异亮氨酸异构体_手性分离_液相色谱电喷雾电离质谱_

高效液相色谱质谱分离分析血浆、尿样中异亮氨酸异构体

http://www.100md.com 《分析化学》 2006年第10期

异亮氨酸异构体,手性分离,液相色谱电喷雾电离质谱,,异亮氨酸异构体，手性分离，液相色谱电喷雾电离质谱,1引言,2实验部分,3结果与讨论

     摘要建立了用邻苯二甲醛和N乙酰L半胱氨酸为柱前手性衍生化试剂，反相高效液相色谱法分离生物样品中异亮氨酸4个异构体，并以电喷雾电离质谱(ESIMS)进行检测的高灵敏度的分析方法。对DIle、DalloIle 和LalloIle检测的线性范围为5～500 ng，相关系数分别为0.9967、0.9968和0.9993 ；对LIle检测的线性范围为50 ng～5 μg；相关系数为0.9990。在正常人血浆中检测出了LIle(204(113.8 mg/L)和LalloIle(116±0.71 mg/L)，在正常人尿样中检测出了LIle(6.10±2.24 mg/L)和DalloIle(0.53±0.17 mg/L)。

    关键词异亮氨酸异构体，手性分离，液相色谱电喷雾电离质谱

    Determination of D and LEnantiomers of Isoleucine and alloIsoleucine in Human Urine and Plasma Using High Performance Liquid ChromatographyElectrospray Ionization Mass Spectrometry

    Zhao Hua, Li Jing, Yuan Pei, Qiu Zongyin*

    Faculty of Pharmceutical Sciences, Chongqing University of Medical Science, Chongqing 400016

    Abstract A sensitive and selective method for the determination of four isoleucine (Ile) isomers (LIle, DIle, LalloIle and DalloIle) in human urine and plasma has been established using highperformance liquid chromatography. This method includes the precolumn derivatization of amino acids with ophthaldialdehyde (OPTA) and NacetylLcysteine (AcCys), and separation using reversed phase high performance liquid chromatography and detected by electrospray ionization mass spectrometry. The linear ranges of DIle, LalloIle and DalloIle spiked in the urine sample are 5-500 ng and that of LIle is 50 ng-5 μg. By using this method, the concentrations of DIle, LalloIle and DalloIle have been determinated in human urine and plasma. The concentrations of LIle and DalloIle are (6.10±2.24) mg/L and (0.53±0.17) mg/L (n=10) respectively in human urine and that of LIle and LalloIle are (204±113.8) mg/L and (1.16±0.71) mg/L (n=5) in human plasma, respectively. ......

百拇医药网 http://www.100md.com/html/DirDu/2006/10/18/25/42/64.htm

您现在查看是摘要页，全文长 10110 字符。