摘要
取适量辣椒制品样品用环己烷-丙酮(3+1)混合液超声提取后,离心分离,取上清液,蒸至近干,用环己烷-乙酸乙酯(1+1)混合液溶解并定容至10mL。用凝胶渗透色谱法(GPC)净化,用环己烷-乙酸乙酯(1+1)混合液淋洗,收集22~30min之间的流出液,于40℃吹氮蒸干,用乙腈-水(8+2)溶液定容至1mL。用Waters Symmetry C18柱分离,用不同比例的水及乙腈的混合液进行梯度淋洗。用二极管阵列检测器(PDA)在波长478nm(苏丹红Ⅰ)及520nm(苏丹红Ⅱ、Ⅲ及Ⅳ)处进行检测,上述4种染料的线性范围均在0.1~5mg·L-1之间。4种染料在辣椒油中的检出限为0.02mg·kg-1,在辣椒酱及辣椒粉中的检出限均为0.005mg·kg-1。用标准加入法测得方法的回收率在79.5%~93.8%之间,测定值的相对标准偏差(n=6)在1.9%~8.3%之间。
Appropriate amount of the chilli product sample was extracted ultrasonically with the mixture of cyclohexane and acetone(3+1).After centrifugation,the supernatants were taken and evaporated to near dryness.The residue was dissolved and made up to 10 mL with the mixture of cyclohexane and ethylacetate(1+1),which is also the mixture in gel permeation chromatography(GPC).Eluates flowed out during the interval of 22-30 min were collected,and evaporated to dryness at 40 ℃ by N2-blowing.The residue was dissolved and made up to 1mL with acetonitrile-water(8+2)solution.Waters Symmetry C18 column was used for separation with mixtures of water and acetonitrile in various proportions used as mobile phase in gradient elution.Detections were made with PDA at 478 nm for Sudan Ⅰ and at 520 nm for Sudan Ⅱ,Ⅲ and Ⅳ.Linearity ranges for the 4dyes were found same between 0.1to 5mg·L-1.Detection limits of the 4dyes found in chilli oil were 0.02mg·kg-1,and in chilli sauce and chilli powder were same as 0.005mg·kg-1.Tests for recovery were made by standard addition method,giving values of recovery in the range of 79.5%-93.8%,with RSD′s(n=6)in the range of 1.9%-8.3%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2015年第1期57-60,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
