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作 者:张静[1,2] 梁颖 张伟[1,2] 孙成均[1,2]
机构地区:[1]四川大学华西公共卫生学院,成都610041 [2]四川省食品安全监测与风险评估重点实验室,成都610041
出 处:《分析试验室》2013年第4期118-121,共4页Chinese Journal of Analysis Laboratory
摘 要:建立了人尿中马尿酸和甲基马尿酸的毛细管电泳同时测定方法。尿样经乙酸乙酯提取,N2流挥干,硼砂-乙腈缓冲液溶解后毛细管电泳法分析。熔融石英毛细管(50 cm×50μm,有效长度41 cm,未涂层)为分离柱;20 mmol/L的硼砂+20%乙腈(pH 9.3)为运行缓冲液,紫外检测波长为230 nm,电泳分离温度为20℃,分离电压为20kV,重力进样高度20 cm,进样时间为10s。在优化的条件下,马尿酸和甲基马尿酸质量浓度在2~50 mg/L范围内具有良好的线性关系,线性相关系数分别为0.9998和0.9994,检出限分别为0.26和0.20 mg/L,加标回收率分别为100.7%~115.5%及93.3%~116.7%。本法适合于尿中马尿酸和甲基马尿酸的同时快速测定。A method for simultaneous determination of hippuric acid and methyl hippuric acid in urine by capillary eIectrophoresis (CE) was established. The sample was extracted with ethyl acetate and the extract was dried up under nitrogen gas. The residue was redissolved in a running buffer solution and analyzed by CE. The experimental parameters were as follows: an uncoated fused-silica-capillary (50 cm × 50μm, 41 cm effective length) was used as the separation column ; a mixed 20 mmol/L borax buffer ( pH 9.3 ) and acetonitrile ( 80 : 20, V/V) was used as the running buffer; the detection wavelength was 230 nm; the electrophoresis temperature was 20℃; gravity sampling time was 10s with gravity sampling height of 20 cm and the running voltage was 20kV. Under the optimized conditions, the linear ranges of the method for hippuric acid and methyl hippuric acid were all in the range of 2 ~ 50 mg/L with the correlation coefficients of 0. 9998 and 0. 9994, respectively. The detection limits were 0. 26 mg/L and 0. 20 mg/L, respectively. The spiked recoveries were 100. 7% ~ 115.5% and 93.3% ~ 116. 7%, respectively. The method is simple, sensitive, accurate and suitable for the determination of hippuric acid and methyl hippurie acid in urine.
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