College of Science, Northwest A&F University, Yangling, China.
J Chromatogr A. 2013 Jun 21;1295:16-23. doi: 10.1016/j.chroma.2013.04.054. Epub 2013 Apr 26.
In this study, two novel sample extraction methods for the analysis of bisphenol A (BPA) in edible oils were developed by using liquid-liquid extraction followed by a dispersive liquid-liquid microextraction (LLE-DLLME) and reversed-phase dispersive liquid-liquid microextraction (RP-DLLME). RP-DLLME showed a superior characteristic over LLE-DLLME and other previously reported procedures because of its easy operation, short extraction time, high sensitivity, low organic solvent consumption and waste generation. The optimized extraction conditions of RP-DLLME for 1.0 g of edible oil diluted in 4 mL of n-hexane were: extractant, 100 μL 0.2 M sodium hydroxide solution (80% methanol, v/v); extraction time, 1 min; centrifugation, 3 min. The determination of BPA was carried out by high performance liquid chromatography coupled with a DAD detector. The method offered excellent linearity over a range of 0.010-0.5 μg g(-1) with a correlation coefficient of r>0.997. Intra-day and inter-day repeatability values expressed as relative standard deviation were 1.9% and 5.9%, respectively. The quantitation limit and detection limit were 6.3 and 2.5 ng g(-1). The target analyte was detected in 5 out of 16 edible oil samples. The recovery rates in real samples ranged from 89.5 to 99.7%.
在这项研究中,开发了两种新的用于食用油脂中双酚 A(BPA)分析的样品提取方法,即液-液萃取后分散液-液微萃取(LLE-DLLME)和反相分散液-液微萃取(RP-DLLME)。与 LLE-DLLME 和其他先前报道的方法相比,RP-DLLME 具有操作简单、萃取时间短、灵敏度高、有机溶剂消耗和废物生成低的优点。在 1.0 g 食用油脂稀释于 4 mL 正己烷的条件下,RP-DLLME 的优化萃取条件为:萃取剂,100 μL 0.2 M 氢氧化钠溶液(80%甲醇,v/v);萃取时间,1 min;离心,3 min。采用高效液相色谱-二极管阵列检测器测定 BPA。该方法在 0.010-0.5 μg g(-1) 范围内具有良好的线性关系,相关系数 r>0.997。日内和日间重复性的相对标准偏差分别为 1.9%和 5.9%。定量限和检测限分别为 6.3 和 2.5 ng g(-1)。在 16 种食用油脂样品中,有 5 种样品检测到目标分析物。实际样品的回收率在 89.5%至 99.7%之间。