基质固相分散-高效液相色谱法测定川味香肠中的苏丹红染料

建立了川味香肠中苏丹红I～IV的基质固相分散(MSPD)-高效液相色谱(HPLC)分析方法。样品以无水硫酸钠作为分散基体,研磨均匀后与中性氧化铝同时装柱,正己烷淋洗净化,以丙酮-正己烷(5∶95,V/V)溶液洗脱。用InertsilODS-spC18柱(4.6mm×250mm,5μm)进行分离,流动相A为含0.1%甲酸的甲醇,流动相B为0.02mol/L的乙酸铵溶液(A∶B=85∶15,V/V),等度洗脱,柱温40℃。二极管阵列检测器检测,检测波长为490nm,利用保留时间和光谱图定性,外标法定量。4种苏丹红染料在0.10～50.00μg/mL范围内线性关系良好,相关系数均大于0.9999,苏丹红I、II、III、IV的检出限(LOD)分别为0.008～0.011mg/kg(信噪比S/N=3)。在添加浓度为5.0～25.0mg/kg范围内平均回收率达85.54%～94.66%,相对标准偏差(RSD)为0.87%～4.23%(n=6)。

Determination of Sudan dyes in Sichuan sausage by combination of matrix solid-phase dispersion and high performance liquid chromatography

A high-performance liquid chromatography(HPLC)method combined with matrix solid-phase dispersion(MSPD)was established for determination of Sudan I～IV in Sichuan sausage.The sample was mixed with anhydrous sodium sulfate to be a part of the chromatography column.The samples were cleaned up with hexane and rinsed with 50mL of acetone-hexane(5:95,V/V).Separation was carried out on reversed-phase Inertsil ODS-sp C18 column(4.6mm×250mm,5μm)by using a mixture of methanol and formic acid(999:1)as mobile phase A,and 0.02mol/L ammonium acetate solution as mobile phase B(A:B=85:15,V/V)at a flow rate of 1.0mL/min.Detected at the wavelength of 490nm by diode array detector as the temperature was hold at 40℃.The retention time and spectra characterization were both used to determine Sudan dyes and the content of Sudan dyes was quantified by external standard method.Sudan I～IV have good linearity in the range of 0.10～50.00μg/mL,the correlation coefficients were all above 0.9999 and the detection limits of four Sudan dyes were 0.008～0.011mg/kg(S/N=3).With the addition of 5.0 to 25.0mg/kg of Sudan standard to samples,the average recovery rates of four Sudan dyes in Sichuan sausage were between 85.54% and 94.66%.The relative standard deviations(RSDs)of spiked samples varied from 0.87% to 4.23%(n=6).