[高效液相色谱法测定小鼠脑中的2,4-二羟基二苯甲酮]

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

作者信息

Wang Yi-chao, Sun Yi, Cui Rong, Li Yuan-li, Zhang Bao-xu

机构信息

Department of Occupational and Environmental Health Sciences, Peking University School of Public Health, Beijing 100191, China.

Department of Toxicology, Peking University School of Public Health, Beijing 100191, China.

出版信息

Beijing Da Xue Xue Bao Yi Xue Ban. 2015 Jun 18;47(3):541-7.

PMID:26080890

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.

摘要

目的

优化并建立小鼠脑组织中2,4-二羟基二苯甲酮（BP-1）的测定实验方法。

方法

采用高效液相色谱法（HPLC）测定BP-1，使用Waters Symmetry C18（4.6 mm×250 mm，5 μm）色谱柱进行等度洗脱，通过正交实验设计优化样品前处理条件。流动相为含3%（体积分数）乙酸（pH 3.40）的甲醇-水（体积比3:1），流速为1.0 mL/min，紫外（UV）检测波长设定为290 nm。采用保留时间进行定性分析，内标法进行定量分析。

结果

在优化的实验条件下，校准曲线在0.2-10.0 mg/L浓度范围内呈线性，相关系数为0.999 8。BP-1的回收率在96.8%至104.5%之间。BP-1的日内精密度和日间精密度分别为3.5%-5.7%和4.5%-6.4%。小鼠脑组织中3个浓度（0.5、2.0、8.0 mg/L）的BP-1提取回收率分别为90.5%、89.5%和97.7%，这3个浓度下BP-1的基质效应分别为102.9%、102.7%和90.9%。