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建立了一种固相萃取-高效液相色谱法同时测定豆制品中的碱性嫩黄O、酸性橙Ⅱ和碱性橙Ⅱ等3种黄色工业染料的方法。样品经体积分数70%乙醇水溶液(含1.0%氨水)涡旋超声提取后,采用Strata-X-AW固相萃取(SPE)小柱净化,洗脱液用氮气吹至近干后用甲醇溶解并定容,过PTFE滤膜后在Kromasil C18色谱柱上,以V(甲醇):V(20 mmol/L乙酸铵)=65:35的溶液为流动相进行分离,检测波长为450 nm。结果表明,在最优的色谱条件下,各目标化合物的加标回收率在89.0%~94.7%之间,相对标准偏差在2.2%~4.6%之间。3种染料在0.2~20.0 mg/L内呈现良好的线性关系,相关系数r≥0.999,豆制品中碱性嫩黄O、酸性橙Ⅱ和碱性橙Ⅱ的检出限分别为0.06、0.06和0.09 mg/kg。该方法用于实际样品的检测取得了满意的效果。
A method for the simultaneous determination of three yellow industrial dyes, Basic Yellow O, Acid Orange Ⅱ and Basic Orange Ⅱ, in soy by solid phase extraction and high performance liquid chromatography was established. The sample was purified by vortexing with 70% ethanol solution (containing 1.0% ammonia solution) by volume and stratified by Strata-X-AW solid phase extraction (SPE) cartridge. The eluate was purged with methanol and dissolved in methanol After passing through a PTFE filter, the separation was performed on a Kromasil C18 column with a mobile phase of V (methanol): V (20 mmol / L ammonium acetate) = 65:35 with a detection wavelength of 450 nm. The results showed that under the optimal chromatographic conditions, the recoveries of the target compounds ranged from 89.0% to 94.7% with relative standard deviations between 2.2% and 4.6%. The three dyes showed a good linearity in the range of 0.2 ~ 20.0 mg / L, the correlation coefficient was r ≥0.999. The detection limits of alkaline yellow O, acid orange Ⅱ and basic orange Ⅱ were 0.06,0.06 and 0.09 mg / kg. The method has been used to test the actual samples with satisfactory results.