基质固相分散萃取-毛细管电泳测定米制品中丙烯酰胺

摘要

建立了基质固相分散萃取-毛细管电泳法检测米制品中丙烯酰胺的新方法.通过实验确定了最佳前处理条件:C18及弗罗里硅土混合作为萃取分散剂(质量比1∶4),样品与分散剂的质量比为5∶9,洗脱液为丙酮-二氯甲烷(体积比6∶4)的混合溶剂,洗脱剂体积为10 mL.在优化实验条件下,以20 mmol/L硼砂(pH 8.4)作缓冲溶液,在15 kV恒压下进行分离,该方法的线性范围为10 ～ 200 μg/mL,相关系数(r)为0.999 8,丙烯酰胺的检出限为0.62 μg/mL,样品中丙烯酰胺的回收率为85.7％ ～ 96.4％.%A new method coupling matrix solid phase dispersion(MSPD) with capillary electrophoresis was developed for the determination of acrylamide in rice product.The optimized conditions obtained in experiments were as follows:Florisil and C18 were used as a mixed dispersant with a mass ratio of 1 ∶ 4.The mass ratio of sample to dispersant was 5 ∶ 9.The mixture of 10 mL acetone-dichloromethane(6 ∶ 4) was used as elution solvent.Under the optimized experimental conditions,20 mmol/L borate solution (pH 8.4) was used as buffer.The sample was separated at a constant voltage of 15 kV.The linear range of acrylamide was in the range of 10-200 μg/mL,with a correlation coefficient(r) of 0.999 8.The limit of detection(LOD,S/N=3) was 0.62 μg/mL for acrylamide and the recoveries were in the range of 85.7％-96.4％.