可调激光光源-微顺序注射联用技术在药物含量测定中的应用

发布时间：2018-10-16 20:42

【摘要】：目的:建立可调激光-微顺序注射-阀上实验室荧光反猝灭法在线监测叔胺类药物含量的方法。方法:四苯硼钠对罗丹明B和亚甲基蓝的荧光信号有猝灭作用,而硫酸氢氯吡格雷,利血平,盐酸尼卡地平和盐酸丙咪嗪等药物分子中的叔胺结构质子化后,与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和亚甲基蓝重新释放出荧光,且荧光信号的增强程度(△F)与这些药物的浓度成线性关系。根据上述原理,采用可调激光-光纤传感技术,建立一种荧光反猝灭法间接测定结构含有叔胺的药物含量的方法。结果:1.荧光信号的增强程度△F与硫酸氢氯吡格雷浓度线性回归方程为△F=4471.7C+12552,r=0.9984,线性范围为(0.07~2.82)×10-5 mol·L-1,检出下限为0.67×10-6mol·L-1,重复性RSD为2.94%,加标回收率在93.0%~99.5%之间。2.荧光信号的增强程度△F与利血平浓度线性回归方程为△F=11791C+278.87,r=0.9986,线性范围为(0.048~1.16)×10-5 mol·L-1,检出下限为0.1×10-6 mol·L-1,重复性RSD为0.58%,加标回收率在95.1%~99%之间。3.荧光信号的增强程度△F与盐酸尼卡地平浓度线性回归方程为△F=2827C+608.41,r=0.9991,线性范围为(0.047~4.97)×10-5 mol·L-1,检出下限为0.31×10-6 mol·L-1,重复性RSD为1.24%,加标回收率在93.8%~102%之间。4.荧光信号的增强程度△F与盐酸丙咪嗪浓度线性回归方程为△F=3574C+667.74,r=0.9995,线性范围为(0.078~3.99)×10-5 mol·L-1,检出下限为0.52×10-6 mol·L-1,重复性RSD为0.45%,加标回收率在94.5%~97.2%之间。用该方法对市售药品进行测定,测定值与药品标示值基本相符。结论:该方法简便易行,高效迅速,可用于测定叔胺类药物中有效成分的含量。
[Abstract]:Aim: to establish a method for on-line monitoring the content of tertiary amines by adjustable laser-microsequential injection-on-valve laboratory fluorescence reverse quenching method. Methods: sodium tetraphenylboron had a quenching effect on fluorescence signals of Rhodamine B and methylene blue, while the tertiary amine structures of clopidogrel sulfate, reserpine, nicardipine hydrochloride and imipramine hydrochloride were protonated. A more stable hydrophobic ion-association complex was formed by reaction with sodium tetraphenylboron. Rhodamine B and methylene blue released fluorescence again, and the enhancement of fluorescence signal (F) was linearly related to the concentration of these drugs. Based on the above principle, an indirect fluorescence quenching method for the determination of the content of drugs containing tertiary amines was established by means of tunable laser-fiber sensing technology. The result is 1: 1. The linear regression equation between fluorescence signal enhancement F and clopidogrel sulfate concentration is F 4471.7C 12552rn 0.9984, the linear range is (0.07 ~ 2.82) 脳 10 ~ (-5) mol L ~ (-1), the detection limit is 0.67 脳 10-6mol L ~ (-1), the repeatability RSD is 2.94, and the recovery rate is between 93.099.5% and 99.5%. The linear regression equation between the enhancement of fluorescence signal F and the concentration of reserpine was F 11791C 278.87 ru 0.9986, the linear range was (0.048 ~ 1.16) 脳 10 ~ (-5) mol L ~ (-1), the detection limit was 0.1 脳 10 ~ (-6) mol L ~ (-1), the repeatability RSD was 0.58%, and the recovery was between 95.199% and 0.3%. The linear regression equation between the enhancement of fluorescence signal F and the concentration of nicardipine hydrochloride was F 2827C 608.41C 0.9991, the linear range was (0.04744.97) 脳 10-5 mol L-1, the detection limit was 0.31 脳 10-6 mol L-1, the reproducibility RSD was 1.240.The recoveries of standard addition were in the range of 93.8102wt%. The linear regression equation between the intensity of fluorescence signal F and the concentration of imipramine hydrochloride is F 3574C 667.74 ru 0.9995, the linear range is (0.078 ~ 3.99) 脳 10 ~ (-5) mol L ~ (-1), the detection limit is 0.52 脳 10 ~ (-6) mol L ~ (-1), the reproducibility RSD is 0.45%, and the recovery rate is between 94.552% and 97.2%. The method was used to determine the marketable drugs, and the determination value was basically consistent with the drug label value. Conclusion: this method is simple and rapid, and can be used for the determination of effective components in tertiary amines.
【学位授予单位】：新疆医科大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.3;R927.2

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