高效液相色谱-荧光检测法分析麦类中麦角克列斯汀碱

High-performance liquid chromatography for determination of ergocristine in wheat

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.