高效液相色谱法同时检测酱油中8种防腐剂

Simultaneous determination of 8 preservatives in soy sauce using high performance liquid chromatography

建立了同时检测酱油中苯甲酸、山梨酸和6种对羟基苯甲酸酯的高效液相色谱-二极管阵列检测器(High performance liquid chromatography-diode array detector,HPLC-DAD)定量分析方法。酱油样品经0.1%甲酸乙腈提取后采用BEH Shield RP18色谱柱分离,乙腈-0.1%甲酸水溶液梯度洗脱,二极管阵列检测器检测,外标法定量。结果表明:8种防腐剂在(0.1~25)mg/kg范围内线性关系良好(r^2=1.0000);方法检出限介于(0.1~0.25)mg/kg之间,在3个浓度水平的加标回收率为97.3%~101.4%,相对标准偏差为0.83%~2.81%(n=6)。该方法操作简便、净化效果好、准确度高,适用于酱油中防腐剂的检测。

A method was developed for the separation and determination of 8 preservatives in soy sauce by high performance liquid chromatography-diode array detector（HPLC-DAD）. Effects of several important factors, such as conditions of sample preparation and conditions of chromatography, were investigated to acquire optimum conditions. Finally the sample was extracted with 0.1% acidic acetonitrile. Then the analytes were separated on a BEH Shield RP18 column, eluted by gradient with acetonitrile and 0.1% formic acid aqueous solution, detected by diode array detector, and quantified by external standard method. The limit of detection（LOD, S/N3） for 8 kinds of preservatives were（0.1~0.25）mg/kg, and the recoveries in soy sauce samples were 97.3%~101.4% with the relative standard deviations（RSDs） ranged 0.83%~2.81%（n=6）. This method is simple, accurate, reliable and reproducible, and can be used for the routine analysis of preservatives in soy sauce.