高效液相色谱法测定化妆品中禁用芳香胺1-萘胺和2-萘胺及其盐类  

Determination of prohibited aromatic amines of 1-naphthylamine and 2-naphthylamine and their salts in cosmetics by high-performance liquid chromatography

作　　者：孟宪双[1] 牛增元 罗忻 刘艺静 白桦[1] 马强[1] 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)

机构地区：[1]中国检验检疫科学研究院,北京100176 [2]青岛海关技术中心,青岛266109 [3]北京中医药大学中药学院,北京102488

出　　处：《分析试验室》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。

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.

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 

分 类 号：O657.7[理学—分析化学]