固相萃取/高效液相色谱法同时测定化妆品中9种卤代酚残留  

Determination of Nine Halophenols Residues in Cosmetics by SPE/HPLC

作　　者：车文军[1] 武中平[1] 卢剑[1] 王莉[1] 王燕芹[2] 

机构地区：[1]江苏省产品质量监督检验研究院,江苏南京210007 [2]南京林业大学理学院,江苏南京210037

出　　处：《分析测试学报》2013年第4期499-503,共5页Journal of Instrumental Analysis

基　　金：国家标准化管理委员会计划项目(20101079-T-607)

摘　　要：建立了固相萃取/高效液相色谱(SPE/HPLC)测定化妆品中9种卤代酚(2,6-二氯酚、2,3-二氯酚、2,5-二氯酚、2,4-二氯酚、3,4-二氯酚、3,5-二氯酚、2,4,6-三氯苯酚、五氯苯酚和硫氯酚)含量的分析方法。试样经饱和氯化钠溶液分散,乙腈超声提取,HLB柱净化后,以甲醇-乙腈-乙酸铵缓冲溶液为流动相,经C8柱分离后进行HPLC检测。结果显示,9种卤代酚在1.0～50.0 mg/L范围内呈良好的线性关系,相关系数均大于0.999,检出限为0.3～0.6 mg/kg。在2.0、4.0、20.0 mg/kg 3个加标浓度水平下,9种卤代酚的平均回收率为92%～105%,相对标准偏差(RSD,n=6)为0.89%～3.1%。该方法灵敏度高、重现性好、定量准确。A solid phase extraction coupled with high performance liquid chromatographic （SPE/ HPLC） method was developed for the determination of nine halophenols, e.g. 2, 6-dichlorophenol, 2, 3-dichlorophenol, 2, 5-dichlorophenol, 2, 4-dichlorophenol, 3, 4-dichlorophenol, 3, 5-di- chlorophenol, 2, 4, 6-trichlorophenol, pentachlorophenol and bithionol, in cosmetics. The sam- ples were dispersed with saturated sodium chloride solution, extracted with acetonitrile under ultra- sonication, and cleaned up with HLB solid phase extraction. The separation of nine halophenols was carried out on a Cs column usingmethanol - acetonitrile - ammonium acetate buffer as mobile phase. The result indicated that the calibration curves of nine halophenols were linear between 1, 0 mg/L and 50. 0 mg/L, with correlation coefficients more than 0. 999. The limits of detection were in the range of 0. 3 - 0. 6 mg/kg. The mean recoveries of nine halophenols at spiked levels of 2. 0, 4. 0, 20. 0 mg/kg were in the range of 92% -105% , with RSDs（n =6） of 0. 89% -3.1%. The method was sensitive, reproducible and accurate.

关 键 词：高效液相色谱 固相萃取 化妆品 卤代酚 测定 

分 类 号：O657.72[理学—分析化学] O625.33[理学—化学]