HPLC-ECD测定重酒石酸去甲肾上腺素的有关物质

目的: 建立重酒石酸去甲肾上腺素有关物质的高效液相色谱-电化学检测方法(HPLC-ECD)。 方法: 采用TSK C₁₈柱(150 mm×4.6 mm,5 μm);以0.05%庚烷磺酸钠溶液(用磷酸调节pH至2.2)-乙腈(925∶ 75)为流动相,玻碳圆盘电极为工作电极,银-氯化银电极为参比电极,工作电位为+0.6 V。 结果: 去甲肾上腺素、肾上腺素、去甲肾上腺酮、多巴胺和2-氯-1-(3,4-二羟基苯基)乙酮均在0.05~5 μg·mL^-1浓度范围内线性关系良好,相关系数分别为0.9998,0.9999,1.0000,0.9999,0.9994 (n=7);检测限分别为0.07,0.07,0.08,0.1和0.2 ng (S/N≥3)。4种有关物质的平均加样回收率为97.2%,100.4%,98.2%,103.1%;RSD为1.6%,1.5%,1.3%,2.8%(n=6)。 结论: 采用高效液相色谱-电化学检测法测定重酒石酸去甲肾上腺素有关物质,方法灵敏度高,选择性强,重现性好,能够用于重酒石酸去甲肾上腺素的质量控制。

Objective: To establish an HPLC-electrochemical detection (HPLC-ECD) method for the determination of norepinephrine bitartrate and its related substances. Method: An ODS column(TSK C₁₈,150 mm×4.6 mm,5 μm) was adopted with a mixture of 0.05% sodium heptanesulfonate solution (adjust to pH 2.2 with phosphoric acid)-acetontrile (925∶ 75) as mobile phase.A glassy carbon disc electrode was used as the working electrode at the potential of+0.6 V. Results: The calibration curves of norepinephrine,epinephrine,noradrenalone,dopamine,2-chloro-1-(3,4-dihydroxyphenyl) ethanone were linear in the concentration range of 0.05-5 μg.mL^-1.The detection limits were 0.07,0.07,0.08,0.1 and 0.2 ng,respectively.The average recovery of epinephrine,noradrenalone,dopamine,2-chloro-1-(3,4-dihydroxyphenyl) ethanone were 97.2%,100.4%,98.2% and 103.1% with RSD of 1.6%,1.5%,1.3% and 2.8% (n=6). Conclusion: The proposed method shows high sensitivity,repeatability and stability.It can be employed for the quality control of related substances of norepinephrine bitartrate.