摘要
提出了一种采用高效液相色谱-荧光检测法(HPLC-FLD)测定麦类样品中麦角克列斯汀碱的方法。麦类样品经V(乙腈)∶V(0.1 mol/L乙酸铵缓冲溶液)=1∶4提取,以C18小柱净化,C18色谱柱(4.6×250 mm,5μm)分离,V(水)∶V(乙腈)=3∶2作流动相,流速1.0 mL/min,以HPLC-FLD定量测定。标准工作溶液浓度在1.0~50.0μg/L范围内,与峰面积成良好的线性关系,线性相关系数〉0.9999,样品在10.0、50.0、250.0μg/kg添加水平的回收率为76%~85%,相对标准偏差(RSD)为6.6%~8.8%(n=8),方法检测限为5.0μg/kg(S/N〉10)。
Ergocristine was determined by high-performance liquid chromatography with fluorescence detection in wheat.Samples were extracted with acetonitrile-0.1 mol/L ammonium acetate buffer solution(1∶4,V/V) and cleanup of extract was accomplished by C18 cartridge.Chromatographic separation was carried out on a C18 column(4.6×250 mm,5 μm) with elution of water-acetonitrile solution(60∶40,V/V) at a flow rate of 1.0 mL/min.Linearity of peak area was obtained over wide range of standard solution concentrations from 1.0 to 50.0μg/L,and the correlation coefficient is greater than 0. 9999. Recoveries and relative standard deviations, by analyzing samples spiked at levels of 10.0, 50.0 and 250.0 μg/kg, were 76% - 85% and 6.6% - 8.8%, respectively. The limit of quantitation (S/ N〉 10) was 5.0μg/kg.
出处
《分析试验室》
CAS
CSCD
北大核心
2010年第1期87-90,共4页
Chinese Journal of Analysis Laboratory
关键词
固相萃取
高效液相色谱
麦角克列斯汀碱
麦类
Solid phase extraction
High-performance liquid chromatography
Ergocristine
Wheat