本文選題：異丙酚　切入點：毛細管微萃取　出處：《新疆醫(yī)科大學》2016年碩士論文　論文類型：學位論文

【摘要】：目的:建立異丙酚生物樣品在線前處理系統及分析方法。方法:1.利用兩相溶劑體系在螺旋管內建立起一種特殊的單向性流體動力學平衡,建立毛細管微萃取的異丙酚生物樣品在線前處理方法,并對毛細管微萃取系統進行影響因素的考察。并將毛細管微萃取系統與熒光光譜法結合用于測定生物樣品中異丙酚含量。2.將毛細管微萃取系統與光纖傳感紫外分光光度法結合用于測定生物樣品中異丙酚的含量。3.將毛細管微萃取系統與光纖傳感微順序注射-閥上實驗室系統(Micro Sequential Injection lab-on-valve,μSIA-LOV)結合,并用于異丙酚的衍生化實驗。結果:1.毛細管微萃取結合熒光光譜法測定全血中異丙酚含量的實驗:以熒光強度為主要考察指標,毛細管微萃取系統最佳萃取條件分別為:毛細管的最佳長度為1.00m,最優(yōu)直徑為0.762mm,最佳打出流速為50μL/s,在毛細管中最優(yōu)停留時間為1.0min,最佳靜置時間是1.0min,選用5.0m L的環(huán)己烷做萃取劑,1.0m L的甲醇做蛋白沉淀劑。異丙酚的血藥濃度在0.05~10.0μg/m L內線性良好(r=0.9958);高(7.5μg/m L)、中(2.5μg/m L)、低(0.25μg/m L)3個濃度的平均提取回收率平均在92.34%~96.33%之間,相對標準偏差(RSD)均10%;日內、日間RSD均15%。2.毛細管微萃取系統結合光纖傳感紫外分光光度法測定生物樣品中異丙酚含量的實驗:異丙酚的血藥濃度在16.0~60.0μg/m L內線性良好(r=0.9988),定量限為16.0μg/mL;低(20.0μg/m L)、中(30.0μg/m L)、高(60.0μg/m L)3個濃度的提取回收率均在91.4%~95.38%之間,低、中、高3個濃度的平均日內精密度RSD分別為8.70%8.60%和4.60%,平均日間精密度RSD分別為10.10%8.20%和5.10%。3.異丙酚在毛細管微萃取-光纖傳感微順序注射-閥上實驗室系統上衍生化實驗:異丙酚血藥濃度在3.0~18.0μg/mL內線性良好(r=0.9975),定量限為3.0μg/m L;低、中、高3個濃度(6.0,12.0,18.0μg/mL)的日內精密度RSD分別為6.8%6.5%和10.7%,日間精密度RSD分別為5.7%8.8%和6.8%,平均回收率在91.0%~97.8%之間。結論:1.毛細管微萃取方法作為樣品前處理技術更加方便、簡單、省時省力,并且該系統可以用軟件控制自動完成,為異丙酚在線前處理提供了一種新方法。2.毛細管微萃取系統結合熒光光譜法測定全血樣品中異丙酚含量,方法簡單,靈敏度高還可以排除全血中雜質的干擾。3.毛細管微萃取系統結合光纖傳感紫外分光光度法測定全血樣品中異丙酚含量,檢測時間短,樣品用量少。為異丙酚血藥濃度在線檢測提供了可能性。4.將異丙酚在毛細管微萃取-光纖傳感微順序注射-閥上實驗室系統衍生化,大大提高了檢測的靈敏度,而且,通過檢測衍生化產物可以有效避免全血中內源性物質的干擾。
[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.
【學位授予單位】：新疆醫(yī)科大學
【學位級別】：碩士
【學位授予年份】：2016
【分類號】：R917

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