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高效液相色谱法测定大鼠血清中4-壬基酚和双酚A 被引量:16

Determination of 4-nonylphenol and Bisphenol A in Rat Serum by High Performance Liquid Chromatography with Fluorescence Detection
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摘要 目的 建立高效液相色谱测定血清 4 -壬基酚和双酚 A的方法。方法 大鼠血清样品用正己烷 -乙醚混合溶剂 (70∶ 30 )提取 ,采用 C1 8色谱柱分离 ,以乙腈 -乙酸铵缓冲液 (p H 4 .5 ) (80∶ 2 0 )为流动相 ,在激发波长 2 2 7nm、发射波长 313nm处用荧光检测器检测。结果 血清中的待测组分的质量浓度与峰面积呈良好的线性关系 ,4 -壬基酚和双酚 A线性范围分别为 0 .0 13~ 5 .0μg/ml,0 .0 0 4~ 3.0μg/ml。本方法的检测限 4 -壬基酚为 13ng/ml,双酚 A为 4 ng/ml,加标回收率 4 -壬基酚为 83.8%~ 10 0 .0 % ,双酚 A为 83.3%~ 10 0 .0 % ;日内精密度为 1.70 %~2 .70 % ,日间精密度为 2 .0 6 %~ 9.78%。结论 该法适用于血清中双酚 A和 4 Objective This study was directed to the development of a simple and highly sensitive method for determination of 4-nonylphenol (4-NP) and bisphenol A (BPA) in rat serum using HPLC with fluorescence detector. Methods 4-NP and BPA in serum samples were extracted by a mixed solvent of n-hexane and diethyl ether (70∶30), the organic layer was dried with nitrogen flow and dissolved with mobile phase. The operating conditions such as C 18 column (250 mm×4.6 mm, 5 μm), acetonitrile-ammonium acetate buffer (pH 4.5) as mobile phase at a flow rate of 1 ml/min and fluorescence detector with the excitation and emission wavelength at 227 nm and 313 nm respectively were used for the determination. Results There was good linear relationship between the concentrations of the analytes in rat serum and their peak areas in the ranges of 0.013-5.0 μg/ml for 4-NP and 0.004-3.0 μg/ml for BPA. The detection limit of the method was 13 ng/ml for 4-NP and 4 ng/ml for BPA.Recoveries of rat serum samples were 83.8%-100.0% for 4-NP and 83.3%-100.0% for BPA. The intra-day precision was 1.70%-2.70%, the inter-day precision was 2.06%-9.78%. Conclusion The results showed that the method is suitable for the determination of BPA and 4-NP in serum.
出处 《四川大学学报(医学版)》 CAS CSCD 北大核心 2004年第2期271-273,276,共4页 Journal of Sichuan University(Medical Sciences)
基金 国家自然科学基金 (批准号 3 0 0 3 0 12 0和 3 0 0 70 678)资助
关键词 高效液相色谱法 血清 4-壬基酚 双酚A High performance liquid chromatography Serum 4-Nonylphenol Bisphenol A
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