摘要
建立阴离子固相萃取-高效液相色谱(high performance liquid chromatography,HPLC)法同时测定肉制品中13种易于滥用的合成色素的检测方法。样品经石油醚除去脂肪后,以氨水乙醇溶液提取,结合低温冷冻法除去蛋白质,通过阴离子固相小柱批量富集净化后,用2%(体积分数)氨水甲醇洗脱,洗脱液氮吹浓缩后得供试液,采用Waters XBridge Shield RP_(18)(250 mm×4.6 mm,5μm)色谱柱分离,以甲醇和0.02 mol/L乙酸铵为流动相进行梯度洗脱,经二极管阵列检测器分析,外标法定量。13种目标化合物在0.1μg/mL~10.0μg/mL质量浓度范围内线性良好,相关系数r均高于0.9995;检出限为0.2 mg/kg~0.5 mg/kg,定量限为0.6 mg/kg~1.5 mg/kg;平均加标回收率为65.2%~102.0%;精密度(n=6)在6.0%以内。采用该方法检测156批肉制品,12批肉制品中检出目标色素,含量范围在0.23 mg/kg~15.7 mg/kg之间,检出色素包括常见的酸性红、苋菜红及日落黄,还发现有非法添加红2G和酸性橙Ⅱ。该方法适用于含有大量脂肪和蛋白质的肉制品中多种合成色素的同时测定。
An analytical method based on anionic solid phase extraction combined with high performance liquid chromatography was established for the determination of 13 synthetic colorants in meat products,which are frequently adulterated with such additives.The samples used for analysis were fat removed from meat using petroleum ether and then extracted using an ammonia-ethanol solution.After deproteinization via cryopreservation,the extracts were purified in bulk by anion-exchange solid phase column chromatography,eluted with methanol containing 2%(volume fraction)ammonia,and concentrated in a stream of nitrogen to obtain the final sample solutions.These samples were separated with a Waters XBridge Shield RP_(18) column(5μm,250 mm×4.6 mm)using 0.02 mol/L NH4Ac solution and methanol as the mobile phase.The 13 synthetic colorants were analyzed using a diode array detector and quantified with reference to an external standard.The 13 synthetic colorants had linear ranges from 0.1μg/mL to 10.0μg/mL.with correlation coefficients(r)greater than 0.9995,whereas limits of detection ranged from 0.2 mg/kg to 0.5 mg/kg and quantitative limits ranged from 0.6 mg/kg to 1.5 mg/kg.Furthermore,the average recoveries were in the range from 65.2%to 102.0%,with relative standard deviations of less than 6.0%(n=6).In total,156 batches of meat products were analyzed using the developed method,among which five of the 13 targeted synthetic colorants(red 2G,acid orangeⅡ,azorubine,amaranth,and sunset yellow)were identified in 12 batches,ranging in concentration from 0.23 mg/kg to 15.7 mg/kg.Notably,these results indicated that colorants such as red 2G and acid orangeⅡ,which were not legally permitted for use in meat products,were detected in some samples This method accordingly proved to be suitable for the simultaneous determination of multiple synthetic colorants in meat products containing large quantities of fat and protein.
作者
李道霞
黄丽娟
唐昌云
蒋燕舒
余晓琴
LI Dao-xia;HUANG Li-juan;TANG Chang-yun;JIANG Yan-shu;YU Xiao-qin(Sichuan Institute for Food and Drug Control,Chengdu 611731,Sichuan,China)
出处
《食品研究与开发》
CAS
北大核心
2021年第17期157-164,共8页
Food Research and Development
基金
中华人民共和国国家卫生和计划生育委员会委托项目(spaq-2016-174)。
关键词
阴离子固相萃取
高效液相色谱法
肉制品
合成色素
红2G
酸性橙Ⅱ
anionic solid phase extraction
high performance liquid chromatography
meat product
synthetic colorant
red 2G
acid orangeⅡ
