阳离子交换固相萃取-流动注射化学发光法测定肾上腺色腙

Cation exchange solid-phase extraction coupled with flow injection chemiluminescent analysis for detection of carbazochrome

目的:基于酸性高锰酸钾氧化肾上腺色腙产生微弱的化学发光现象,建立一种简单、灵敏、选择性高,可用于药物质量控制和体内药物分析的肾上腺色腙的化学发光新方法。方法:药物样品经阳离子交换固相萃取技术净化后,采用流动注射化学发光法分析。结果:方法测定肾上腺色腙的线性范围为7.0×10-10～1.0×10-7μg.mL-1,检出限为2.0×10-10μg.mL-1(3σ),对1.0×10-8μg.mL-1的样品连续进行11次平行测定,相对标准偏差为2.5%;用于肾上腺色腙注射剂测定的回收率为96%～98%,而用于尿样中加入肾上腺色腙1.00×10-7～5.00×10-9μg.mL-1,回收率为80.2%～98.6%。结论:该方法具有很高的灵敏度和较好的选择性,不但可以用于制剂的分析,还适用于血样、尿样等复杂的生物样品中极低浓度肾上腺色腙的分析。

Objective：To establish a sensitive and simple method for the determination of carbazochrome based on that carbazochrome can be oxidized by acidic potassium permanganate to produce chemiluminescence.This method should be suitable for drug quality control and in vivo pharmaceutical analysis.Method：Coupled with solid-phase extraction for sample cleaning-up,carbazochrome was detected using flow injection chemiluminescent analysis.Results：The linear range was 7.0×1.0-10-1.0×1.0-7 μg·mL-1 with a detection limit of 2.0×1.0-10 μg·mL-1（3σ）.Standard sample at the concentration of 1.0×10-8 μg·mL-1was repeatedly detected for 11 times,and a relative standard deviation of 2.5% was obtained.The recoveries for injection sample was 96%-98%,and those for urine samples spiked with carbazochrome standards at the concentrations of 1.00×10-7-5.00×10-9 μg·mL-1were 80.2%-98.6%.Conclusion：This method shows high sensitivity and good selectivity for carbazochrome detection.It can be used for assay commercial preparations as well as biological samples such as serum and urine.