摘要
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)。
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 disper- sive 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).
出处
《中国调味品》
CAS
北大核心
2012年第3期95-100,共6页
China Condiment
关键词
郫县豆瓣
苏丹红I^IV
高效液相色谱
固相分散萃取
Pixian Horsebean Chilli Paste
sudan I-IV
high-performance liquid chromatography
solid-phase dispersive extraction
作者简介
杨春林(1982-),男,硕士,工程师,研究方向为食品安全与质量控制。通讯作者