基于表面活性剂荧光增强的荧光光谱法测定心得安片剂和人尿中盐酸普萘洛尔的含量  

Determination of Propranolol Hydrochloride in Propranolol Tablets and Human Urine by Fluorescence Spectrometry Based on Surfactant Fluorescence Enhancement

作　　者：谈文林 陈智[1] TAN Wenlin;CHEN Zhi(Dazhou Vocational and Technical College,Dazhou 635000,China)

机构地区：[1]达州职业技术学院,达州635000

出　　处：《理化检验（化学分册）》2024年第10期973-979,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家体育总局体育文化发展中心资助项目(19TD001);达州市科学研究“十四五”规划资助项目(DZ22D130)。

摘　　要：基于盐酸普萘洛尔(PRH)的内源荧光特性及十六烷基三甲基溴化铵(CTAB)对PRH荧光增强作用,优化了磷酸盐缓冲溶液(PBS)酸度、CTAB浓度、反应时间、激发波长、发射波长等试验条件,进行了题示研究。心得安片剂经研细、水超声分散、离心、稀释后,分取适量,加入0.1 mol·L^(-1)PBS(pH 5.8)和10μmol·L^(-1)CTAB溶液,涡旋,于室温保存2 min,在激发波长290 nm、发射波长365 nm下测量体系的荧光强度。服用心得安片剂前后的人尿经100℃保温后分取适量,按照心得安片剂溶液的步骤测试。结果显示:PRH的浓度在0.40~100μmol·L^(-1)内和体系的荧光强度呈线性关系,检出限(3s/k)为120 nmol·L^(-1);尿样中常见共存物质Cl^(-)、Na^(+)、Mg^(2+)、睾酮、Br^(-)、K^(+)、Cu^(2+)、安体舒通、Zn^(2+)、Ca^(2+)、苄硫噻嗪、双氢克尿塞对PRH无干扰;对心得安片剂和实际尿样进行3个浓度水平的加标回收试验,PRH的回收率为95.0%~105%,测定值的相对标准偏差(n=5)为0.48%~2.8%。方法用于服用心得安片剂不同时间尿样的分析,2 h时尿样中PRH浓度较高,12 h及以后PRH几乎不能检出。Based on the intrinsic fluorescence characteristics of propranolol hydrochloride(PRH)and the fluorescence enhancement effect of cetyltrimethylammonium bromide(CTAB)on PRH,test conditions such as the acidity of phosphate buffer solution(PBS),CTAB concentration,reaction time,excitation wavelength,and emission wavelength were optimized,and the research mentioned by the title was conducted.After grinding,water ultrasonic dispersion,centrifugation,and dilution of propranolol tablets,an appropriate amount was taken,and 0.1 mol·L^(−1) PBS(pH 5.8)and 10μmol·L^(−1) CTAB solution were added.The mixture was vortexed,and stored at room temperature for 2 min.The fluorescence intensity of the system was measured at an excitation wavelength of 290 nm and emission wavelength of 365 nm.Urine samples before and after taking propranolol tablets were incubated at 100℃,and an appropriate amount was taken for detection according to the steps of propranolol tablet solution.It was shown that linear relationship between values of the PRH concentration and system fluorescence intensity was kept in the range of 0.40-100μmol·L^(−1),with detection limit(3s/k)of 120 nmol·L^(−1).Commonly coexisting substances in urine samples including Cl^(−),Na^(+),Mg^(2+),testosterone,Br^(−),K^(+),Cu^(2+),spironolactone,Zn^(2+),Ca^(2+),benzthiazide,and hydrochlorothiazide did not interfere with PRH.Test for the spiked recovery was made on propranolol tablets and actual urine samples at the 3 concentration levels,giving recoveries of PRH in the range of 95.0%-105%,and RSDs(n=5)of the determined values ranged from 0.48%to 2.8%.The proposed method was used for the analysis of urine samples taking propranolol tablets for different time.The concentration of PRH in the urine sample was high at 2 h,and PRH was almost undetectable not less than 12 h.

关 键 词：盐酸普萘洛尔(PRH) 荧光增强作用 荧光光谱法 十六烷基三甲基溴化铵(CTAB) 人尿 

分 类 号：O657.32[理学—分析化学]