应用化学 ›› 2020, Vol. 37 ›› Issue (7): 816-822.DOI: 10.11944/j.issn.1000-0518.2020.07.200017

• 研究论文 • 上一篇    下一篇

正相高效液相色谱法分析壬基环己醇聚氧乙烯醚中残留壬基环己醇

胡学一a, 胡益涛a, 方云a,*, 夏咏梅a, 钱飞b   

  1. a江南大学化学与材料工程学院,合成与生物胶体教育部重点实验室 江苏 无锡 214122;
    b江苏凌飞科技股份有限公司 江苏 无锡 214264
  • 收稿日期:2020-01-15 出版日期:2020-07-01 发布日期:2020-07-07
  • 通讯作者: 方云,教授; Tel:0510-85917920; E-mail:yunfang@126.com; 研究方向:胶体与界面化学
  • 基金资助:
    国家重点研发计划(2017YFB0308904)资助

Quantitative Analysis of Residual Nonylcyclohexanol in Nonylcyclohexanol Polyoxyethylene Ethers by Normal Phase High Performance Liquid Chromatography

HU Xueyia, HU Yitaoa, FANG Yuna,*, XIA Yongmeia, QIAN Feib   

  1. aThe Key Laboratory of Synthetic and Biological ColloidsMinistry of Education,School of Chemical and Materials Engineering,Jiangnan University,Wuxi,Jiangsu 214122,China;
    bJiangsu Lingfei Technology Co.,Ltd.,Wuxi,Jiangsu 214264,China
  • Received:2020-01-15 Published:2020-07-01 Online:2020-07-07
  • Contact: FANG Yun, professor; Tel:0510-85917920; E-mail:yunfang@126.com; Research interests:colloid and interface chemistry
  • Supported by:
    Supported by the National Key Research and Development Plan of China(No.2017YFB0308904)

摘要: 壬基环己醇聚氧乙烯醚(NCEOn)是非环境友好型壬基酚聚氧乙烯醚(NPEOn)潜在的升级换代产品。 本文采用正相高效液相色谱法(NP HPLC)测定产品中残存壬基环己醇(NC),用Weilbull法测定其中聚乙二醇(PEG)含量,用电喷雾电离质谱法评价聚氧乙烯(PEO)多分散指数(PDI),以此鉴定NCEOn的品质。 为了建立快速分析NCEOn产品中NC含量的方法,以满足跟踪检测的需求,本文筛选了反相HPLC和NP HPLC两类5种方法,并进行比较和初步条件优化,确定了用Inertsil NH2色谱柱和示差折光检测器以及乙酸乙酯为洗脱液的NP HPLC法定量分析NC,方法的回收率为91.77%~107.6%,相对标准偏差为4.46%,最低检测限为9.8 μg/mL。 经测定,NCEO7和NCEO9产品中NC的残留量分别为0.158%和0.139%,PEG质量分数为7.1%和7.3%,PDI为85.0%和88.6%,证实NCEOn产品具有NC残留量少、PEG含量低和产品PEO窄分布特征,具有在化妆品或个人洗护用品等民用产品中替代NPEOn的潜能。

关键词: 壬基环己醇聚氧乙烯醚, 壬基环己醇, 高效液相色谱, 分析, 壬基酚聚氧乙烯醚

Abstract: Nonylcyclohexanol polyoxyethylene ethers (NCEOn) are novel potential upgraded products for replacing the non-eco-friendly nonylphenol polyoxyethylene ethers (NPEOn). The product qualities of NCEOn were determined revolving the residual nonylcyclohexanol (NC) by normal phase high performance liquid chromatography (NP HPLC), the polyethylene glycol (PEG) content by Weilbull procedure and the polydispersity index (PDI) by electrospray ionization mass spectrometry (ESI MS) technique. An NP HPLC program was finally proposed for rapidly determining the residual NC in NCEOn by combining an Inertsil NH2 column, a refractive index detector with the eluent of ethyl acetate on the basis of five preliminary experiments of NP HPLC and reversed phase HPLC. This setup achieves a recovery of 91.77%~107.6%, a relative standard deviation (RSD) of 1.59%~4.46% and a limit of detection (LOD) 9.8 μg/mL. NCEO7 and NCEO9 contain 0.158% and 0.139% of NC, and 7.1% and 7.3% of PEG, respectively, which indicates that the NCEOn products have good qualities with a low NC residue, a low PEG content and a narrow distribution characteristic. Therefore, NCEOn is a potential substitute of NPEOn used in daily chemicals such as cosmetics, personal care products and toiletries.

Key words: nonylcyclohexanol polyoxyethylene ether, nonylcyclohexanol, high performance liquid chromatography, analysis, nonylphenol polyoxyethylene ether