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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 high performance liquid chromatography-diode array detector (HPLC-DAD) quantitative analysis method was developed for simultaneous determination of benzoic acid, sorbic acid and 6 kinds of parabens in soy sauce. Soy sauce samples were extracted with 0.1% formic acid in acetonitrile, separated by BEH Shield RP18 column and eluted with a gradient of acetonitrile-0.1% formic acid, detected by a diode array detector, and quantified by an external standard method. The results showed that the linear range of the eight preservatives was within the range of (0.1-25) mg / kg (r ~ 2 = 1.0000). The detection limits of the eight kinds of preservatives ranged from 0.1-0.25 mg / kg. The spiked recoveries ranged from 97.3% to 101.4% with relative standard deviations of 0.83% -2.81% (n = 6). The method has the advantages of simple operation, good purification effect and high accuracy, and is suitable for the detection of preservatives in soy sauce.