| Objective:A biological sample online pretreatment system and an analytical method for propofol were established.Method:1.Firstly,a special one-way hydrodynamic balance in a spiral tube through a two-phase solvent system was established.And related influencing factors of the micro-capillary extraction(MCE) system were observed and studied.Then the MCE system was combined with fluorescence spectroscopy for determination of propofol in biological sample.2.MCE-Fiber Optic Sensing System was combined with UV spectrophotometry for determination of propofol in biological sample.3.MCE system and micro sequential injection-valve laboratory systems(μSIA-LOV) were combined for derivatization experiments of propofol.Results:1.Determination of propofol in whole blood via Capillary Microextraction combined with Fluorescence Spectrometry:The fluorescence intensity served as the main index.The optimum extraction conditions of MCE system were:the optimum capillary length was 1.00 m,the optimum diameter of 0.762 mm,the optimal flow rate of 50μL/s,the capillary optimal residence time was 1.0min and the best holding time was 1.0min. 5.0m L of cyclohexane was chosen as extractant and 1.0mL of methanol as protein precipitant.Blood concentration of propofol in the range of 0.05~10.0μg/m L showed good linearity(r=0.9958),average recoveries were between 92.34% to 96.33% within the range of concentrations of 7.5μg/mL, 2.5μg/mL, 0.25μg/mL. The RSD of average recovery rate was less than 10%,RSDs of within-day and between-day were both lower than 15%.2.MCE system combined optical fiber sensing UV spectrophotometry to detect propofol in biological sample:Propofol in the 16.0~60.0μg/m L had good linearity(r=0.9988).The quantification limit was 16.0μg/mL,Concentrations of 20.0μg/m L,30.0μg/m L,60.0μg/mL,the spike recovery of which was founded to be in the range of 91.4%-95.38%.RSDs of intraday precision were 8.7%,8.6% and 4.6%.RSDs of day to day precision were 10.1%,8.2% and 5.1%;3.Propofol derivatization experiments through MCE system and μSIA-LOV:Propofol of 3.0~18.0μg/m L showed good linearity(r=0.9975),quantitative limit was 3.0μg/m L,RSDs of intraday precision were 6.8%,6.5% and 10.7% with concentrations of 6.0,12.0,18.0μg/m L,RSD of day to day precision were 5.7%,8.8% and 6.8%,The average recovery was 91.0%~97.8%.Conclusions:1.MCE method is used as sample pre-treatment technology because it is more convenient,simpler,time-saving,and the system can be controlled automatically by the software.2.Detection of propofol in whole blood sample via MCE system combined with fluorescence spectrometry,which is simple and has high sensitivity,can also exclude interference of impurities in whole blood.3.MCE system coupled with optical fiber sensing UV spectrophotometry uses shorter time and smaller amount of sample,offering the possibility of online testing for propofol.4.Propofol was derivatized through MCE-fiber sensing-μSIA-LOV systems,greatly improving the detection sensitivity,and interference caused by endogenous substances can be effectively avoided by detecting the derivative. |
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