Wang Ting-Ting, Xuan Rong-Rong, Ma Jun-Feng, Tan Yao, Jin Zhen-Feng, Chen Yi-Hui, Zhang Li-Hua, Zhang Yu-Kui
School of Materials and Chemical Engineering/School of Safety Engineering, Ningbo University of Technology, Ningbo, Zhèjiāng, 315016, China.
Obstetrical Department, Affiliated Hospital of Ningbo University School of Medicine, Ningbo, Zhèjiāng, 315016, China.
Anal Bioanal Chem. 2016 Sep;408(24):6671-7. doi: 10.1007/s00216-016-9779-2. Epub 2016 Jul 18.
In this study, a simple solid-phase extraction (SPE) approach by using activated attapulgite as sorbent was successfully developed for the determination of melamine in milk formula samples. Crucial factors impacting the extraction efficiency, including sample solvent, elution solvent, and sample loading volume, were investigated. Under the optimal extraction conditions, the sample loading volume was up to 200 mL and the adsorption capacity of the melamine gave rise to 1154 μg g(-1). Excellent linear calibration curves (r (2) > 0.999) were achieved, and then the limit of detection (S/N = 3) and the limit of quantification (S/N = 10) were found to be 0.15 and 0.5 ng mL(-1), respectively. The recoveries of the melamine spiked in four milk formula samples at three concentration levels ranged from 83.5 to 111.0 % with relative standard deviations (RSDs) less than 10.2 %. Furthermore, RSDs of batch to batch (n = 4) of the acidified attapulgite used in this developed method were in the range of 2.3∼7.3 %. In comparison to the commercial Oasis MCX, the acidified attapulgite sorbent even outperformed (at least in terms of reproducibility) for melamine analysis in real food samples. Because of its simplicity, the newly developed SPE method based on acidified attapulgite nanoparticles should provide a promising tool for daily monitoring of doped melamine in milk formula or other complex matrices.
在本研究中,成功开发了一种以活性凹凸棒石为吸附剂的简单固相萃取(SPE)方法,用于测定奶粉样品中的三聚氰胺。研究了影响萃取效率的关键因素,包括样品溶剂、洗脱溶剂和样品进样量。在最佳萃取条件下,样品进样量可达200 mL,三聚氰胺的吸附容量达1154 μg g⁻¹。获得了出色的线性校准曲线(r²>0.999),然后检测限(S/N = 3)和定量限(S/N = 10)分别为0.15和0.5 ng mL⁻¹。在四个奶粉样品中添加三个浓度水平的三聚氰胺,回收率在83.5%至111.0%之间,相对标准偏差(RSD)小于10.2%。此外,本开发方法中使用的酸化凹凸棒石批次间(n = 4)的RSD在2.3%至7.3%范围内。与市售的Oasis MCX相比,酸化凹凸棒石吸附剂在实际食品样品中三聚氰胺分析方面甚至表现更优(至少在重现性方面)。由于其简单性,新开发的基于酸化凹凸棒石纳米颗粒的SPE方法应为日常监测奶粉或其他复杂基质中掺杂的三聚氰胺提供一个有前景的工具。