摘要
建立了化妆品中禁用芳香胺1-萘胺和2-萘胺同分异构体及其盐类的高效液相色谱分析方法。膏霜和乳液类试样依次经氯化钠破乳、溶剂萃取;水剂类试样直接经超声辅助溶剂萃取。萃取液经Waters Sep-Pak C18固相萃取柱净化后由XBridge BEH Phenyl色谱柱分离,以0.02 mol/L磷酸二氢钠溶液和甲醇为流动相梯度洗脱,二极管阵列检测器测定,检测波长240 nm,外标法定量。在优化的样品前处理和色谱条件下,1-萘胺和2-萘胺实现基线分离,检出限和定量限分别为0.5μg/kg和1.0μg/kg,平均回收率为88.7%~107.3%,相对标准偏差为2.3%~6.8%。该方法解决了法规明确而技术空白的问题,适用于化妆品的日常检验及质量控制。
A high-performance liquid chromatography(HPLC) method was established for the analysis of the prohibited aromatic amines of 1-naphthylamine and 2-naphthylamine isomers and their salts in cosmetics.The cream and emulsion samples were successively demulsified by sodium chloride and extracted by solvent,while the lotion samples were directly subjected to ultrasound-assisted solvent extraction.And the extracts were purified by a Waters Sep-Pak C18 solid-phase extraction column and separated by an XBridge BEH Phenyl chromatographic column,along with gradient elution using 0.02 mol/L sodium dihydrogen phosphate solution and methanol as mobile phase at detection wavelength of 240 nm with diode array detector,and quantified by external standard method.Under the optimized pretreatment and chromatographic conditions,1-naphthylamine and 2-naphthylamine were baseline separated.The limits of detection and limits of quantitation were 0.5 and 1.0 μg/kg,respectively.The average recoveries were 88.7%-107.3%,and the relative standard deviations were 2.3%-6.8%.The method could solve the problem of clear regulations but technical blank,and is suitable for daily inspection and quality control of cosmetics.
作者
孟宪双
牛增元
罗忻
刘艺静
白桦
马强
MENG Xianshuang;NIU Zengyuan;LUO Xin;LIU Yijing;BAI Hua;MA Qiang(Chinese Academy of Inspection and Quarantine,Beijing 100176,China;Technology Center of Qingdao Customs,Qingdao 266109,China;School of Chinese Materia Medica,Beijing University of Chinese Medicine,Beijing 102488,China)
出处
《分析试验室》
EI
CAS
CSCD
北大核心
2023年第10期1341-1346,共6页
Chinese Journal of Analysis Laboratory
基金
国家市场监督管理总局科技计划项目(2021MK162)
中央级公益性科研院所基本科研业务费专项资金资助项目(2022JK15)资助。
关键词
固相萃取
高效液相色谱法
禁用芳香胺
同分异构体
化妆品
solid-phase extraction
high-performance liquid chromatography
prohibited aromatic amines
iso-mers
cosmetics