QuEChERS净化法快速检测食品中的脱氢乙酸  

QuEChERS Purification Method for Rapid Detection of Dehydroacetic Acid in Food

作　　者：黄珊[1] 范云燕[1] 孙琦[1] 苏颖 HUANG Shan;FAN Yunyan;SUN Qi;SU Ying(Nanning Center for Disease Control and Prevention,Nanning 530023)

机构地区：[1]南宁市疾病预防控制中心,南宁530023

出　　处：《食品工业》2020年第7期309-312,共4页The Food Industry

摘　　要：建立一种使用QuEChERS法净化,C18柱(未封端C18柱)检测脱氢乙酸的高效液相色谱方法。结果表明,样品在pH 8.0条件下用水提取,离心后取3 mL上清液加入0.2 g PSA、0.2 g C18及0.05 g GCB粉末净化,用C18柱进行分析,流动相为pH 8.0甲醇+0.02 mol/L乙酸铵(5+95)。结果表明,在此条件下脱氢乙酸峰拖尾因子为0.863,保留时间为8.514 min,样品检出限为2.2×10^-4~7.5×10^-4 g/kg,线性范围为2~80 mg/L,相关系数为0.99988。加标样品(加标浓度3~50 mg/L)回收率为94.9%~117.6%,RSD为1.8%~4.9%(N=8)。方法满足国家标准要求,大幅减少样品检测时间、提高分析效率。A high performance liquid chromatography(HPLC)method was developed to detect dehydroacetic acid.The samples were extracted with water at pH 8.0.After centrifugation,take 3 mL supernatant and purify it with QuEChERS method,and 0.2 g PSA,0.2 g C18 and 0.05 g GCB powder were added to purify the supernatant.The determination was performed on C18 column(unsealed C18 column).The mobile phase was methanol+0.02 mol/L ammonium acetate(5+95).The results showed that chromatographic peak trailing factor was 0.863 and peak retention time of dehydroacetic acid was 8.514 min.The limits of detection were 2.2×10^-4-7.5×10^-4 g/kg,and the method showed good linearity between 2 mg/L and 80 mg/L(r=0.99988).The recovery rates(3-50 mg/L)of samples were between 94.5%and 117.6%,and relative standard deviations ranged from 1.8%to 9%(N=8).The method meet the requirements of national standards,and it greatly improvesd the speed and efficiency of sample detection.

关 键 词：高效液相色谱 QuEChERS净化 脱氢乙酸 PH 

分 类 号：O657.72[理学—分析化学] TS207.3[理学—化学]