U. S. Food and Drug Administration, Office of Regulatory Science, CFSAN, 5001 Campus Drive, College Park, MD 20740, USA.
J Chromatogr A. 2019 Dec 6;1607:460400. doi: 10.1016/j.chroma.2019.460400. Epub 2019 Jul 26.
1,4-dioxane is a potential human carcinogen and contaminant produced during the manufacturing process from specific cosmetic ingredients, such as certain detergents and emulsifiers. As such, 1,4-dioxane is not identified on product ingredient labels. To assess the concentration of 1,4-dioxane in cosmetic products, a gas chromatography-tandem mass spectrometry (GC-MS/MS) method using pulsed split injection and electron ionization was developed and validated. For liquid cosmetic products such as shampoo and lotion, test portions were extracted using fast ultrasound-assisted extraction (UAE) procedure without sample cleanup. For solid products (e.g. beauty bars), a C solid phase extraction (SPE) procedure was optimized to reduce potential interferences. The corresponding stable isotopically labeled analogue (1,4-dioxane-d) was selected as an internal standard to compensate for matrix effects and sample recovery. Method recovery experiments were performed in lotion, oil gel, hair detangler, bubble bath and beauty bar (solid) sample matrices with recoveries of 84-108% and relative standard deviations less than 5% at three spike concentrations. Method limits of detection (LOD) and quantification (LOQ) for 1,4-dioxane were determined at 0.2 μg/g and 0.5 μg/g, respectively. The method was successfully used to determine 1,4-dioxane in 82 leave-on and rinse-off cosmetic products marketed toward children including bath products, hair treatment, lotions, beauty bars, washes, shampoos, and other products. 1,4-dioxane was detected in 47 of the 82 products with an average concentration of 1.54 μg/g (range: 0.23-15.3 μg/g). The method can increase sample throughput and reduce matrix-induced interferences.
1,4-二恶烷是一种潜在的人类致癌物质和污染物，在某些化妆品成分（如某些清洁剂和乳化剂）的制造过程中产生。因此，1,4-二恶烷不会在产品成分标签上标识。为了评估化妆品产品中 1,4-二恶烷的浓度，开发并验证了一种使用脉冲分流注射和电子电离的气相色谱-串联质谱（GC-MS/MS）方法。对于洗发水和乳液等液体化妆品产品，测试部分使用快速超声辅助提取（UAE）程序提取，无需样品净化。对于固体产品（例如美容棒），优化了 C 固相萃取（SPE）程序以减少潜在的干扰。选择相应的稳定同位素标记类似物（1,4-二恶烷-d）作为内标，以补偿基质效应和样品回收率。在乳液、油凝胶、头发梳理剂、泡泡浴和美容棒（固体）样品基质中进行方法回收率实验，回收率为 84-108%，三个加标浓度下的相对标准偏差小于 5%。1,4-二恶烷的方法检出限（LOD）和定量限（LOQ）分别为 0.2μg/g 和 0.5μg/g。该方法成功用于测定 82 种市售儿童用的留用和冲洗型化妆品中的 1,4-二恶烷，包括沐浴产品、头发处理、乳液、美容棒、清洁剂、洗发水和其他产品。在 82 种产品中的 47 种产品中检测到 1,4-二恶烷，平均浓度为 1.54μg/g（范围：0.23-15.3μg/g）。该方法可以提高样品通量并减少基质诱导的干扰。
