高效液相色谱法测定食品中3种碱性橙含量

HPLC Determination of 3 Alkali Orange Dyestuffs in Foodstuffs

应用高效液相色谱法测定了3种非法作为色素加入于食品中的碱性橙染料即碱性橙2(CDG)、碱性橙21(AOG)及碱性橙22(AOR)。将均质样品(20.00g)与无水硫酸钠2g混合后,用无水乙醇超声提取3次,每次用30mL。将提取液合并,先在45℃真空蒸发,最后用吹氮法蒸干。用流动相(0.02mol·L^(-1)乙酸铵溶液与甲醇按39比61的比例混合)溶解残渣并定容至5mL。将此溶液离心分离,取其上清液用于高效液相色谱分析。Agilent C_(18)色谱柱用于各组分的分离。用二极管阵列检测器在430nm波长处检测CDG,在480nm波长处检则AOG及AOR,3种染料的线性范围均在0.50～20.0mg·L^(-1)之间,方法的检出限(3S/N)均为0.10mg·L^(-1)应用此方法分析了黄鱼样品,并以此为基体加入3种染料的标准溶液后进行分析,测得其平均回收率依次91.2%,93.6%及96.0%,测定值的相对标准偏差(n=6)均小于2%。

HPLC was applied to the determination of 3 alkali orange dyestuffs,namely chrysoidine G（CDG）, astrazon orange G（AOG） and astrazon orange R（AOR）,which were added contrabandly to foodstuffs as colorants.The homogenized sample（20.00 g） was mixed with 2 g of anhydrous Na_2SO_4 and extracted thrice ultrasonically with absolute alcohol（30 mL＋30 mL＋30 mL）.The extracts were combined and evaporated first at 45℃in vacuum and then by N_2-blowing to dryness.The residue was taken up with the mobile phase（mix 0.02 mol·L^（-1） NH_4OAc solution with methanol in the ratio of 39 ＋ 61 by volume） and made up to 5 mL.After centrifugation,the supernatant was used for HPLC analysis by separation on Agilent C_（18） column.Diode array detector was used for the determination of CDG at 430 nm and of AOG as well as AOR at 480 nm.Linearity ranges for the 3 dyestuffs were found to be same between 0.50 to 20.0 mg·L^（-1）,with detection limits（3S/N） of 0.10 mg·L^（-1）.Tests for recovery and precision were performed by addition of standards to a sample of yellow croaker,and the results of average recovery found were 91.2%,93.6%and 96.0%for the 3 dyestuffs respectively, with RSD＇s（n=6） less than 2%.