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目的建立了同时测定饮料中10种防腐杀菌剂的高效液相色谱-二极管阵列检测器(HPLC-DAD)测定方法。方法样品用甲醇提取,通过C8固相萃取柱净化,以甲醇-0.02 mol/L乙酸铵为流动相,经C18反相色谱柱(250 mm×4.6 mm,5.0μm)分离,二极管阵列检测器检测,外标法定量。结果 10种防腐杀菌剂在0.1~10.0μg/ml范围内线性关系良好(r≥0.995 1),检出限为0.25~1.0μg/ml(S/N=10),10种防腐杀菌剂在两种饮料基质(果汁饮料、碳酸饮料)中添加3个水平的样品中的回收率74.1%~94.1%;相对标准偏差为5.3%~15.1%。结论该方法操作简单、快速、检出限低,满足国内外对饮料类食品中上述10种防腐杀菌剂的限量要求,适用于饮料中10种防腐杀菌剂的检测。
Objective To establish a HPLC-DAD method for simultaneous determination of 10 preservatives and bactericides in beverages. Methods The sample was extracted with methanol and purified by C8 solid phase extraction. The column was separated on a C18 reversed-phase column (250 mm × 4.6 mm, 5.0 μm) using methanol-0.02 mol / L ammonium acetate as the mobile phase. Diode array detector , External standard method. Results The results showed that the linear range of the 10 kinds of antiseptics was 0.1 ~ 10.0μg / ml (r≥0.9951), the detection limit was 0.25 ~ 1.0μg / ml (S / N = 10) The recoveries of three kinds of samples (fruit juice drinks, carbonated drinks) in three levels of samples were 74.1% ~ 94.1% with relative standard deviations of 5.3% ~ 15.1%. Conclusion The method is simple, rapid, and has a low detection limit to meet the domestic and international requirements for the above 10 kinds of antiseptic and bactericidal agents in beverage foods. It is suitable for the detection of 10 kinds of antiseptic and bactericidal agents in beverages.