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

Flow-injection chemiluminescence analysis of codeine phosphate in tablets and injection by microemulsions

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0.001～15μg·mL-1,检出限(3σ)为0.03 ng·mL-1,对浓度为1.0μg·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 AuCl-4.When the ion-complexes extracted and carried by dichloromethane entered a microemulsion of cetyltrimethylammonium chlorine containing luminol,the dissociated AuCl-4 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.