固相分散萃取-高效液相色谱法测定郫县豆瓣中四种苏丹红染料的研究

建立了郫县豆瓣中苏丹红Ⅰ～Ⅳ的固相分散萃取(SPDE)-高效液相色谱(HPLC)分析方法。样品用无水硫酸钠作为分散剂,以乙腈提取样品中的苏丹红,提取液用中性氧化铝层析柱进行净化。用Inertsil ODS-sp C18柱(4.6mm×250mm,5μm))分离,流动相A为乙腈,流动相B为0.1%甲酸水溶液(A∶B为90∶10,V/V),等度洗脱,流速1mL/min,柱温40℃。二极管阵列检测器检测,检测波长为517nm,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0.10～20.00μg/mL范围内线性关系良好,相关系数均大于0.9999,苏丹红Ⅰ～Ⅳ的检出限(LOD)分别为0.009～0.013mg/kg(信噪比S/N=3)。在添加浓度为0.5～10.0mg/kg范围内平均回收率达81.67%～93.28%,相对标准偏差(RSD)为1.07%～4.61%(n=6)。

Determination of sudan dyes in Pixian Horsebean Chilli Paste by solid-phase dispersive extraction coupled with high performance liquid chromatography

A high-performance liquid chromatography(HPLC) method combined with solid-phase dispersive extraction(SPDE) was established for determination of sudan Ⅰ～Ⅳ in Pixian Horsebean Chilli Paste.The anhydrous sodium sulfate was the dispersing agent in the process of solid-phase dispersive extraction.The sample was extracted with acetonitrile and the extract was cleaned up with aluminum oxide column.Separation was carried out on reversed-phase Inertsil ODS-sp C18 column(4.6 mm × 250 mm,5 μm) by using acetonitrile as mobile phase A,a mixture of formic acid and water(1∶999) as mobile phase B(A∶B is 90∶10,V/V) at a flow rate of 1.0 mL/min.Detected at the wavelength of 517 nm by diode array detector as the temperature was hold at 40 ℃.The retention time and spectra characterization were all 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 0.10~20.00 μg/mL,the correlation coefficients were all above 0.9999 and the detection limits of four sudan dyes were 0.009~0.013 mg/kg(S/N=3).With the addition of 0.5 to 10.0 mg/kg of sudan standard to samples,the average recovery rates of four Sudan dyes in Pixian Horsebean Chilli Paste were between 81.67% and 93.28%.The relative standard deviations(RSDs) of spiked samples varied from 1.07% to 4.61%(n=6).