摘要
建立一种可用于定量的毛细管电泳法分离山莨菪碱对映体.系统研究了三种手性选择剂:羟丙基-β-环糊精(HP-β-CD),甲基-β-环糊精(Me-β-CD),羧甲基-β-环糊精(CM-β-CD)及其浓度、缓冲溶液浓度和pH对山莨菪碱拆分的影响.在110mmol/L Tris-H3PO4缓冲液中加入20.0mg/mL HP-β-CD和5.0mg/mL CM-β-CD(pH4.0)条件下,山莨菪碱的4个对映体达到基线分离.血清样品通过固相萃取预处理和浓缩,对映体的固相萃取回收率在82.9%～90.7%,相对标准偏差RSD%均小于7%.山莨菪碱的4个对映体血标准溶液浓度与电泳峰面积在77.86～0.39μg/mL范围内呈良好的线性,r≥0.999,检出限(S/N=3)为0.08μg/mL.平均日内和日间精密度(RSD%)分别小于4.2%和6.5%,方法回收率为95.1%和105%.建立的方法准确、可靠,应用于监测兔连续3d口服75mg山莨菪碱后血清中山莨菪碱的血药浓度,结果满意.
To establish a capillary electrophoresis method under which anisodamine enantiomers can be sufficiently separated for quantification, hydroxypropyl-β-cyclodextrin （HP-β-CD）, methyl-β-cyclodextrin （Me-β-CD） and carboxymethyl-β-cyclodextrin （CM-β-CD） were used as chiral selectors. Effects of the concentration of cyclodextrin, pH and concentration of buffer were investigated. The baseline separation of four enantiomers of anisodamine was obtained in 110 mmol/L Tris-H3PO4 buffer-20.0 mg/mL HP-β-CD-5.0 mg/mL CM-β-CD at pH 4.0. Prior to electrophoresis, the analytes were purifed and preconcentrated by solid phase extraction from plasma. Standard curves constructed using blank plasma spiked with anisodamine in the range 77.86-0.39 μg/mL, showed acceptable linearity with correlation coefficients, r≥0.999. The detection limits for the four enantiomers of anisodamine were all 0.08 μg/mL. Mean intra- and inter-day precisions （RSD%） were 〈4.2% and 6.5%, respectively. The method showed recoveries for the four enantiomers ranging from 95.1% to 105%. Acceptable precision and accuracy of the method were demonstrated for pharmacokinefic studies by determining the concentrations of anisodamine enantiomers in rabbit plasma, after administration of 75 mg of anisodamine during three consecutive days.
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
2009年第8期801-807,共7页
Acta Chimica Sinica
基金
广西自然科学基金(No.0640038)
肇庆市科技计划(No.10560)
肇庆学院自然科学基金(No.0737)资助项目
关键词
毛细管电泳
手性拆分
山莨菪碱
固相萃取
capillary electrophoresis
chiral separation
anisodamine
solid phase extraction
