铁强化酱油中乙二胺四乙酸铁钠含量的胶束液相色谱法测定  

Determination of NaFeEDTA in Iron Fortified Soy Sauce by Micellar Liquid Chromatography

作　　者：林仁权[1] 夏海鸣 戚荣平 孟琪 桑娴 LIN Renquan;XIA Haiming;QI Rongping;MENG Qi;SANG Xian(Gongshu Center For Disease Prevention And Control,Hangzhou 310022)

机构地区：[1]杭州市拱墅区疾病预防控制中心,杭州310022

出　　处：《食品工业》2024年第8期274-279,共6页The Food Industry

基　　金：杭州市拱墅区医药卫生科技计划项目A类项目A202308。

摘　　要：建立了胶束超高效液相色谱法测定铁强化酱油中乙二胺四乙酸铁钠(NaFeEDTA)含量的分析方法。样品仅需简单的稀释和离心,经0.22μm微孔滤膜过滤,即可直接上机,以Waters AccQ·Tag Ultra C18柱(2.1×100 mm, 1.7μm)为色谱柱,以0.010 mol/L十六烷基三甲基溴化铵(CTAB)水溶液(内含5%乙腈和0.025 mol/L磷酸二氢钾)为流动相,流速为0.30 mL/min,采用二极管阵列检测器,检测波长为254 nm,柱温为30℃,外标法进行定量测定。在选定试验条件下, NaFeEDTA质量浓度在0.50~35.0 mg/L范围内具有良好的线性关系(r≥0.999),检出限为50 mg/kg。考察了Na Fe EDTA回收率,对酱油样品进行的3个水平(5.0, 10.0和20.0 mg/kg)的添加回收试验,结果表明,该方法的回收率在88.0%~99.0%之间。对样品重复测定6次,其峰面积的相对标准偏差均为3.3%。该方法操作简单,重现性好,可用于酱油中Na Fe EDTA含量的检测。To establish a method for the determination of NaFeEDTA by micellar liquid chromatography.after a simple dilution and centrifugation,the supernatant was passed over 0.22μm filter membrane,The samples were injected into a UPLC directly with the Waters AccQ·Tag Ultra(2.1×100 mm,1.7μm).The micellar mobile phase was 0.010 mol/L CTAB(Contain 5%acetonitrile and 0.020 mol/L potassium dihydrogen phosphate).The flow rate was 0.30 mL/min and the detection wavelength was 254 nm.The column temperature was 30℃.The method within the 0.50-35.0 mg/L has a good linear relationship(r≥0.999),which the detection limit is 50 mg/kg,The results showed that the mean spiked recoveries of cereals at 3 spiked levels(5.0,10.0 and 20.0 mg/kg)ranged from 88.0%to 99.0%,An iron-fortified soy sauce sample was analyzed for 6 times,and the relative standard deviation(SRSD)of peak areas of NaFeEDTA was 3.3%.This method had simple operation and good repeatability.the method could be applied in the determination of NaFeEDTA in Iron-fortified soy sauce.

关 键 词：乙二胺四乙酸铁钠 胶束液相色谱法 铁强化酱油 

分 类 号：O657.72[理学—分析化学] TS264.21[理学—化学]