OSAKA-SODA-CAPCELL-PAK-C_(18)色谱柱同时检测面制品中5种添加剂  

Simultaneous determination of five additives in flour products by OSAKA-SODA-CAPCELL-PAK-C18

作　　者：路凌怡 倪蓉[1] 刘兰侠[1] 陈翔[1] 钱杰峰[1] LU Ling-yi;NI Rong;LIU Lan-xia;CHEN Xiang;QIAN Jie-feng(Xuhui District Center for Disease Control and Prevention,Shanghai 200237,China)

机构地区：[1]上海市徐汇区疾病预防控制中心,上海200237

出　　处：《中国卫生检验杂志》2022年第11期1308-1310,1314,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立一种快速、简单的可同时测定面制品中安赛蜜、糖精钠、苯甲酸、山梨酸和脱氢乙酸添加剂的高效液相色谱法。方法样品通过氢氧化钠和硫酸锌沉淀后,利用OSAKA-SODA-CAPCELL-PAK-C_(18)(4.6 mm×150mm,5μm)色谱柱,以乙腈和0.02mol/L磷酸二氢钾为流动相、梯度洗脱、用二极管阵列检测器检测。安赛蜜、苯甲酸、山梨酸和脱氢乙酸的检测波长为225nm,糖精钠为205nm,以保留时间定性,外标法定量分析。结果5种添加剂在0.5μg/ml~50.0μg/ml具有良好的线性关系(r>0.9999),检出限为0.0002 g/kg-0.006 g/kg,样品的平均回收率为93.6%~105.0%,相对标准偏差为0.16%-1.56%。结论本实验利用CAPCELL-PAK-C_(18)柱,以氢氧化钠和硫酸锌为蛋白沉淀剂,乙腈和磷酸二氢钾为流动相,进一步优化了同时检测面制品中5种添加剂的方法。该方法前处理方便、保留时间稳定、色谱峰型好、分析速度快、回收率高,适用于大批量样品的快速检验。Objective To develop a rapid and simple high performance liquid chromatography(HPLC)method for the simultaneous determination of acesulfame,saccharin sodium,benzoic acid,sorbic acid and dehydroacetic acid in flour products./Methods The samples were precipitated with sodium hydroxide and zinc sulfate.The supernatant was analyzed with the mobile.phase consisting of acetonitrile and 0.02 mol/L potassium dihydrogen phosphate on OSAKA-SOD-CAPCELL-PAK-C_(18)column(4.6 mm×150 mm,5μm)by gradient elution,and detected by diode array detector.Acesulfase,benzoic acid,sorbic acid and dehydroacetic acid were confirmed by diode array detector(DAD)at 225 nm,and sodium saccharin was detected at 205 nm so as to make qualitative retention time and quantitative analysis by external standard method.Results The linear range of acesulfase,sodium saccharin,benzoic acid,sorbic acid and dehydroacetic acid was within 0.5μg/ml-50.0μg/ml,which showed good linearity(r>0.9999).The limits of detection were within 0.0002 g/kg-0.0006 g/kg,the average recoveries were within 93.6%-105.0%,and the relative standard deviations(RSD)were within 0.16%-1.56%.Conclusion Using OSAKA-SODA-CAPCELL-PAK-C_(18)column,sodium hydroxide and zinc sulfate as protein precipitant,acetonitrile and potassium dihydrogen phosphate as mobile phase,the method for simultaneous detection of five additives in flour products was further optimized.The method has advantages of convenient pretreatment,stable retention time,good chromatographic peak shape,fast analysis speed and high recovery,and is suitable for rapid detection of large quantities of samples.

关 键 词：高效液相色谱法 添加剂 蛋白沉淀剂 

分 类 号：O657.72[理学—分析化学]