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日用化学工业（中英文）

日用化学工业 ›› 2022, Vol. 52 ›› Issue (4): 438-443.doi: 10.3969/j.issn.1001-1803.2022.04.014

• 分析与检测 • 上一篇    下一篇

盐析分相萃取-高效液相色谱法测定香皂中2,4,6-三氯苯酚、五氯苯酚和硫氯酚

张烈远1,2,刘捷光2,韩颖2,万建春2,占春瑞2,*(),王文君1,*()   

  1. 1. 江西农业大学 食品科学与工程学院,江西 南昌 330045
    2. 南昌海关技术中心,江西 南昌 330038
  • 收稿日期:2021-05-19 修回日期:2021-03-21 出版日期:2022-04-22 发布日期:2022-04-25
  • 通讯作者: 占春瑞,王文君

Determination of 2, 4, 6-trichlorophenol, pentachlorophenol and bithionol in soap by salting out phase separation extraction -high performance liquid chromatography

Zhang Lieyuan1,2,Liu Jieguang2,Han Ying2,Wan Jianchun2,Zhan Chunrui2,*(),Wang Wenjun1,*()   

  1. 1. College of Food Science and Engineering, Jiangxi Agricultural University, Nanchang, Jiangxi 330045, China
    2. Technical Center of Nanchang Customs, Nanchang, Jiangxi 330038, China
  • Received:2021-05-19 Revised:2021-03-21 Online:2022-04-22 Published:2022-04-25
  • Contact: Chunrui Zhan,Wenjun Wang

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摘要：

建立了香皂中禁用防腐剂2,4,6-三氯苯酚、五氯苯酚和硫氯酚含量检测的高效液相色谱分析方法。样品经过热水溶解,加入乙腈混合提取,盐析得到提取液。采用Agilent ZORBAX Eclipse XDB-C18色谱柱（5 μm,4.6 mm×250 mm）分离,以甲醇-乙腈-乙酸铵三元流动相进行梯度洗脱,柱温30 ℃,流速1.0 mL/min,检测波长为300 nm,外标法定量。实验结果表明,三种物质的线性相关系数均大于0.999,2,4,6-三氯苯酚、五氯苯酚检出限（LOD）和定量限（LOQ）分别为1.5和5.0 mg/kg,硫氯酚检出限（LOD）和定量限（LOQ）分别为0.8和2.5 mg/kg。三个质量浓度水平添加平均回收率81.8%~103.0%,相对标准偏差（RSD）为3.88%~8.57%（n=6）。该方法快速、准确,经济,适用于出口化妆品香皂中2,4,6-三氯苯酚、五氯苯酚和硫氯酚快速筛查和定量分析。

关键词: 禁用防腐剂, 2,4,6-三氯苯酚, 五氯苯酚, 硫氯酚, 盐析分相萃取, 高效液相色谱法, 出口化妆品, 香皂

Abstract:

An efficient high performance liquid chromatography analysis method for detecting the content of prohibited preservatives 2, 4, 6-trichlorophenol, pentachlorophenol and bithionol in exported cosmetic soaps was established. There is no literature about the determination of 2, 4, 6-trichlorophenol, pentachlorophenol and bithionol method in soaps. The sample was made into uniform crumbs, dissolved in hot water, mixed with acetonitrile for extraction, and was salted out to obtain the extracting solution. Gradient elution was carried out with methanol-acetonitrile-ammonium acetate as ternary mobile phase. It was at a flow rate of 1.0 mL/min through an Agilent ZORBAX Eclipse XDB-C18 chromatographic column （5 μm, 4.6 mm×250 mm）, and the column temperature was 30 ℃. The UV detection wavelength was 300 nm. The external standard method was used for quantification. The experimental results show that the linear correlation coefficients of the three substances are more than 0.999. The limit of detection （LOD） and the limit of quantification （LOQ） of 2, 4, 6-trichlorophenol and pentachlorophenol are 1.5 and 5.0 mg/kg, respectively, and the limit of detection （LOD） and limit of quantification （LOQ）of bithionol is 0.8 and 2.5 mg/kg, respectively. Average recoveries of standard addition at three levels are in the range of 81.8% to 103.0%, with the relative standard deviation （RSD） in the range of 3.88% to 8.57% （n=6）. The method is quick, accurate and economical. It is suitable for the quick screening and quantitative analysis of 2, 4, 6-trichlorophenol, pentachlorophenol and bithionol in exported cosmetic soaps. It fills the blank of determination method of the three substance in exported cosmetic soaps, and provides testing technology support for customs supervision of exported cosmetic soaps.

Key words: prohibited preservatives, 2, 4, 6-trichlorophenol, pentachlorophenol, bithionol, salting out phase separation extraction, high performance liquid chromatography, exported cosmetics, soap

中图分类号: 

  • TQ648