摘要
建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定食品中碱性橙2、碱性嫩黄O、碱性紫5BN和罗丹明B四种碱性工业染料的分析方法。样品用乙腈提取,经WCX固相萃取柱净化后,采用Agilent Zorbax Eclipse Plus C_18柱(2.1 mm×50 mm,1.8μm)为分离柱,以乙腈和含0.1%甲酸的5 mmol/L乙酸铵溶液作为流动相,梯度洗脱。在电喷雾正离子模式下(ESI+),用多重反应监测(MRM)模式进行检测,基质匹配外标法定量。在优化的试验条件下,碱性橙2的检出限为0.2μg/kg,定量限为0.6μg/kg,碱性嫩黄O、碱性紫5BN和罗丹明B的检出限为0.1μg/kg,定量限为0.3μg/kg;碱性橙2、碱性嫩黄O、碱性紫5BN和罗丹明B的线性范围为1.0~50μg/kg,相关系数均大于0.99。在2,10和50μg/kg三个添加水平下平均回收率为86.5%~108.3%,相对标准偏差为2.01%~7.91%。该方法简单、灵敏度高、结果准确可靠,可用于食品中四种碱性工业染料的同时测定。
A method was developed for determination of four industrial basic dyes(chrysoidine G, auramine O, basic violet 5BN, and rhodamine B) in foods using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Samples were extracted with acetonitrile solution and then cleaned up by WCX solid phase extraction cartridge. The target analytes were separated on an Agilent Zorbax Eclipse Plus C_18 column(2.1 mm×50 mm, 1.8 μm) with gradient elution using acetonitrile and 5 mmol/L ammonium acetate with 0.1%(volume ration) formic acid as mobile phases. Four basic dyes were determined by multiple reactions monitoring(MRM) mode with electrospray positive ion soure, and quantified by black matrix external standard. Under the optimal experimental conditions, LOD of chrysoidine G was 0.2 μg/kg, and LOQ was 0.6 μg/kg. LODs of auramine O, basic violet 5BN and rhodamine B were all 0.1 μg/kg, LOQs were all 0.3 μg/kg. The method showed a good linearity of chrysoidine G, auramine O, basic violet 5BN and rhodamine B in the range of 1.0~50 μg/kg with correlation coefficients more than 0.99. The average recoveries for samples spiked at three levels(2, 10 and 50 μg/kg) were ranged from 86.5% to 108.3%, and the relative standard deviations(RSD) from 2.01% to 7.91%. This method was simple, sensitive, accurate and reliable, which was suitable for the simultaneous determination of the four industrial basic dyes in foods.
出处
《食品工业》
CAS
北大核心
2016年第5期278-282,共5页
The Food Industry
基金
广东省专业镇中小微企业服务平台建设项目(2013B091604003)
动物源性食品安全监测技术研究和公共服务平台(粤科规财字[2014]208号)
作者简介
通讯作者