Chen YiQuan, Chen JinFa, Xi Zhiming, Yang Guidi, Wu Zujian, Li JianRong, Fu FengFu
Department of Chemistry, Key Laboratory of Analysis and Detection for Food Safety of Ministry of Education, Fujian Provincial Key Laboratory of Analysis and Detection for Food Safety, Fuzhou University, Fuzhou, Fujian, P. R. China.
Department of Plant Protection, Fujian Agriculture and Forest University, Fuzhou, Fujian, P. R. China.
Electrophoresis. 2015 May;36(9-10):1208-15. doi: 10.1002/elps.201500015. Epub 2015 Apr 20.
We herein reported a method for the simultaneous detection of trace Cr(VI), Cr(III), and chromium(III) picolinate (CrPic) in foods using CE-ICP-MS together with ultrasonic-assisted extraction. The Cr(III) (Cr(3+) ) was chelated with trans-1,2-diaminocyclohexane-N,N,N´,N´-tetraacetic acid (DCTA) to form a single charged Cr-DCTA(-) complex. Then, Cr(VI) (CrO4 (2-) ), Cr-DCTA(-) , and CrPic were separated by CE within 8 min under a separation voltage of -13 KV followed by their monitoring with ICP mass spectrometer (ICP-MS). The proposed method is simple, effective, and sensitive. It has an instrument detection limit of 0.10, 0.18, and 0.20 ngCr/mL for Cr(VI), Cr(III), and CrPic, respectively. With the help of the methods, we have successfully determined Cr(VI), Cr(III), and CrPic in nutritional supplement (CrPic yeast tablet) with an RSD (n = 5) <6% and a recovery of 93-103%. The experimental results showed that CrPic was the main speciation of chromium in the nutritional supplement, with a concentration of 1514.6 μg Cr/g.
我们在此报道了一种使用毛细管电泳-电感耦合等离子体质谱联用技术(CE-ICP-MS)并结合超声辅助萃取法同时检测食品中痕量六价铬(Cr(VI))、三价铬(Cr(III))和吡啶甲酸铬(CrPic)的方法。三价铬(Cr(3+))与反式-1,2-二氨基环己烷-N,N,N´,N´-四乙酸(DCTA)螯合形成单电荷的Cr-DCTA(-)络合物。然后,在-13 KV的分离电压下,Cr(VI)(CrO4 (2-))、Cr-DCTA(-)和CrPic在8分钟内通过毛细管电泳分离,随后用电感耦合等离子体质谱仪(ICP-MS)进行监测。所提出的方法简单、有效且灵敏。对于Cr(VI)、Cr(III)和CrPic,其仪器检测限分别为0.10、0.18和0.20 ngCr/mL。借助该方法,我们成功测定了营养补充剂(吡啶甲酸铬酵母片)中的Cr(VI)、Cr(III)和CrPic,相对标准偏差(RSD,n = 5)<6%,回收率为93 - 103%。实验结果表明,吡啶甲酸铬是该营养补充剂中铬的主要存在形态,浓度为1514.6 μg Cr/g。