HPLC-ECD测定重酒石酸去甲肾上腺素的有关物质
金薇;彭兴盛;陈阳;杨永健
【期刊名称】《药物分析杂志》 【年(卷),期】2011(031)008
【摘要】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 nn,5μm);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+0.6V.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 ~5μg·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. 【总页数】4页(1485-1488)
【关键词】肾上腺素激动药;重酒石酸去甲肾上腺素;有关物质;高效液相色谱;电化学安培检测
【作者】金薇;彭兴盛;陈阳;杨永健
【作者单位】上海市食品药品检验所,上海 201203;上海市食品药品检验所,上海 201203;第二军医大学,上海 200433;上海市食品药品检验所,上海 201203;上海市食品药品检验所,上海 201203 【正文语种】中文 【中图分类】R917 【文献来源】
https://www.zhangqiaokeyan.com/academic-journal-cn_chinese-journal-pharmaceutical-analysis_thesis/0201241367914.html
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