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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 determine the content of clopidogrel hydrogen sulphate by adjustable laser - micro-order injection - on-valve laboratory anti-quenching fluorescence spectrometry. METHODS: Sodium tetraphenylborate reacted with rhodamine B, quenched by fluorescence signal and treated with clopidogrel bisulfate, which reacted with sodium tetraphenylborate in sodium tetraphenylborate-rhodamine B system to form more stable hydrophobic ions The association substance, Rhodamine B re-release of fluorescence, detection of fluorescence signal enhancement (ΔF), ΔF and clopidogrel hydrogen sulfate concentration (C) of the regression equation to calculate the clopidogrel hydrogen sulfate content. Results: The linear regression equation of ΔF of fluorescent signal and clopidogrel bisulfate C was ΔF = 4 471.7C + 12 552, r = 0.998 4, linear range was 0.7 ~ 28.2μmol·L -1, and the detection limit was 0.067μmol·L -1, the repeatability of RSD was 2.9%, and the recoveries of samples ranged from 93.0% to 99.5%. This method was used to determine the commercial clopidogrel hydrogen sulfate tablets, the results were 97% to 100%. Conclusion: This method can be used to determine the content of clopidogrel hydrogen sulfate in the drug.