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食品研究与开发:2017,38(12):143-146
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QuEChERS-HPLC-MS/MS快速测定染色黄鱼中3种碱性橙类染料
孙稚菁,王灵芝,任国杰*,张国翠,卢熠川
(大连市产品质量检测研究院,辽宁 大连 116630)
Determination of 3 Basic Orange in Dyed Yellow Croaker by QuEChERS -High Performance Liquid Chromatography-Tandem Mass Spectrometry
SUN Zhi-jing, WANG Ling-zhi, REN Guo-jie*, ZHANG Guo-cui, LU Yi-chuan
(Dalian Institute of Product Quality Supervision & Inspection, Dalian 116630, Liaoning, China)
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投稿时间:2017-03-06    
中文摘要: 采用高效液相色谱-串联质谱法建立快速检测染色黄鱼中碱性橙Ⅱ,碱性橙 21 和碱性橙 22 的分析方法。将 待测样品经 QuEChERS 法进行预处理,选用乙腈溶液超声提取,经氯化钠和 C18 粉末净化,以 10 mmol/L 的醋酸铵溶 液(含有 0.1 %甲酸)-乙腈(含有 0.1 %甲酸)作为流动相,经 Agilent poroshell 120 EC-C18(2.7 μm,2.1 mm×50 mm)色谱 柱分离,采用多反应检测模式(MRM)检测。用标准曲线外标法进行定量。在优化条件下,目标物的线性范围为 1 μg/L~100 μg/L,相关系数均大于 0.999。该 3 种碱性橙类染料的定量下限为 5 μg/kg。在 3 个浓度水平下,各目标物 的回收率均大于 85 %,相对标准偏差(RSD)均低于 5 %。方法准确、快速、简便、灵敏、可靠。可用于染色黄鱼中此 3 种碱性橙类染料的快速测定。
Abstract:A high performance liquid chromatography- tandem mass spectrometry (HPLC-MS/MS) method was developed for the rapid determination of 3 basic orange in dyed yellow croaker. To pass through the QuEChERS method under test sample preprocessing, ultrasonic extraction with acetonitrile solution, purifica- tion by sodium chloride and C18 powder, the extract was separated on an Agilent poroshell 120 EC-C18(2.7 μm,2.1 mm×50 mm)using a gradient elution program with mobile phase of 10 mmol/L ammonium acetate(contain- ing 0.1 % formic acid) -acetonitrile(containing 0.1 % formic acid), with multiple reactions monitoring(MRM) mode for testing. Using external standard method for the quantitative standard curve. The linear ranges of 3 ana- lytes were in the range of 1 μg/L-100 μg/L, with correlation coefficients more than 0.999. The limits of quanti- ation (LOQs) were 5 μg/kg. The average recoveries at three spiked levels were greater than 85 %, with RSDs less than 10 %. This method is accurate, simple, sensitive and reliable, and can be used for analysis of 3 basic orange in dyed yellow croaker.
文章编号:201712031     中图分类号:    文献标志码:A
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