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目的:建立高效液相色谱方法,监测血清中胺碘酮及去乙基胺碘酮的血药浓度。方法:以决奈达隆为内标,血清经蛋白沉淀后采用Alltima C18色谱柱(4.6 mm×250 mm,5μm)进行分析,以乙腈-100 mmol·L~(-1)磷酸二氢钠(磷酸调pH至3.0)(55∶45)为流动相,流速1.0 mL·min~(-1),柱温30℃,检测波长241 nm。并将测定结果和薄层扫描法的测定结果进行统计分析和比较。结果:方法具有良好的专属性,血清中的内源性物质和临床常见合用药物不干扰测定;胺碘酮质量浓度在0.048~3.842μg·mL~(-1)的范围内线性良好(r=0.999 6),去乙基胺碘酮质量浓度在0.051~4.084μg·mL~(-1)的范围内线性良好(r=0.999 8);胺碘酮和去乙基胺碘酮的最低检测限均为0.02μg·mL~(-1),定量限均为0.05μg·mL~(-1);准确度和精密度良好,相对回收率和绝对回收率均在97.5%~104.2%之间,日内精密度和日间精密度均小于8.0%;稳定性良好,在室温、冻融和冷藏(2~4℃)条件下胺碘酮和去乙基胺碘酮浓度的相对误差(RE)均小于±9%。方法学比较显示:新建的HPLC法和薄层扫描法的测定结果具有良好的相关性,且无显著性差异(P>0.05),但在<0.02μg·mL~(-1)的低浓度区,2种方法有显著性差异(P<0.05),HPLC法测定结果高于薄层扫描法。结论:该方法快速、简便,易推广,可作为血清中胺碘酮及去乙基胺碘酮的血药浓度监测方法。
OBJECTIVE: To establish a HPLC method for the determination of serum amiodarone and deethionate in plasma. Methods: Dronedarone was used as an internal standard. After the protein was precipitated by serum, Alltima C18 column (4.6 mm × 250 mm, 5 μm) was used for the analysis. The concentration of acetonitrile - 100 mmol·L -1 sodium dihydrogen phosphate Phosphoric acid was adjusted to pH 3.0) (55:45) as mobile phase at a flow rate of 1.0 mL · min -1. The column temperature was 30 ℃ and the detection wavelength was 241 nm. The results of the measurement and the results of TLC were statistically analyzed and compared. Results: The method was of good specificity. The endogenous substances in serum and common clinical drugs did not interfere with the determination. The linear range of amiodarone was 0.048 ~ 3.842μg · mL ~ (-1) (r = 0.999 6). The linearity was good (r = 0.999 8) in the range of 0.051 ~ 4.084 μg · mL -1. The detection limits of amiodarone and deethionate (0.02μg · mL -1) and the limit of quantitation (LOD) were both 0.05μg · mL -1. The accuracy and precision were good. The relative and absolute recoveries were between 97.5% and 104.2% The intra-day precision and intra-day precision were less than 8.0%. The stability was good. The relative errors (REs) of amiodarone and deethionate concentrations at room temperature, freezing and thawing and cold storage (2-4 ℃) Less than ± 9%. The methodological comparison shows that there is a good correlation between the newly developed HPLC method and the TLC scanning method (P> 0.05), but in the low concentration area <0.02μg · mL -1 , There was a significant difference between the two methods (P <0.05). The results of HPLC were higher than those of TLC. Conclusion: The method is rapid, simple and easy to popularize. It can be used as a monitoring method of plasma concentration of amiodarone and deethionate in serum.