摘要
试验建立高效液相色法快速准确测定大黄鱼中非法染料硫代黄素的分析方法。样品经乙腈-水溶剂提取,乙腈饱和正己烷除脂,XBridge C_(18)色谱柱分离,以甲醇-0.02%甲酸水为流动相梯度洗脱,二极管阵列检测器检测,外标法定量。对硫代黄素的稳定性进行系统性考察,同时分别考察不同提取溶剂、净化方式等对硫代黄素提取效率的影响。结果显示,硫代黄素在0.5~200.0μg/mL浓度范围内线性关系良好,线性相关系数(R)大于0.999,方法检出限为0.2 mg/kg,定量限为0.5 mg/kg。在0.5,1.0和5.0 mg/kg 3个浓度水平下,加标回收率在91.6%~97.8%,相对标准偏差在1.5%~2.1%。该方法简便、高效、准确性好、抗干扰能力强,适用于大黄鱼中非法染料的快速定性、定量分析。
A high performance liquid chromatography(HPLC) method was developed for the rapid determination of Thioflavin T(ThT) in Larimichthys crocea.The sample was extracted with acetonitrile-water and the fat in samples was removed by acetonitrile saturated n-hexane.The separation of targeted compound was performed on an XBridge C_(18) column using methanol-0.02% formic acid as mobile phase under gradient elution mode,and detected with diode-array detector by external standard method.The stability of ThT was systematically investigated.The effects of different extraction solvents and purification methods on ThT extraction efficiency were discussed.The results showed that ThT had a good linear relationship in the linear range of 0.5-200.0 μg/mL with the good correlation coefficient(R≥0.999).The limit of detection(SLOD) and the limit of quantitation(SLOQ) of ThT were 0.2 mg/kg and 0.5 mg/kg,respectively.The average recoveries at 0.5,1.0 and 5.0 mg/kg three different concentrations were in the range of 91.6%-97.8%,with relative standard deviation(S_(RSD),n=6) in the range of 1.5%-2.1%.The method was easy,accurate and highly reproducible.The developed method was suitable for rapid qualitative and quantitative analysis of illegal dye in Larimichthys crocea.
作者
郑文静
赵慧男
孙珊珊
薛霞
刘艳明
张艳侠
ZHENG Wenjing;ZHAO Huinan;SUN Shanshan;XUE Xia;LIU Yanming;ZHANG Yanxia(Shandong Institute for Food and Drug Control,Jinan 250101;Shandong Research Center of Engineering and Technology for Safety Inspection of Food and Drug,Jinan 250101)
出处
《食品工业》
CAS
2022年第1期323-327,共5页
The Food Industry
基金
国家重点研发计划(2017YFC1601600)。
作者简介
通信作者:刘艳明;通信作者:张艳侠。
