摘要
建立了用薄层层析和薄层扫描法对N-乙酰-L-半胱氨酸合成进行流程诊断的方法.采用硅胶G板,以正丁醇-醋酸-水(4.5∶1.5∶1)为展开剂,单波长直线扫描,扫描波长λ=700nm.对合成反应的初始阶段、反应中、反应后取样样品进行定性和定量检测.原料在反应滴加后的初始阶段转化率达到97.08%,说明水相合成法较为合理,有效地抑制了L-半胱氨酸的氧化.设计的流程诊断法对N-乙酰-L-半胱氨酸和半胱氨酸盐酸盐的线性范围分别为15.1～36.5mg/mL、1.5～3.1mg/mL.平均回收率分别为99.93%～100.05%、99.94%～100.10%.RSD分别为0.32%～0.34%、0.31%～0.34%.该方法可靠、简便易行,有利于反应流程诊断控制.
The process diagnosis for synthesizing reaction of N-acetyl-L-cysteine (NAC) was established by thin layer chromatography (TLC) and TLC-scanning. The method involves a silica gel- G plate, a mobile phase of n-butanol-acetic acid-water(4.5∶1.5∶1),a single-wavelength linear scanning at 700 nm. By qualitative and quantitative detection of different moment samples of synthesizing reaction of N-acetyl-L-cysteine, it was deducted that the conversion ratio of L-cysteine being at 97.08% on the preliminary moment of reaction. NAC: calibration curve range :15.1~36.5 mg/mL; average recovery : 99.93%~100.05%; RSD: 0.32%^(0.34%.) L-cysteine hydrochloride: calibration curve range :1.5~3.1 mg/mL; average recovery :99.94%^(100.10%;) RSD: 0.31%~0.34%. The method is simpler and more feasible for controlling the reaction as compared with HPLC.
出处
《浙江大学学报（理学版）》
CAS
CSCD
2004年第1期62-65,共4页
Journal of Zhejiang University（Science Edition）
基金
国家自然科学基金资助项目(20006013)
浙江省重点科技计划资助项目(2002C21018).
