Han Fang, He You-Zhao, Yu Chang-Zhu
Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026, China.
Talanta. 2008 Feb 15;74(5):1371-7. doi: 10.1016/j.talanta.2007.09.007. Epub 2007 Sep 19.
A convenient and automated method for on-line pretreatment and determination of three parabens (i.e. methyl, ethyl and propyl p-hydroxybenzoate) in cosmetic products is proposed by using flow injection analysis (FIA), solid-phase extraction (SPE) and micellar electrokinetic chromatography (MEKC). An improved split-flow interface is used to couple SPE on C(8)-bonded silica with MEKC separation, which can avoid running buffer contamination and reduce buffer consumption, especially, containing expensive reagents. The analytes are loaded onto a C(8) column at 0.6 mL/min for 60s and eluted with a mixed eluent of 40% (v/v) 10 mmol/L sodium tetraborate buffer (pH 9.3) and 60% (v/v) ethanol at 0.75 mL/min. The MEKC separation is accomplished with a running buffer of 20 mmol/L sodium tetraborate (pH 9.3) containing 100 mmol/L sodium dodecyl sulfate (SDS) at 15 kV. For butyl p-hydroxybenzoate did not be detected in the cosmetic products, it was used as an internal standard (IS) added into the real samples. This FIA-SPE-MEKC method using IS allows the sample separation within 12 min and the sample throughput of five samples per hour with the relative standard deviation (R.S.D.) less than 2.3% (n=5). The limits of detection (LOD) are in the range from 0.07 to 0.1 microg/mL (S/N=3 and n=11). The proposed method has been used to determine three parabens in real cosmetic products satisfactorily.
提出了一种利用流动注射分析(FIA)、固相萃取(SPE)和胶束电动色谱(MEKC)对化妆品中三种对羟基苯甲酸酯(即对羟基苯甲酸甲酯、乙酯和丙酯)进行在线预处理和测定的便捷自动化方法。采用改进的分流接口将C(8)键合硅胶上的固相萃取与胶束电动色谱分离相结合,可避免运行缓冲液污染并减少缓冲液消耗,特别是对于含有昂贵试剂的情况。分析物以0.6 mL/min的流速加载到C(8)柱上60秒,然后用40%(v/v)10 mmol/L硼酸钠缓冲液(pH 9.3)和60%(v/v)乙醇的混合洗脱液以0.75 mL/min的流速洗脱。胶束电动色谱分离在含100 mmol/L十二烷基硫酸钠(SDS)的20 mmol/L硼酸钠(pH 9.3)运行缓冲液中于15 kV下完成。由于在化妆品中未检测到对羟基苯甲酸丁酯,将其用作内标(IS)添加到实际样品中。这种使用内标的FIA-SPE-MEKC方法可在12分钟内完成样品分离,每小时可处理五个样品,相对标准偏差(R.S.D.)小于2.3%(n = 5)。检测限(LOD)在0.07至0.1 μg/mL范围内(S/N = 3且n = 11)。所提出的方法已成功用于测定实际化妆品中的三种对羟基苯甲酸酯。