高效液相色谱-荧光检测法分析麦类中麦角克列斯汀碱

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/N10)。

High-performance liquid chromatography for determination of ergocristine in wheat

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 C_(18) cartridge. Chromatographic separation was carried out on a C_(18) 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 50.0 μg/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 5.0 μg/kg.