Zhou Wanlong, Wang Perry G, Wittenberg James B, Rua Diego, Krynitsky Alexander J
U.S. Food and Drug Administration, Office of Regulatory Science, CFSAN/HFS-717, 5100 Paint Branch Parkway, College Park, MD 20740-3835, USA.
U.S. Food and Drug Administration, Office of Regulatory Science, CFSAN/HFS-717, 5100 Paint Branch Parkway, College Park, MD 20740-3835, USA.
J Chromatogr A. 2016 May 13;1446:134-40. doi: 10.1016/j.chroma.2016.04.003. Epub 2016 Apr 2.
A rapid and sensitive gas chromatography with tandem mass spectrometry (GC-MS/MS) method has been developed and validated to quantitatively determine cosmetic ingredients, such as toluene, N-methylpyrrolidone, 2,4-dihydroxybenzophenone (benzophenone-1, BP-1), and diethylene glycol dimethacrylate, in nail products. In this procedure, test portions were extracted with acetone, followed by vortexing, sonication, centrifugation, and filtration. During the extraction procedure, BP-1 was derivatized making it amenable to GC-MS analysis, using N,O-bis(trimethylsilyl)trifluoroacetamide. The four ingredients were quantified by GC-MS/MS in an electron ionization mode. Four corresponding stable isotopically labeled analogues were selected as internal standards, which were added at the beginning of the sample preparation to correct for recoveries and matrix effects. The validated method was used to screen 34 commercial nail products for these four cosmetic ingredients. The most common ingredients detected in the nail products were toluene and BP-1. Toluene was detected in 26 products and ranged from 1.36 to 173,000μg/g. BP-1 ranged from 18.3 to 2,370μg/g in 10 products.
已开发并验证了一种快速灵敏的气相色谱-串联质谱法（GC-MS/MS），用于定量测定美甲产品中的化妆品成分，如甲苯、N-甲基吡咯烷酮、2,4-二羟基二苯甲酮（二苯甲酮-1，BP-1）和二乙二醇二甲基丙烯酸酯。在此过程中，用丙酮提取测试部分，然后进行涡旋、超声处理、离心和过滤。在提取过程中，使用N,O-双（三甲基硅基）三氟乙酰胺对BP-1进行衍生化，使其适合GC-MS分析。通过GC-MS/MS在电子电离模式下对这四种成分进行定量。选择了四种相应的稳定同位素标记类似物作为内标，在样品制备开始时加入以校正回收率和基质效应。经验证的方法用于筛选34种商业美甲产品中的这四种化妆品成分。美甲产品中检测到的最常见成分是甲苯和BP-1。在26种产品中检测到甲苯，含量范围为1.36至173000μg/g。在10种产品中，BP-1的含量范围为18.3至2370μg/g。
