Yang H H Wendy
U.S. Food and Drug Administration, Center for Food Safety and Applied Nutrition, Office of Cosmetics and Colors, College Park, MD 20740, USA.
J AOAC Int. 2017 Jan 1;100(1):230-235. doi: 10.5740/jaoacint.16-0067.
A new practical and time-saving ultra-high performance liquid chromatography (UHPLC) method has been developed for determining the organic impurities in the anthraquinone color additives D&C Violet No. 2 and D&C Green No. 6. The impurities determined are p-toluidine, 1-hydroxyanthraquinone, 1,4-dihydroxyanthraquinone, and two subsidiary colors. The newly developed UHPLC method uses a 1.7-μ particle size C-18 column, 0.1 M ammonium acetate and acetonitrile as eluents, and photodiode array detection. For the quantification of the impurities, six-point calibration curves were used with correlation coefficients that ranged from 0.9974 to 0.9998. Recoveries of impurities ranged from 99 to 104%. Relative standard deviations ranged from 0.81 to 4.29%. The limits of detection for the impurities ranged from 0.0067% to 0.216%. Samples from sixteen batches of each color additive were analyzed, and the results favorably compared with the results obtained by gravity-elution column chromatography, thin-layer chromatography, and isooctane extraction. Unlike with those other methods, use of the UHPLC method permits all of the impurities to be determined in a single analysis, while also reducing the amount of organic waste and saving time and labor. The method is expected to be implemented by the U.S. Food and Drug Administration for analysis of color additive samples submitted for batch certification.
已开发出一种新的实用且省时的超高效液相色谱（UHPLC）方法，用于测定蒽醌类色素添加剂D&C紫罗兰色号2和D&C绿色色号6中的有机杂质。所测定的杂质为对甲苯胺、1-羟基蒽醌、1,4-二羟基蒽醌以及两种副色。新开发的UHPLC方法使用粒径为1.7μm的C-18柱，以0.1M醋酸铵和乙腈作为洗脱剂，并采用光电二极管阵列检测。对于杂质的定量分析，使用了六点校准曲线，相关系数范围为0.9974至0.9998。杂质回收率范围为99%至104%。相对标准偏差范围为0.81%至4.29%。杂质的检测限范围为0.0067%至0.216%。对每种色素添加剂的16批样品进行了分析，结果与重力洗脱柱色谱法、薄层色谱法和异辛烷萃取法所得结果相比良好。与其他方法不同，使用UHPLC方法可以在一次分析中测定所有杂质，同时还减少了有机废物量，节省了时间和人力。预计美国食品药品监督管理局将采用该方法对提交批次认证的色素添加剂样品进行分析。
