北京大学学报（医学版）
北京大學學報（醫學版）
북경대학학보（의학판）
JOURNAL OF BEIJING MEDICAL UNIVERSITY(HEALTH SCIENCES)
2015年
3期
541-547
,共7页
王一超%孙艺%崔蓉%李园利%张宝旭
王一超%孫藝%崔蓉%李園利%張寶旭
왕일초%손예%최용%리완리%장보욱
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
2 ,4-二羥基二苯甲酮%色譜法,高壓液相%正交試驗%小鼠%腦組織
2 ,4-이간기이분갑동%색보법,고압액상%정교시험%소서%뇌조직
2,4-dihydroxybenzophenone%Chromatography,liquid,high pressure%Orthogonal test%Mice%Brain tissue
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,5μm)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0.9998；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。
目的：：建立和優化小鼠腦組織中2,4-二羥基二苯甲酮(2,4-dihydroxybenzophenone,BP-1)的測定方法。方法：採用正交試驗設計優化樣品預處理條件,Waters Symmetry? C18(4.6 mm ×250 mm,5μm)色譜柱分離,等度洗脫,流動相為含3%(體積分數)乙痠的甲醇-水(體積比為3∶1),pH為3.40,流速為1.0 mL/min,紫外檢測器檢測,檢測波長為290 nm,高效液相色譜法測定小鼠腦組織中BP-1,保留時間定性,以內標法定量。結果：在優化的實驗條件下,BP-1在0.2~10.0 mg/L濃度範圍內線性關繫良好,相關繫數為0.9998；BP-1的加標迴收率為96.8%~104.5%；日內和日間精密度分彆為3.5%~5.7%和4.5%~6.4%；低、中、高3種濃度BP-1的提取迴收率分彆為90.5%、89.5%和97.7%；低、中、高3種濃度BP-1的基質效應分彆為102.9%、102.7%和90.9%。結論：該方法簡便、準確,適用于小鼠腦組織中BP-1的測定。
목적：：건립화우화소서뇌조직중2,4-이간기이분갑동(2,4-dihydroxybenzophenone,BP-1)적측정방법。방법：채용정교시험설계우화양품예처리조건,Waters Symmetry? C18(4.6 mm ×250 mm,5μm)색보주분리,등도세탈,류동상위함3%(체적분수)을산적갑순-수(체적비위3∶1),pH위3.40,류속위1.0 mL/min,자외검측기검측,검측파장위290 nm,고효액상색보법측정소서뇌조직중BP-1,보류시간정성,이내표법정량。결과：재우화적실험조건하,BP-1재0.2~10.0 mg/L농도범위내선성관계량호,상관계수위0.9998；BP-1적가표회수솔위96.8%~104.5%；일내화일간정밀도분별위3.5%~5.7%화4.5%~6.4%；저、중、고3충농도BP-1적제취회수솔분별위90.5%、89.5%화97.7%；저、중、고3충농도BP-1적기질효응분별위102.9%、102.7%화90.9%。결론：해방법간편、준학,괄용우소서뇌조직중BP-1적측정。
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) ace-tic 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, ac-curate, and suitable for determination of the contents of BP-1 in mouse brain.
