色谱 ›› 2018, Vol. 36 ›› Issue (3): 190-194.DOI: 10.3724/SP.J.1123.2017.11006

• 研究快报 • 上一篇    下一篇

基于石墨烯海绵的固相萃取-液相色谱法测定化妆品中6种紫外吸收剂

王雪梅1,2, 王娟1, 杜彤彤1, 马晓敏1, 卢小泉1,2   

  1. 1. 西北师范大学化学化工学院, 甘肃 兰州 730070;
    2. 甘肃省生物电化学与环境分析重点实验室, 甘肃 兰州 730070
  • 收稿日期:2017-11-06 出版日期:2018-03-08 发布日期:2018-04-04
  • 通讯作者: 王雪梅,Tel:(0931)7973035,E-mail:wxm98@163.com
  • 基金资助:

    国家自然科学基金项目(21467028);甘肃省科技支撑计划项目(1304GKCA042).

Determination of six ultraviolet filters in cosmetics by high performance liquid chromatography coupled with solid-phase extraction based on graphene sponge

WANG Xuemei1,2, WANG Juan1, DU Tongtong1, MA Xiaomin1, LU Xiaoquan1,2   

  1. 1. College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070, China;
    2. Key Laboratory of Bioelectrochemistry & Environmental Analysis of Gansu Province, Lanzhou 730070, China
  • Received:2017-11-06 Online:2018-03-08 Published:2018-04-04
  • Supported by:

    National Natural Science Foundation of China (No. 21467028); Science and Technology Support Plan of Gansu Province (No. 1304GKCA042).

摘要:

以石墨烯海绵(GS)为固相萃取材料,建立了固相萃取-高效液相色谱(SPE-HPLC)同时测定化妆品中6种紫外吸收剂的分析方法。样品经甲醇超声提取,用自制的石墨烯海绵固相萃取小柱净化富集,丙酮洗脱。采用Agilent Zorbax SB-C18色谱柱(150 mm×4.6 mm,5 μm)进行分离,甲醇-水(95∶5,v/v)为流动相,紫外检测波长为340 nm。结果表明,6种紫外吸收剂均在各自的范围内线性关系良好,2-(2'-羟基-5'-甲基苯基)苯并三氮唑的相关系数(r) > 0.997,其他5种r > 0.999。方法的检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.08~1.82 μg/L和0.26~6.07 μg/L。在20、50和100 μg/L 3个加标水平下,6种目标物的加标回收率为61.1%~119.0%,相对标准偏差(RSD)小于1%(n=6)。该法简便、快速,灵敏度高,重复性好,适用于不同类型化妆品中紫外吸收剂的检测。

关键词: 高效液相色谱, 固相萃取, 化妆品, 石墨烯海绵, 紫外吸收剂

Abstract:

A method for the simultaneous determination of six UV filters in cosmetics by high performance liquid chromatography (HPLC) coupled with solid-phase extraction (SPE) based on graphene sponge (GS) was established. The samples were extracted with methanol by ultrasonic, then cleaned up by home-made SPE cartridges and eluted with acetone. The six UV filters were separated on an Agilent Zorbax SB-C18 column (150 mm×4.6 mm, 5 μm). Methanol-water (95:5, v/v) was used as mobile phase and the detection wavelength was 340 nm. The results showed that the limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) of the six UV filters were 0.08-1.82 μg/L and 0.26-6.07 μg/L, respectively. The correlation coefficients (r) were greater than 0.999 except 2-(2'-hydroxy-5'-methyl-phenyl) benzotriazole (r>0.997). The recoveries of the six UV filters were 61.1%-119.0%, and the relative standard deviations (RSDs) were less than 1% (n=6) at the three spiked levels of 20, 50 and 100 μg/L. The method is simple, rapid, sensitive and repeatable, and is suitable for the determination of the UV filters in cosmetics.

Key words: cosmetics, graphene sponge (GS), high performance liquid chromatography (HPLC), solid-phase extraction (SPE), ultraviolet filters

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