College of Pharmacy, Kyung Hee University, Seoul 130-701, South Korea.
J Chromatogr A. 2013 Jul 5;1297:186-95. doi: 10.1016/j.chroma.2013.04.064. Epub 2013 Apr 29.
A novel analysis strategy was created for comprehensive qualitative and quantitative impurity profiling of the coloring agent Sudan III by gas chromatography/mass spectrometry (GC/MS). The identification of impurities in commercial Sudan III was performed by GC/MS combined with trimethylsilylation (TMS). A total of 24 impurities were identified or tentatively characterized in commercial Sudan III dyes by GC/MS and were mainly classified as phenylazo and naphtholazo analogs. Four new impurities with coplanar structures, suspected of being toxic compounds, were observed in commercial Sudan III dyes. For further identification and sensitive detection of polar impurities, an extract was trimethylsilyl-derivatized to improve the GC chromatographic properties and mass spectrometric detection sensitivity. On the basis of the impurities identified by GC/MS, pathways for the formation of the major impurities during the manufacture of Sudan III were suggested. Four impurities regulated by the EU commission and the US Code of Federal Regulations (CFR) in Sudan III were quantified by GC/MS-scan mode. Method validation was conducted to determine linearity, precision, accuracy, and limit of quantification (LOQ). The linear dynamic range extended from 0.001 to 4.0%, with a correlation coefficient (R(2)) greater than 0.997 for GC/MS. The LOQs of the impurities ranged from 2.73 to 4.39μg/g for GC/MS. Based on the established method, the levels of regulated impurities in five commercial Sudan III dyes manufactured by different chemical companies were successfully determined. This study provides very useful information for the quality control of Sudan III and evaluation of its manufacture.
创建了一种新的分析策略，用于通过气相色谱/质谱法（GC/MS）对着色剂苏丹红 III 进行全面的定性和定量杂质分析。通过 GC/MS 结合三甲基硅烷化（TMS）对商业苏丹红 III 中的杂质进行鉴定。通过 GC/MS 鉴定并初步表征了商业苏丹 III 染料中的 24 种杂质，主要分为偶氮苯和萘酚偶氮类似物。在商业苏丹 III 染料中观察到四种具有共面结构的新杂质，疑似为有毒化合物。为了进一步鉴定和灵敏检测极性杂质，将提取物进行三甲基硅烷基化衍生化，以改善 GC 色谱性能和质谱检测灵敏度。基于 GC/MS 鉴定的杂质，提出了苏丹红 III 制造过程中主要杂质形成的途径。采用 GC/MS-扫描模式对欧盟委员会和美国联邦法规（CFR）规定的苏丹红 III 中的四种杂质进行定量。通过线性、精密度、准确度和定量限（LOQ）进行方法验证。GC/MS 的线性动态范围从 0.001 扩展到 4.0%，相关系数（R²）大于 0.997。杂质的 LOQ 范围为 2.73 至 4.39μg/g。基于建立的方法，成功测定了五个不同化学公司生产的商业苏丹红 III 染料中规定杂质的水平。本研究为苏丹红 III 的质量控制和制造评估提供了非常有用的信息。
