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目的建立二极管阵列-超高效液相色谱法同时测定食品中苯甲酸、山梨酸、安赛蜜、糖精钠及脱氢乙酸的分析方法。方法样品采取优化的前处理方法,纯水超声提取,高速离心后准确量取清亮液体经0.22μm滤膜过滤,5种添加剂通过乙腈-磷酸二氢钾洗脱体系与甲醇-乙酸铵洗脱体系的比对分析实验,同时采用二极管阵列检测器和保留时间对待测组分进行双重定性鉴别,采取外标法定量。结果 5种成分采用2种洗脱体系均能得到良好的检测结果,在0.001~0.10 mg/m L范围内,有良好的线性关系(r≥0.9999)。CFAPA-175酱油中山梨酸的检测及PTC T118果汁中苯甲酸的检测2个能力验证,采用乙腈和磷酸二氢钾洗脱体系均取得满意结果。结论乙腈-磷酸二氢钾洗脱体系有较好的分离效果,运行时间短,方法操作简单、快速、准确,绿色环保,可应用于批量样品中5种添加剂的检测。
OBJECTIVE To establish a method for the simultaneous determination of benzoic acid, sorbic acid, acesulfame potassium, sodium saccharin and dehydroacetic acid in food by using diode array-ultra performance liquid chromatography. Methods The samples were treated with optimized pretreatment method. The pure water was extracted by ultrasonic. After the high speed centrifugation, the clear liquid was filtered through 0.22μm membrane. The five kinds of additives were separated by acetonitrile-potassium dihydrogen phosphate elution system and methanol-ammonium acetate Of the comparative analysis of experiments, while the use of diode array detector and retention time of the components to be tested for dual qualitative identification, external standard method. Results The results showed that all the five components were well eluted by the two elution systems. There was a good linear relationship (r ≥ 0.999) between 0.001-0.10 mg / mL. The detection of sorbic acid in CFAPA-175 soy sauce and the detection of benzoic acid in PTC T118 juice were validated by two capabilities. Both acetonitrile and potassium dihydrogen phosphate elution system gave satisfactory results. CONCLUSION Acetonitrile-potassium dihydrogen phosphate elution system has good separation effect, short running time, simple, rapid, accurate and green method. It can be applied to the detection of five kinds of additives in bulk samples.