LC-MS检测食品中的非法添加物酸性橙和碱性橙

发布时间：2018-04-03 23:53

本文选题：LC-ESI-MS　切入点：固相萃取　出处：《天津科技大学》2013年硕士论文

【摘要】：酸性橙和碱性橙是用于丝绸、纤维、羊毛等染色的两类合成工业染料,由于这两类合成工业染料廉价且易于着色,很多不法商贩为牟取暴利将这些合成工业染料非法添加到食品中。因此建立一种高准确度和高灵敏度的方法来检测这两类合成工业染料有重要意义。本论文主要研究了四种酸性橙(酸性橙6、酸性橙20、酸性橙52、酸性橙7和三种碱性橙(碱性橙2、碱性橙21、碱性橙22)的分离检测方法。实验采用超声波辅助提取、X-AW混合弱阴离子交换柱净化、Zorbax Elipse Plus C18柱(2.1×150 mm i.d.,3.5μm)梯度洗脱分离、LC-MS检测,建立了同时测定食品中四种酸性橙和三种碱性橙的高灵敏度、高准确度的检测方法。实验主要优化了仪器的质谱条件、液相色谱分离条件、固相萃取净化条件和从食品基质中提取七种工业染料的条件,最终建立了在Zorbax Elipse Plus C18柱(2.1×150 mmi.d.,3.5μm)上,用水(pH值为9,A)与乙腈(B)(60：40,v/v)作为初始流动相0.3 mL/min进行梯度洗脱,在电喷雾离子源(ESI)的负离子和正离子检测模式下分别对酸性橙和碱性橙进行检测的方法。实验结果表明,该实验方法在5-500μg/L内线性范围良好,相关系数大于0.9998,测定其峰面积的标准偏差(RSD)在2.93%-10.72%之间,仪器检出限在0.5-1μg/L。实验所建立的检测方法的方法检出限(LOD)在0.5-3μg/L,在加标浓度为10μg/kg、50μg/kg、100μg/kg时,三种样品的加标回收率在74.13%-125.60%之间,相对标准偏差(RSDs)为2.22%-25.37%,说明建立的方法可以准确的对食品中非法添加的酸性橙和碱性橙进行定量。
[Abstract]:Acid orange and alkaline orange are two kinds of synthetic industrial dyes used in silk, fiber and wool dyeing.Many illegal traders illegally add these synthetic industrial dyes to food for profiteering.Therefore, it is important to establish a high accuracy and high sensitivity method for the detection of these two synthetic industrial dyes.In this paper, four kinds of acid orange (acid orange 6, acid orange 20, acid orange 52, acid orange 7) and three basic oranges (alkaline orange 2, alkaline orange 21, alkaline orange 22) were studied.Ultrasonic assisted extraction of X-AW mixed weak anion exchange column was used to purify Zorbax Elipse Plus C18 column (2.1 脳 150mm i.d.f. 3.5 渭 m) gradient elution and separation. The high sensitivity of simultaneous determination of four acidic oranges and three basic oranges in food was established.A high accuracy detection method.The conditions of mass spectrometry, separation by liquid chromatography, purification by solid phase extraction and extraction of seven kinds of industrial dyes from food matrix were optimized. Finally, the conditions were established on Zorbax Elipse Plus C18 column 2.1 脳 150mmi.d.k. 3.5 渭 m).The initial mobile phase was #number0# mL/min for gradient elution. The acid orange and alkaline orange were detected in the mode of anion and positive ion detection in the electrospray ion source (ESI), respectively, and the pH value of the water was 9a) and acetonitrile was 60: 40v / v / v) as the initial mobile phase, and the acid orange and the alkaline orange were detected respectively under the mode of anion and positive ion detection in the electrospray ion source (ESI).The experimental results show that the linear range of the method is good in the range of 5-500 渭 g / L, the correlation coefficient is greater than 0.9998, the standard deviation (RSDs) for the determination of the peak area is between 2.93-10.72% and the detection limit of the instrument is 0.5-1 渭 g / L.The detection limit of the method was 0.5-3 渭 g / L, and the standard concentration was 10 渭 g / kg ~ 50 渭 g / kg ~ (-1) 渭 g/kg. The recoveries of the three samples ranged from 74.13% to 125.60%.The relative standard deviation (RSDs) was 2.22- 25.37, which indicated that the established method could be used to quantify the acid orange and alkaline orange added illegally in food.
【学位授予单位】：天津科技大学
【学位级别】：硕士
【学位授予年份】：2013
【分类号】：R155.5;O657.63

【相似文献】