色谱 ›› 2017, Vol. 35 ›› Issue (12): 1301-1305.DOI: 10.3724/SP.J.1123.2017.08026

• 研究论文 • 上一篇    下一篇

香水中邻苯二甲酸酯总量测定及其暴露评估

赵斯含, 王正萌, 邓红侠, 段家惠, 王进义, 刘书慧   

  1. 西北农林科技大学化学与药学院, 陕西 杨凌 712100
  • 收稿日期:2017-08-30 出版日期:2017-12-08 发布日期:2017-12-15
  • 通讯作者: 刘书慧,Tel:(029)87080325,E-mail:shliu815@126.com

Determination of total phthalates in perfume and their exposure assessment

ZHAO Sihan, WANG Zhengmeng, DENG Hongxia, DUAN Jiahui, WANG Jinyi, LIU Shuhui   

  1. College of Chemistry and Pharmacy, Northwest A & F University, Yangling 712100, China
  • Received:2017-08-30 Online:2017-12-08 Published:2017-12-15

摘要:

建立了快速测定香水中邻苯二甲酸酯(PAEs)的前处理方法。将香水中的PAEs水解为邻苯二甲酸(PA),再利用磷酸三丁酯萃取酸化液中的PA,使用高效液相色谱-二极管阵列检测器定量分析,并评估了PAEs的暴露量。实验考察并优化了影响PAEs水解率的因素,包括KOH的浓度和体积、乙醇的体积、水解时间和温度,优化后的水解条件:10 mL 4 mol/L KOH,1 mL乙醇,水解时间20 min,水解温度80℃。目标分析物的线性范围为3~240 μmol/L(R2=0.9991),LOD和LOQ分别为4.6 μmol/kg和5.9 μmol/kg,加标回收率为83.4%~92.7%,日内和日间精密度(RSD)不大于6.8%(n=5)。选择35种香水进行测定,PAEs总量范围在

关键词: 暴露水平, 高效液相色谱, 邻苯二甲酸, 水解, 香水

Abstract:

A novel method for rapid screening of phthalates (PAEs) in perfumes was developed. The PAEs were hydrolyzed to phthalic acid (PA), and the PA in the acidified solution was extracted with tributyl phosphate (TBP) which was detected by high performance liquid chromatography-diode array detection (HPLC-DAD). Meanwhile exposure dose to PAEs was estimated by the percentage of a topically applied dose that permeates the skin. The parameters such as the concentration and volume of KOH, the volume of ethanol, hydrolysis time and temperature were employed to evaluate the hydrolysis efficiency of PAEs. The optimized hydrolysis conditions were 10 mL of 4 mol/L KOH, and 1 mL of ethanol at 80℃ for 20 min. The linear range of phthalic acid was 3-240 μmol/L with a good correlation coefficient (R2=0.9991). The limits of detection (LOD) and quantification (LOQ) were 4.6 μmol/kg and 5.9 μmol/kg, respectively. The recoveries varied from 83.4% to 92.7% with relative standard deviations equal to or lower than 6.8%(n=5). A total of 35 perfume samples were determined, and the contents of total PAEs were found in the range of

Key words: exposure dose, high performance liquid chromatography (HPLC), hydrolysis, perfumes, phthalates (PAEs)

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