摘要
目的建立高效液相色谱法测定果冻、口香糖和明胶囊壳中11种合成着色剂及8种铝色淀的含量。方法样品经提取溶剂(乙醇:2%氨水:水=7:2:1,V:V:V)2次超声提取,离心后的上清液经固相萃取柱净化,用Agilent SB-C18 (4.6 mm×250 mm, 5μm)柱分离, 0.02 mol/L乙酸铵水溶液-甲醇作为流动相梯度洗脱,二极管阵列检测器检测,外标法定量。结果 11种合成着色剂在0.1～10 mg/L范围内与峰面积呈良好线性关系,相关系数均达到0.9999,方法精密度良好,相对标准偏差(relative standard deviation, RSD)为1.4%～3.9%(n=6)。11种着色剂加标回收率为80.1%～110%, RSD为0.15%～5.5%(n=3), 8种铝色淀加标回收率为80.8%～105.6%, RSD为0.4%～5.4%(n=3)。检出限为0.1～0.4 mg/kg,定量限为0.2～1.1 mg/kg。结论该方法简便灵敏,准确可靠,适用于果冻、口香糖和明胶胶囊壳中合成着色剂及铝色淀的测定。
Objective To establish a method for the determination of 11 kinds of synthetic colorants and 8 kinds of aluminum lakes in the jelly,chewing gum and capsule shell by high performance liquid chromatography.Methods The sample was extracted twice by ultrasonic extraction solvent(ethanol: 2% ammonia: water=7:2:1,V:V:V),the supernatant after centrifugation was purified by solid phase extraction column,and separated by Agilent SB-C18 column(4.6 mm×250 mm,5 μm) at the flow rate of 0.02 mol/L by gradient elution using with the 0.02 mol/L ammonium acetate aqueous solution-methanol,then detected by diode array detector,and quantitated by external standard method.Results There were linear relationships between the peak areas of 11 compounds in the range of 0.1-10 mg/L and the correlation coefficients were all greater than 0.9999.Precisions of method were good with the relative standard deviations(RSDs) of 1.4%-3.9%(n=6).Recoveries of 11 kinds of colorants were 80.1%-110%,and the RSDs were 0.15%-5.5%(n=3).The recoveries of 8 kinds of aluminum lakes were 80.8%-105.6%,and the RSDs were 0.4%-5.4%(n=3).The limits of detection and limits of quantitative ranged within 0.1-0.4 mg/kg and 0.2-1.1 mg/kg,respectively.Conclusion The method is simple,rapid and sensitive,which is suitable for the determination of 11 kinds of synthetic pigments and 8 kinds of aluminum lakes in jelly,chewing gum and capsule shell.
作者
赵梅
黄丙楠
曹进
刘素丽
王宏伟
钮正睿
ZHAO Mei;HUANG Bing-Nan;CAO Jin;LIU Su-Li;WANG Hong-Wei;NIU Zheng-Rui(National Institutes of Food and Drug Control,Beijing 100050,China)
出处
《食品安全质量检测学报》
CAS
2019年第1期31-39,共9页
Journal of Food Safety and Quality
基金
国家重点研发计划项目(2017YFC1601300)~~
关键词
合成着色剂
铝色淀
高效液相色谱法
synthetic pigments
aluminum lakes
high performance liquid chromatography
