超声辅助分散乳液微萃取/高效液相色谱法同时测定辣椒粉中的5种染色剂  

Simultaneous Determination of Five Dyes in Chilli Powder by Ultrasonicassisted Dispersive Emulsion Microextraction Coupled with High Performance Liquid Chromatography

作　　者：苏日辉 阮贵华[1] 曾令镇 陈正毅[1] 杜甫佑[1] 

机构地区：[1]桂林理工大学化学与生物工程学院,广西桂林541004

出　　处：《分析测试学报》2015年第5期546-551,共6页Journal of Instrumental Analysis

基　　金：国家自然科学基金(21065003;21265004);广西自然科学基金(2014GXNSFAA118064)

摘　　要：建立了超声辅助分散乳液微萃取技术结合高效液相色谱法（HPLC）同时测定辣椒粉中对位红、苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ的方法。考察了萃取剂的种类及其体积、分散剂体积分数、盐效应、p H值、萃取时间和离心时间等因素对萃取效果的影响,确定最佳萃取条件为：0.75 m L环己烷为萃取剂,10%乙腈为分散剂,振荡1 min,以6 000 r/min离心5 min,吸取萃取相过0.22μm有机尼龙滤头,进行HPLC分析。最优条件下,在辣椒粉中分别添加50,250,1 000 ng/g 3个水平的染色剂,测得市售散装、包装辣椒粉中5种染色剂的加标回收率为82%~114%,相对标准偏差（RSD,n=3）为0.7%~8.8%。所有目标化合物在25~5 000 ng/m L范围内线性良好,相关系数（r2）均不小于0.998 9;检出限为1~11 ng/m L。本方法具有简单快捷、灵敏准确等特点,满足辣椒粉中5种染色剂检测的要求。A method based on ultrasonic-assisted dispersive emulsion microextraction procedure coupled with high performance liquid chromatography（ HPLC） was developed for the preconcentration and determination of Para red,Sudan Ⅰ,Sudan Ⅱ,Sudan Ⅲ and Sudan Ⅳ in chilli powder. Experimental conditions affecting the microextraction procedure such as types and volumes of extraction solvent,content of disperser solvent, salt concentration, p H value, extraction time and centrifugal time were optimized. The ultrasonic-assisted dispersive emulsion microextraction conditions were optimized by using 0. 75 m L cyclohexane as extraction solvent and 10% acetonitrile as disperser solvent,and the mixture was oscillated for 1 min. The extractant phase was separated by centrifugation at6 000 r / min for 5 min,then filtered through 0. 22 μm nylon membranes and injected into the HPLC system for analysis. Under the optimum conditions,this method was employed to analyze five dyes in loose chilli powder and packaging chilli powder. At three spiked levels of 50-1 000 ng / g,the average recoveries for five dyes in chilli powder ranged from 82% to 114%,with relative standard deviations（ RSD,n = 3） between 0. 7% and 8. 8%. The calibration curves of 5 dyes were linear in the concentration range of 25-5 000 ng / m L with correlation coefficients（ r2） not less than 0. 998 9 and limits of detection（ LOD） of 1-11 ng / m L. This method is convenient,sensitive and accurate,and is suitable for the determination and confirmation of 5 dyes in chilli powder.

关 键 词：对位红 苏丹红 超声辅助分散乳液微萃取 高效液相色谱(HPLC) 

分 类 号：O657.7[理学—分析化学] TS193.2[理学—化学]