摘要
利用2,4-二硝基氟苯为柱前衍生试剂,建立了测定山黧豆中毒素β-Ν-草酰基-L-α,β-二氨基丙酸(简称-βODAP)及其无毒性的异构体α-N-草酰基-L-α,β-二氨基丙酸(简称α-ODAP)的恒组分洗脱高效液相色谱方法。利用固相萃取进行样品预处理并优化了流动相的pH值,利用Hyperchem和Gaussian 98优化得到二者的空间结构并计算了它们的极性,从理论上解释了两个异构体的色谱行为。最佳色谱条件是固定相C18,5μm,15 mm×4.6 mm,流动相为25 mmol/L KH2PO4/乙腈,(90∶10,V/V),流速为0.8 mL/m in,室温,测定了特定条件下山黧豆成长过程中两个异构体的含量。
An isocratic high performance liquid chromatographic （HPLC） method was developed to analyze neurotoxin β-N-oxalyl-L-α,β -diaminopropionic acid （β-ODAP） and its innoxious isomer, α-N-oxalyl-L-α,β- diaminopropionic acid （α-ODAP） in Lathyrus sativus by precolumn derivatization with 2,4-dinitrofluorobenzene （DNFB）. The chromatographic conditions were optimized including solid phase extraction （SPE） pretreatment and pH of the buffer in mobile phase. For further explanation of the retention behavior of two isomers in theory, Hyperchem software was used to obtain the optimal structures and Gaussian 98 W to calculate the polarity of two isomers. Under the optimized conditions such as column of C18（5μm, 15 mm × 4.6 mm, mobile phase of 25 mmoL/L KH2PO4-acetonitrile （90： 10, V/V） , flow rate of 0.8 mL/min and room temperature condition, the contents and ratio of the two isomers from different plant developing procedures of Lathyrus sativus in special environment were obtained.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2006年第1期100-102,共3页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金资助项目(No.30270965)
国家重点发展规划项目(No.2000018603)
