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柱前衍生化高效液相色谱法拆分人体血浆和尿液中阿替洛尔对映体的研究 被引量:10

Study on Precolumn Derivatization HPLC Assay Method of Atenolol Enantiomers in Human Plasma and Urine
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摘要 高效液相色谱法分离和测定人体血浆和尿液中 S(- ) -和 R(+) -阿替洛尔对映体。选用盐酸甲氧胺为内标 ,R (+) -苯乙基异氰酸酯为衍生化试剂 ,ODS为固定相 ,流动相为水 -甲醇 -异丙醇 -二氯甲烷 (5 3 2∶4 1 6∶4 8∶0 4 ) ,荧光检测波长 2 35 /30 0nm (Ex/Em)。血、尿样品经碱化后乙酸乙酯提取 ,并用氯仿 2次抽提。S(- ) -和R (+) -阿替洛尔对映体血、尿样品的线性范围分别为 10~ 10 0 0ng/mL和 2 5~ 15 0 0ng/mL ,绝对回收率均在 84 %以上 ,RSD均小于6 0 %。 A new HPLC method was developed for the determination of atenolol(AT) enantiomers in plasma and urine after derivatization with a homochiral reagent.Methoxamine HCl was used as the internal standard,R(+)-PEIC as a homochiral reagent.Separation was carried out on a 250 mm×4 mm×5 μm ODS Hypersil column and a mobile phase of water-ethanol-isopropanol-dichloromethane(53 2∶41 6∶4 8∶0 4).Fluorescent detector set at an excitation wavelength of 235 nm with an emission wavelength of 300 nm.Plasma samples and urine samples diluted with water were extracted with ethyl acetate,and chloroform subsequently.The standard curves for the enantiomers were linear over the range of 10~1000 ng/mL in plasma and 25~1500 ng/mL in urine.The minimal absolute recoveries of S-atenolol,R-atenolol were over 84.8 %,respectively and the maximal RSD was 5.0 %.The method has been used in pharmacokinetics and pharmacodynamics of atenolol enantiomers.
出处 《药物分析杂志》 CAS CSCD 北大核心 1998年第6期363-366,共4页 Chinese Journal of Pharmaceutical Analysis
基金 广东省自然科学基金资助课题批准文号 :930 954
关键词 阿替洛尔 对映体 高效液相色谱 衍生化法 atenolol(AT) enantiomers HPLC chemical derivarization
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