本文選題：LC-ESI-MS　切入點：固相萃取　出處：《天津科技大學(xué)》2013年碩士論文

【摘要】：酸性橙和堿性橙是用于絲綢、纖維、羊毛等染色的兩類合成工業(yè)染料,由于這兩類合成工業(yè)染料廉價且易于著色,很多不法商販為牟取暴利將這些合成工業(yè)染料非法添加到食品中。因此建立一種高準(zhǔn)確度和高靈敏度的方法來檢測這兩類合成工業(yè)染料有重要意義。本論文主要研究了四種酸性橙(酸性橙6、酸性橙20、酸性橙52、酸性橙7和三種堿性橙(堿性橙2、堿性橙21、堿性橙22)的分離檢測方法。實驗采用超聲波輔助提取、X-AW混合弱陰離子交換柱凈化、Zorbax Elipse Plus C18柱(2.1×150 mm i.d.,3.5μm)梯度洗脫分離、LC-MS檢測,建立了同時測定食品中四種酸性橙和三種堿性橙的高靈敏度、高準(zhǔn)確度的檢測方法。實驗主要優(yōu)化了儀器的質(zhì)譜條件、液相色譜分離條件、固相萃取凈化條件和從食品基質(zhì)中提取七種工業(yè)染料的條件,最終建立了在Zorbax Elipse Plus C18柱(2.1×150 mmi.d.,3.5μm)上,用水(pH值為9,A)與乙腈(B)(60：40,v/v)作為初始流動相0.3 mL/min進(jìn)行梯度洗脫,在電噴霧離子源(ESI)的負(fù)離子和正離子檢測模式下分別對酸性橙和堿性橙進(jìn)行檢測的方法。實驗結(jié)果表明,該實驗方法在5-500μg/L內(nèi)線性范圍良好,相關(guān)系數(shù)大于0.9998,測定其峰面積的標(biāo)準(zhǔn)偏差(RSD)在2.93%-10.72%之間,儀器檢出限在0.5-1μg/L。實驗所建立的檢測方法的方法檢出限(LOD)在0.5-3μg/L,在加標(biāo)濃度為10μg/kg、50μg/kg、100μg/kg時,三種樣品的加標(biāo)回收率在74.13%-125.60%之間,相對標(biāo)準(zhǔn)偏差(RSDs)為2.22%-25.37%,說明建立的方法可以準(zhǔn)確的對食品中非法添加的酸性橙和堿性橙進(jìn)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.
【學(xué)位授予單位】：天津科技大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2013
【分類號】：R155.5;O657.63

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