流动注射微乳液化学发光法测定片剂和注射剂中磷酸可待因的含量

目的: 建立测定磷酸可待因的化学发光快速分析方法。 方法: 在酸性条件下,磷酸可待因被质子化后与阴离子AuCl₄^-形成离子缔合物,该缔合物被二氯甲烷带入鲁米诺的十六烷基三甲基氯化铵(CTAC)微乳液中,离解出来的AuCl₄^-立即与鲁米诺产生化学发光。在一定浓度范围内,发光强度与磷酸可待因的含量成线性关系,从而间接测定磷酸可待因的含量。 结果: 在优化的试验条件下,磷酸可待因的检测线性范围为 0.001~15 μg·mL^-1,检出限(3σ)为 0.03 ng·mL^-1,对浓度为1.0 μg·mL^-1 的磷酸可待因进行11次平行测定,其RSD为1.2%。 结论: 该法快速、简便,已成功用于片剂、针剂和尿样中磷酸可待因的测定。

Objective: Chemiluminescence method was developed for determination of Codeine phosphate. Methods: In acidic condition,codeine phosphate was easily protonated and formed ion-complexes with AuCl₄^-.When the ion-complexes extracted and carried by dichloromethane entered a microemulsion of cetyltrimethylammonium chlorine containing luminol,the dissociated AuCl₄^- reacted with luminol and produced chemiluminescnece signal.In certain concentration range,the chemiluminescnece intensities were proportional to the concentration of codeine phosphate,and then the codeine phosphate was determined indirectly. Results: On the optimum conditions,the linear range was 0.001 to 15 μg·mL^-1 and the detection limit was 0.03 ng·mL^-1 with a relative standard deviation (n=11) of 1.2% for 1.0 μg·mL^-1 codeine phosphate. Conclusion: The method is simple,rapid.and has been applied to the determination of codeine phosphate in tablets,injections and urine samples successfully.