毛细管微萃

发布时间：2018-03-07 02:39

本文选题：异丙酚　切入点：毛细管微萃取　出处：《新疆医科大学》2016年硕士论文　论文类型：学位论文

【摘要】：目的:建立异丙酚生物样品在线前处理系统及分析方法。方法:1.利用两相溶剂体系在螺旋管内建立起一种特殊的单向性流体动力学平衡,建立毛细管微萃取的异丙酚生物样品在线前处理方法,并对毛细管微萃取系统进行影响因素的考察。并将毛细管微萃取系统与荧光光谱法结合用于测定生物样品中异丙酚含量。2.将毛细管微萃取系统与光纤传感紫外分光光度法结合用于测定生物样品中异丙酚的含量。3.将毛细管微萃取系统与光纤传感微顺序注射-阀上实验室系统(Micro Sequential Injection lab-on-valve,μSIA-LOV)结合,并用于异丙酚的衍生化实验。结果:1.毛细管微萃取结合荧光光谱法测定全血中异丙酚含量的实验:以荧光强度为主要考察指标,毛细管微萃取系统最佳萃取条件分别为:毛细管的最佳长度为1.00m,最优直径为0.762mm,最佳打出流速为50μL/s,在毛细管中最优停留时间为1.0min,最佳静置时间是1.0min,选用5.0m L的环己烷做萃取剂,1.0m L的甲醇做蛋白沉淀剂。异丙酚的血药浓度在0.05~10.0μg/m L内线性良好(r=0.9958);高(7.5μg/m L)、中(2.5μg/m L)、低(0.25μg/m L)3个浓度的平均提取回收率平均在92.34%~96.33%之间,相对标准偏差(RSD)均10%;日内、日间RSD均15%。2.毛细管微萃取系统结合光纤传感紫外分光光度法测定生物样品中异丙酚含量的实验:异丙酚的血药浓度在16.0~60.0μg/m L内线性良好(r=0.9988),定量限为16.0μg/mL;低(20.0μg/m L)、中(30.0μg/m L)、高(60.0μg/m L)3个浓度的提取回收率均在91.4%~95.38%之间,低、中、高3个浓度的平均日内精密度RSD分别为8.70%8.60%和4.60%,平均日间精密度RSD分别为10.10%8.20%和5.10%。3.异丙酚在毛细管微萃取-光纤传感微顺序注射-阀上实验室系统上衍生化实验:异丙酚血药浓度在3.0~18.0μg/mL内线性良好(r=0.9975),定量限为3.0μg/m L;低、中、高3个浓度(6.0,12.0,18.0μg/mL)的日内精密度RSD分别为6.8%6.5%和10.7%,日间精密度RSD分别为5.7%8.8%和6.8%,平均回收率在91.0%~97.8%之间。结论:1.毛细管微萃取方法作为样品前处理技术更加方便、简单、省时省力,并且该系统可以用软件控制自动完成,为异丙酚在线前处理提供了一种新方法。2.毛细管微萃取系统结合荧光光谱法测定全血样品中异丙酚含量,方法简单,灵敏度高还可以排除全血中杂质的干扰。3.毛细管微萃取系统结合光纤传感紫外分光光度法测定全血样品中异丙酚含量,检测时间短,样品用量少。为异丙酚血药浓度在线检测提供了可能性。4.将异丙酚在毛细管微萃取-光纤传感微顺序注射-阀上实验室系统衍生化,大大提高了检测的灵敏度,而且,通过检测衍生化产物可以有效避免全血中内源性物质的干扰。
[Abstract]:Objective: to establish an on-line pretreatment system for propofol biological samples and its analytical method. Methods: 1. To establish a special unidirectional hydrodynamic equilibrium in helical tube by using two-phase solvent system. An on-line pretreatment method for propofol biological samples by capillary microextraction was established. The influence factors of capillary microextraction system were investigated, and the capillary microextraction system was combined with fluorescence spectrometry to determine propofol content in biological samples. The capillary microextraction system was combined with optical fiber sensing ultraviolet spectrum to determine propofol content in biological samples. The content of propofol in biological samples was determined by spectrophotometry. The capillary microextraction system was combined with the optical fiber sensing microsequence-injection-on-valve (渭 SIA-LOV) system, which was used for the determination of propofol in biological samples. Results: 1. Capillary microextraction combined with fluorescence spectrometry for the determination of propofol in whole blood. The optimum extraction conditions of capillary microextraction system are as follows: the optimum length of capillary is 1.00 m, the optimum diameter is 0.762mm, the optimal flow rate is 50 渭 L / s, the optimal residence time is 1.0 min, the optimal stalling time is 1.0 min, and the optimum setting time is 1.0 min. The plasma concentration of propofol was 0.05 ~ 10.0 渭 g / mL and the average recovery of propofol was 96.33% in the concentration of 7.5 渭 g / mL, 2.5 渭 g / mL, 0.25 渭 g 路mL ~ (-1), respectively, and the concentration of propofol was 0.05 ~ 10.0 渭 g / m ~ (-1) in the range of 0.05 ~ 10.0 渭 g 路ml ~ (-1), 0.9958 渭 g / m ~ (-1). Relative standard deviations (RSDs) are 10. The experiment of determining propofol content in biological samples by capillary microextraction system combined with optical fiber sensing ultraviolet spectrophotometry: the plasma concentration of propofol is 16.0 ~ 60.0 渭 g / mL, the limit of quantification is 16.0 渭 g 路mL ~ (mL), the content of propofol is 20.0 渭 g / mL, the concentration of propofol is 30.0 渭 g / mL 路mL ~ (-1), the concentration of propofol is 0.9988 渭 g / mL, the limit of quantification is 16.0 渭 g / mL, and the limit is 16.0 渭 g / mL. The recoveries of the three concentrations were 91.4 渭 g / mL and 95.38%, respectively. The average intraday precision (RSD) of three concentrations of low, medium and high concentrations was 8.70? 8.60% and 4.60, the average day precision RSD is 10. 10? 8.20% and 5.10.3. Derivatization of propofol in capillary microextraction, optical fiber sensing microsequential injection-on-valve laboratory system: propofol concentration in the plasma of 3.0 ~ 18.0 渭 g / mL with a good linearity of 0.9975 渭 g / mL with a quantitative limit of 3.0 渭 g / mL. The intra day precision (RSD) of the three concentrations of 6.0g / mL was 6.8g / mL and 12.0 渭 g / mL, respectively. 6.5% and 10.7, respectively, the daytime precision RSD is 5. 7? The average recoveries of 8.8% and 6.8 were between 91.0% and 97.8%. Conclusion: 1. Capillary microextraction is more convenient, simple, time-saving and labor-saving as a sample pretreatment technique, and the system can be automatically completed by software control. A new method for on-line pretreatment of propofol was provided. The capillary microextraction system combined with fluorescence spectrometry was used to determine propofol content in whole blood samples. The high sensitivity can also eliminate the interference of impurities in whole blood .3.The capillary microextraction system combined with optical fiber sensing ultraviolet spectrophotometry for the determination of propofol in whole blood samples, the detection time is short. It provides the possibility for on-line detection of propofol concentration. 4. Derivatization of propofol in capillary microextraction-optical fiber sensing microinjection-valve system can greatly improve the sensitivity of the detection. The detection of derivative products can effectively avoid the interference of endogenous substances in whole blood.
【学位授予单位】：新疆医科大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：R917

【相似文献】