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-al-lo-Ile和L-allo-Ile检测的线性范围为5~500ng,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50ng^5μg;相关系数为0.9990。在正常人血浆中检测出了L-Ile(204(113.8mg/L)和L-allo-Ile(1·16±0.71mg/L),在正常人尿样中检测出了L-Ile(6.10±2.24mg/L)和D-allo-Ile(0.53±0.17mg/L)。
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 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.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2006年第10期1433-1436,共4页
Chinese Journal of Analytical Chemistry
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
Isomers of isoleucine, chiral separation, liquid chromatography-electrospray ionization mass spectrometry