色谱

色谱 ›› 2013, Vol. 31 ›› Issue (1): 64-70.DOI: 10.3724/SP.J.1123.2012.08046

• 研究论文 • 上一篇    下一篇

胶束电动毛细管色谱法同时测定复方化学消毒剂及日化产品中邻苯二甲醛、对氯间二甲基苯酚及三氯生

解娜1,2, 丁晓静2,3*, 宋宝花1,2, 李佳2,3, 王志1*   

  1. 1. 河北农业大学理学院, 河北 保定 071001; 2. 北京市疾病预防控制中心, 北京 100013; 3. 首都医科大学公共卫生与家庭医学学院, 北京 100069
  • 收稿日期:2012-08-27 修回日期:2012-10-10 出版日期:2013-01-28 发布日期:2013-01-21
  • 通讯作者: 丁晓静

Simultaneous determination of o-phthalaldehyde, p-chloro-m-xylenol and triclosan in compound chemical disinfectants and daily chemicals by micellar electrokinetic chromatography

XIE Na1,2, DING Xiaojing2,3*, SONG Baohua1,2, LI Jia2,3, WANG Zhi1*   

  1. 1. College of Sciences, Agricultural University of Hebei, Baoding 071001, China; 2. Beijing Center for Diseases Control and Prevention, Beijing 100013, China; 3. College of Public Health and Domestic Medicine, Capital Medical University, Beijing 100069, China
  • Received:2012-08-27 Revised:2012-10-10 Online:2013-01-28 Published:2013-01-21
  • Contact: Xiao JingDING

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187

被引次数

26

摘要： 建立了邻苯二甲醛(OPA)、对氯间二甲基苯酚(PCMX)和三氯生3种杀菌剂同时分离测定的胶束电动毛细管色谱(MEKC)新方法。详细研究了影响上述3种杀菌剂同时分离与准确定量的因素: 如分离缓冲溶液的浓度及pH,十二烷基硫酸钠(SDS)浓度、样品缓冲溶液等。以40.2 cm (有效长度: 30 cm)×50 μm未涂层熔融石英毛细管为分离柱,20 mmol/L硼砂-80 mmol/L SDS(无需调pH)为分离缓冲溶液,2 mmol/L硼砂-8 mmol/L SDS (含体积分数为10%甲醇)为样品缓冲溶液,检测波长为214 nm。3种杀菌剂的校正峰面积的相对标准偏差(RSD)在1.1%～ 3.8%范围内,迁移时间的RSD均小于0.9%, OPA、PCMX和三氯生的检出限(LOD,信噪比为3)分别为4.0、0.4、0.4 mg/L,定量限(LOQ,信噪比为10)分别为12、1.2、1.2 mg/L,校正峰面积与相应的质量浓度分别在12～2 000 mg/L、1.2～200 mg/L和1.2～200 mg/L范围内具有良好的线性关系,相关系数分别为0.9994、0.9993和0.9995。该法前处理简单,可快速、准确地同时测定3种组分,非常适合常规实验室分析。

关键词: 对氯间二甲基苯酚, 胶束电动毛细管色谱, 邻苯二甲醛, 日用化学品, 三氯生, 杀菌剂, 消毒剂

Abstract: A novel method for the separation and determination of o-phthalaldehyde (OPA), p-chloro-m-xylenol (PCMX) and triclosan in daily chemicals and compound chemical disinfectants in a single run by micellar electrokinetic chromatography (MEKC) was established. The factors such as the buffer concentration and pH, the concentration of sodium dodecyl sulfate (SDS), and the sample buffer, were investigated in detail. The analysis was carried out using a 50 μm uncoated capillary of 40.2 cm in total length (effective length: 30 cm). The running buffer was 20 mmol/L Na2B4O7 and 80 mmol/L SDS. The sample buffer was 2 mmol/L Na2B4O7-8 mmol/L SDS (without pH adjustment) containing 10% (v/v) methanol. The detection wavelength was 214 nm. The relative standard deviations (RSDs) of the corrected peak areas of the three components were in the range of 1.1%-3.8%, and the RSDs of migration times were less than 0.9%. The limits of detection (LODs, S/N=3) were 4.0, 0.4 and 0.4 mg/L, and the limits of quantification (LOQs, S/N=10) were 12, 1.2, and 1.2 mg/L for OPA, PCMX and triclosan, respectively. The corrected peak areas and the concentrations of the three components showed good linear relationship within the ranges of 12-2 000 mg/L, 1.2-200 mg/L and 1.2-200 mg/L with the correlation coefficients of 0.9994, 0.9993 and 0.9995 for OPA, PCMX and triclosan, respectively. The method was used for the determination of the three components in compound chemical disinfectants, hand washing liquids, soaps and a toothpaste. The results showed that the three components could be assayed in a single run with simple sample pretreatment, rapidity, accuracy and low cost, and the method is convenient for routine analysis.

Key words: bactericides, daily chemical, disinfectant, o-phthalaldehyde (OPA), p-chloro-m-xylenol (PCMX), triclosan, micellar electrokinetic chromatography (MEKC)