Jan-E Sudarat, Santaladchaiyakit Yanawath, Burakham Rodjana
Materials Chemistry Research Center, Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science, Khon Kaen University, Khon Kaen 40002, Thailand.
Department of Chemistry, Faculty of Engineering, Rajamangala University of Technology Isan, Khon Kaen Campus, Khon Kaen 40000, Thailand.
J Chromatogr Sci. 2017 Jan;55(1):90-98. doi: 10.1093/chromsci/bmw140. Epub 2016 Sep 12.
An ultrasound-assisted surfactant-enhanced emulsification micro-extraction (UASEME) procedure has been developed for pre-concentration of benzoic acid (BA) and paraben preservatives, including methylparaben, ethylparaben, propylparaben and butylparaben, prior to high-performance liquid chromatography-ultraviolet (HPLC-UV) analysis. Separations were performed on a Lichrospher RP-18 endcapped 5 µm, using an isocratic mobile phase of 40% acetonitile, at a flow rate of 1 mL min The selected UASEME conditions comprised the use of 10 mL sample extract, 125 µL 1-octanol as extraction solvent and 0.05 mmol L Tween 20 as emulsifier, 0.5% sodium chloride, ultrasonication time of 6 min and centrifugation time of 10 min. Method performance demonstrated wide linear range between 0.5 and 7,000 µg L (R > 0.9903) and limits of detection between 0.03 and 10 µg L, which providing the enrichment factors of 15-184. The method precision (relative standard deviation) was <7%. The developed UASEME coupled with HPLC-UV has been successfully applied to determine four paraben preservatives in various sample matrices such as water, beverages and personal care products. The recoveries in the range of 70-138.1% were obtained. However, BA could not be determined in real sample extracts.
已开发出一种超声辅助表面活性剂增强乳化微萃取(UASEME)方法,用于在高效液相色谱-紫外(HPLC-UV)分析之前对苯甲酸(BA)和对羟基苯甲酸酯类防腐剂(包括对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯和对羟基苯甲酸丁酯)进行预富集。分离在粒径为5 µm的Lichrospher RP-18封端柱上进行,使用40%乙腈的等度流动相,流速为1 mL/min。选定的UASEME条件包括使用10 mL样品提取物、125 µL 1-辛醇作为萃取溶剂、0.05 mmol/L吐温20作为乳化剂、0.5%氯化钠、6 min的超声处理时间和10 min的离心时间。方法性能表明线性范围宽,为0.5至7000 µg/L(R>0.9903),检测限为0.03至10 µg/L,富集因子为15 - 184。方法精密度(相对标准偏差)<7%。所开发的UASEME与HPLC-UV联用已成功应用于测定水、饮料和个人护理产品等各种样品基质中的四种对羟基苯甲酸酯类防腐剂,回收率在70 - 138.1%范围内。然而,在实际样品提取物中无法测定BA。