北京大学学报(医学版) ›› 2015, Vol. 47 ›› Issue (3): 541-547. doi: 10.3969/j.issn.1671-167X.2015.03.031

• 技术方法 • 上一篇    下一篇

高效液相色谱法测定小鼠脑组织中2,4二羟基二苯甲酮

王一超1, 孙艺1, 崔蓉1△, 李园利2, 张宝旭2   

  1. (北京大学公共卫生学院 1.劳动卫生与环境卫生学系,2.毒理学系,北京100191)
  • 出版日期:2015-06-18 发布日期:2015-06-18

Determination of 2,4-dihydroxybenzophenone in mouse brain by high performance liquid chromatography

WANG Yi-chao1, SUN Yi1, CUI Rong1△, LI Yuan-li2, ZHANG Bao-xu2   

  1. (1.Department of Occupational and Environmental Health Sciences, 2.Department of Toxicology, Peking University School of Public Health, Beijing 100191, China)
  • Online:2015-06-18 Published:2015-06-18

摘要: 目的:建立和优化小鼠脑组织中2,4-二羟基二苯甲酮(2,4-dihydroxybenzophenone,BP-1)的测定方法。方法:采用正交试验设计优化样品预处理条件,Waters Symmetry®C18(4.6 mm×250 mm,5 μm)色谱柱分离,等度洗脱,流动相为含3%(体积分数)乙酸的甲醇-水(体积比为3∶1),pH为3.40,流速为1.0 mL/min,紫外检测器检测,检测波长为290 nm,高效液相色谱法测定小鼠脑组织中BP-1,保留时间定性,以内标法定量。结果:在优化的实验条件下,BP-1在0.2~10.0 mg/L浓度范围内线性关系良好,相关系数为0.999 8;BP-1的加标回收率为96.8%~104.5%;日内和日间精密度分别为3.5%~5.7%和4.5%~6.4%;低、中、高3种浓度BP-1的提取回收率分别为90.5%、89.5%和97.7%;低、中、高3种浓度BP-1的基质效应分别为102.9%、102.7%和90.9%。结论:该方法简便、准确,适用于小鼠脑组织中BP-1的测定。

关键词:  , 2, 4二羟基二苯甲酮, 色谱法, 高压液相, 正交试验, 小鼠, 脑组织

Abstract: Objective:To optimize and establish the experimental methods for the determination of 2,4-dihydroxybenzophenone (BP-1) in mouse brain. Methods: BP-1 was determined by high performance liquid chromatography (HPLC) and separated by Waters Symmetry® C18 (4.6 mm×250 mm, 5 μm) using isocratic elution, and the sample preparation conditions were optimized by orthogonal experiment design. The mobile phase was methanolwater (volume ratio 3∶1) containing 3% (volume fraction) acetic acid (pH 3.40) at a flow rate of 1.0 mL/min, and ultraviolet (UV) detection wavelength was set at 290 nm. Retention time was used for qualitative analysis and internal standard method for quantitative analysis. Results: Under the optimized experimental conditions, the calibration curve was linear with a correlation coefficient of 0.999 8 over the concentration range of 0.2-10.0 mg/L. The recoveries of BP-1 were between 96.8% and 104.5%. The intra-day and inter-day precision of BP-1 were 3.5%-5.7% and 4.5%-6.4%, respectively. The extraction recoveries of BP-1 at three concentrations (0.5, 2.0, 8.0 mg/L) in the mouse brain were 90.5%, 89.5%, and 97.7%, and the matrix effect of BP-1 at these three concentrations were 102.9%, 102.7%, and 90.9%, respectively. Conclusion:The method is simple, accurate, and suitable for determination of the contents of BP-1 in mouse brain.

Key words: 2,4-dihydroxybenzophenone, Chromatography, liquid, high pressure, Orthogonal test, Mice, Brain tissue

中图分类号: 

  • R99

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