 column（4.6 mm×150 mm,5 μm）at 30 ℃.The mobile phase consisted of methanol-water（54：46） at a flow-rate of 1.0 mL·min-1.The detection wavelength was 285 nm.Results The method had a good specificity.Plasma impurities did not interfere with the determination of the analyte.The linearity was good in the concentration range from 1.0 to 40.0 μg·mL-1 and the lowest limit of quantification was 1.0 μg·mL-1.The precision and accuracy（RSD,%） within batches and between batches were both less than 15%.Serum samples had a good stability after placement at room temperature for 6 hours,freezer storage（-20 ℃） for 2 weeks and repeated freezing and thawing 3 times,and placement in the auto-sampler for 6 hours.Methodological quality control complied with relevant provisions.Conclusion HPLC method is sensitive,fast,accurate and simple for monitoring plasma carbamazepine concentrations with a wide liner range.