Khalikova Maria A, Satínský Dalibor, Smidrkalová Tereza, Solich Petr
Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Heyrovského 1203, 500 05 Hradec Králové, Czech Republic.
Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Heyrovského 1203, 500 05 Hradec Králové, Czech Republic.
Talanta. 2014 Dec;130:433-41. doi: 10.1016/j.talanta.2014.07.038. Epub 2014 Jul 21.
The presented work describes the development of a simple, fast and effective on-line SPE-UHPLC-UV/vis method using fused core particle columns for extraction, separation and quantitative analysis of the nine illegal dyes, most frequently found in chilli-containing spices. The red dyes Sudan I-IV, Sudan Red 7B, Sudan Red G, Sudan Orange G, Para Red, and Methyl Red were separated and analyzed in less than 9 min without labor-consuming pretreatment procedure. The chromatographic separation was performed on Ascentis Express RP-Amide column with gradient elution using mixture of acetonitrile and water, as a mobile phase at a flow rate of 1.0 mL min(-1) and 55°C of temperature. As SPE sorbent for cleanup and pre-concentration of illegal dyes short guard fused core column Ascentis Express F5 was used. The applicability of proposed method was proven for three different chilli-containing commercial samples. Recoveries for all compounds were between 90% and 108% and relative standard deviation ranged from 1% to 4% for within- and from 2% to 6% for between-day. Limits of detection showed lower values than required by European Union regulations and were in the range of 3.3-10.3 µg L(-1) for standard solutions, 5.6-235.6 µg kg(-1) for chilli-containing spices.
本文介绍了一种简单、快速且有效的在线固相萃取-超高效液相色谱-紫外/可见分光光度法的开发,该方法使用熔融核颗粒柱对含辣椒香料中最常见的九种非法染料进行萃取、分离和定量分析。红色染料苏丹红I-IV、苏丹红7B、苏丹红G、苏丹橙G、对位红和甲基红在不到9分钟内即可分离并分析,无需耗时的预处理程序。色谱分离在Ascentis Express RP-酰胺柱上进行,使用乙腈和水的混合物作为流动相,以1.0 mL min(-1)的流速和55°C的温度进行梯度洗脱。作为用于净化和预浓缩非法染料的固相萃取吸附剂,使用了短保护熔融核柱Ascentis Express F5。所提出方法的适用性在三种不同的含辣椒商业样品中得到了验证。所有化合物的回收率在90%至108%之间,日内相对标准偏差范围为1%至4%,日间相对标准偏差范围为2%至6%。检测限低于欧盟法规要求的值,标准溶液的检测限在3.3-10.3 µg L(-1)范围内,含辣椒香料的检测限在5.6-235.6 µg kg(-1)范围内。