目的:采用可调激光-微顺序注射-阀上实验室荧光反猝灭法测定硫酸氢氯吡格雷含量。方法:四苯硼钠与罗丹明B反应,荧光信号猝灭,加硫酸氢氯吡格雷后,其与四苯硼钠-罗丹明B体系中的四苯硼钠反应形成更稳定的疏水性离子缔合物,使罗丹明B重新释放出荧光,检测荧光信号的增强程度(ΔF),通过ΔF与硫酸氢氯吡格雷的浓度(C)的回归方程,计算硫酸氢氯吡格雷含量。结果:荧光信号的ΔF与硫酸氢氯吡格雷C线性回归方程为ΔF=4 471.7C+12 552,r=0.998 4,线性范围为0.7-28.2μmol·L^-1,检出下限为0.067μmol·L^-1,重复性RSD为2.9%,加样回收率在93.0%~99.5%之间。用该方法对市售硫酸氢氯吡格雷片进行测定,结果为97%-100%。结论:该方法可用于测定药物中硫酸氢氯吡格雷含量。
Objective: To analyze elopidogrel hydrogen sulfate by fluorescence quenching method in the laboratory of a tunable laser micro sequential injection valve ( MicroSIA Lab-on-valve, ^18SIA-LOV ) method. Methods: Rhodamine B had fluorescence quenching effect at stable conformation with sodium tetraphenylboron. When clopidogrel hydrogen sulfate reacted with sodium tetraphenylboron to form a more stable hydrophobic ion association complex, rhodamine B was released and fluorescence intensity of solution was enhanced ( △F ). The fluorescence signal enhancement A F had good linearity with the concentration ( C ) of clopidogrel hydrogen sulfate. Results: the linearity equation of this method was A F=4 471.7C+12 552, r=0.998 4, the range was 0.7-28.2 μmol · L-1, detection limit was 0.067 μmol · L-1, the RSD of this method was 2.9%, and the standard added recovery rates were between 93.0%-99.5%. This method was applied to the quantitative analysis of commercially clopidogrel bisulfate tablets. The results were 97%-100%. Conclusion: This method can be used for quality control of clopidogrel hydrogen sulfate.