色谱

色谱 ›› 2012, Vol. 30 ›› Issue (09): 870-875.DOI: 10.3724/SP.J.1123.2012.04014

• 研究论文 • 上一篇    下一篇

高效液相色谱法同时测定染发剂中11种氨基苯酚

祝伟霞1, 王彩娟2, 杨冀州1*, 魏蔚1, 孙转莲1, 张书胜2   

  1. 1. 河南出入境检验检疫局, 河南 郑州 450003; 2. 郑州大学化学与分子工程学院, 河南 郑州 450042
  • 收稿日期:2012-04-09 修回日期:2012-05-22 出版日期:2012-09-28 发布日期:2012-09-20
  • 通讯作者: 杨冀州,研究员,主要从事色谱分析研究工作. Tel: (0371)65685749, E-mail: jizhouyang@163.com.
  • 基金资助:

    河南省科技攻关项目(122102110167)和质检总局制修订项目(2009B102).

Simultaneous determination of 11 aminophenols in hair dyes by high performance liquid chromatography

ZHU Weixia1, WANG Caijuan2, YANG Jizhou1*, WEI Wei1, SUN Zhuanlian1, ZHANG Shusheng2   

  1. 1. Henan Entry-Exit Inspection and Quarantine Bureau, Zhengzhou 450003, China; 2. College of Chemistry and Molecular Engineering of Zhengzhou University, Zhengzhou 450042, China
  • Received:2012-04-09 Revised:2012-05-22 Online:2012-09-28 Published:2012-09-20

PDF

547

被引次数

20

摘要： 建立了高效液相色谱测定直接型与氧化型染发剂中11种氨基苯酚含量的分析方法。样品在亚硫酸氢钠的保护下用甲醇提取,高速冷冻离心净化;采用Agilent Zorbax SB C18色谱柱分离,流动相为5 mmol/L庚烷磺酸钠-40 mmol/L pH 2.8磷酸盐缓冲液和乙腈,梯度洗脱,11种氨基苯酚分别于230、270和400 nm下检测。11种氨基苯酚在0.05～500 mg/L线性范围内相关系数不小于0.9992,4-氨基-3-硝基苯酚、2-氨基-5-硝基苯酚、3-硝基-4-(2-羟乙基)氨基苯酚的方法定量限为5 mg/kg,其他8种氨基苯酚包括对氨基苯酚、对甲氨基苯酚、间氨基苯酚、邻氨基苯酚、5-氨基-2-甲基苯酚、4-氨基-3-甲基苯酚、2-甲基-5-(2-羟乙基)氨基苯酚和2-氨基-4-硝基苯酚定量限为20 mg/kg,方法回收率为88.5%～109.5%,相对标准偏差为2.2%～8.3%。测定了多种市售染发剂,结果表明该方法操作简单、测定结果准确,可用于直接型与氧化型染发剂中11种氨基苯酚的测定。

关键词: 氨基苯酚, 多波长, 高效液相色谱, 冷冻离心, 染发剂

Abstract: An analytical method was developed for the simultaneous determination of 11 aminophenols in direct and oxidized hair dyes by high performance liquid chromatography (HPLC). The samples were extracted with methanol using sodium bisulfite for anti-oxidation. The purification was carried out with the high speed frozen centrifugation. The separation was performed on an Agilent Zorbax SB C18 column with the mobile phases of acetonitrile and an ion pair system of sodium heptanesulfonate and phosphate under a gradient elution. The analytes were detected at three different wavelengths of 230, 270 and 400 nm. In the concentration range of 0.05~500 mg/L, the correlation coefficients for the 11 aminophenols were not less than 0.9992. The limits of quantification including 4-amino-3-nitrophenol, 2-amino-5-nitrophenol, and 4-(2-hydroxyethyl)amino-3-nitrophenol were 5 mg/kg. Other aminophenols including 4-aminophenol, 4-methyl aminophenol, 3-aminophenol, 2-aminophenol, 5-amino-o-cresol, 4-amino-3-methylphenol, 5-(2-hydroxyethyl)amino-o-cresol and 2-amino-4-nitrophenol were 20 mg/kg. The recoveries of the aminophenols spiked at different levels ranged from 88.5% to 109.5% with the relative standard deviations (RSDs) within the range of 2.2%~8.3%. The commercially available hair dye samples were analyzed for the aminophenols and the results showed that the method was suitable for the determination of the 11 aminophenols in direct and oxidized hair dyes.

Key words: aminophenols, frozen centrifugation, hair dye, multi-wavelength, high performance liquid chromatography (HPLC)