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目的:用正交试验设计法优化测定小鼠脑组织中1,3-二苯-1,3-丙二酮含量的实验条件,提高测定方法的灵敏度。方法:运用基团贡献法筛选萃取剂,然后采用正交试验设计法优化实验条件。结果:乙酸乙酯/Triton X-100(90:10,v/v)是小鼠脑中1,3-二苯-1,3-丙二酮的最优萃取剂。当萃取剂体积为400μl,Triton X-100所占体积比为20%,萃取时间为3 min,离心时间为4 min,定容溶液中水所占体积比为10%时,萃取效率最高。在上述最优的实验条件下测定DPPD的定量下限为2μg/ml;加标回收率为103.5%~112.0%;日内和日间精密度测定结果的相对标准偏差多小于10%。结论:正交试验设计法对测定小鼠脑中1,3-二苯-1,3-丙二酮含量的实验条件的优化效果令人满意,建立的检测方法能够很好地满足实际测定的需求。
OBJECTIVE: To optimize the experimental conditions for the determination of 1,3-diphenyl-1,3-propanedione in brain tissue of mice by orthogonal test design and to improve the sensitivity of the assay. Methods: The group contribution method was used to screen extractant, and then the orthogonal design was used to optimize the experimental conditions. Results: Ethyl acetate / Triton X-100 (90: 10, v / v) was the optimal extractant of 1,3-diphenyl-1,3-propanedione in mouse brain. When the extractant volume was 400μl, the volume ratio of Triton X-100 was 20%, the extraction time was 3 min, the centrifugation time was 4 min and the volume ratio of water in constant volume solution was 10%, the extraction efficiency was the highest. The lower limit of quantification (DPPD) was 2μg / ml. The recoveries were 103.5% -112.0%. The relative standard deviations (RSDs) of intra-day and inter-day precision were less than 10%. Conclusion: The orthogonal test design method for the determination of mouse brain 1,3-diphenyl-1,3-propanedione content optimization of the experimental results satisfactory, the established detection method can well meet the actual measured demand.