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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 chemiluminescence immunoassay for adrenopyrazone based on acidic potassium permanganate oxidation, and to establish a simple, sensitive and selective method for the chemiluminescence of the adrenal hydrazone, which can be used for drug quality control and in vivo drug analysis. Methods: The drug samples were purified by cation exchange solid-phase extraction and analyzed by flow injection chemiluminescence. Results: The linear range of this method was 7.0 × 10-10 ~ 1.0 × 10-7μg.mL-1, the detection limit was 2.0 × 10-10μg.mL-1 (3σ), and the linear range of 1.0 × 10-8μg .mL-1 samples for 11 consecutive parallel determination, the relative standard deviation of 2.5%; for the determination of adrenal hydrazone injection recovery rate of 96% to 98%, and for the urine sample was added adrenylhydrazone 1.00 × 10 -7 ~ 5.00 × 10-9μg.mL-1, the recovery rate was 80.2% ~ 98.6%. Conclusion: This method has high sensitivity and good selectivity. It can not only be used for the analysis of preparations, but also for the analysis of very low concentrations of adrenochromes in complex biological samples such as blood samples and urine samples.