Trace Element, Spectroscopy and Speciation Group (GETEE), Strategic Grouping in Materials (AEMAT), Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, niversidade de Santiago de Compostela, Avenida das Ciencias, s/n, 15782, Santiago de Compostela, Spain.
Trace Element, Spectroscopy and Speciation Group (GETEE), Strategic Grouping in Materials (AEMAT), Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, niversidade de Santiago de Compostela, Avenida das Ciencias, s/n, 15782, Santiago de Compostela, Spain.
Talanta. 2020 Dec 1;220:121418. doi: 10.1016/j.talanta.2020.121418. Epub 2020 Jul 19.
This study combines ultrasound-assisted extraction and vortex-assisted dispersive micro-solid phase extraction using an ionic imprinted polymer as a selective sorbent for rapid isolation and pre-concentration of inorganic arsenic species (As(III) and As(V)) in extracts from rice samples prior to their determination by high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry. All factors affecting the ultrasound assisted extraction of the species from rice (ultrasound amplitude, sonication time and sonication mode) and their selective pre-concentration by ionic imprinted polymer-based vortex-assisted dispersive micro-solid phase extraction (sorbent amount, extract pH, vortex extraction time and speed, eluting solution and vortex elution time and speed) were optimized. The analytical performance of the procedure was studied at optimum conditions: ultrasound continuous sonication at 40% amplitude for 2.0 min using 1:1 methanol/ultrapure as an extractant, 50 mg of sorbent, extract pH at 8.0, vortex loading at 1000 rpm for 1.0 min, and elution with ultrapure water by vortexing at 1000 rpm for 1.0 min, pre-concentration procedure which leads to a pre-concentration factor of 10. The limits of detection obtained for As (III) and As (V) were 0.20 and 0.41 μg kg, respectively, and were well below the maximum levels established by the European Union in rice and rice containing products. The method was found to be precise (intraday and interday relative standard deviations ≤ 11%) and selective. The accuracy was confirmed by analysing the ERM-BC211 (rice, As species) certified reference material, and the method was successfully applied to commercial rice samples.
本研究结合超声辅助提取和涡旋辅助分散固相微萃取,使用离子印迹聚合物作为选择性吸附剂,用于快速分离和浓缩大米样品提取物中的无机砷形态(As(III) 和 As(V)),然后采用高效液相色谱-电感耦合等离子体质谱法进行测定。优化了影响从大米中超声辅助提取物种的所有因素(超声幅度、超声时间和超声模式)和通过基于离子印迹聚合物的涡旋辅助分散固相微萃取选择性预浓缩的所有因素(吸附剂用量、提取 pH 值、涡旋提取时间和速度、洗脱溶液和涡旋洗脱时间和速度)。在最佳条件下研究了该程序的分析性能:使用 1:1 甲醇/超纯水作为提取剂,以 40%的幅度连续超声 2.0 分钟,使用 50mg 吸附剂,提取 pH 值为 8.0,以 1000rpm 的速度涡旋加载 1.0 分钟,并用 1000rpm 的速度涡旋洗脱超纯水 1.0 分钟,预浓缩程序导致预浓缩因子为 10。对于 As(III) 和 As(V),检测限分别为 0.20 和 0.41μgkg,均远低于欧盟在大米和含大米产品中规定的最大水平。该方法具有良好的精密度(日内和日间相对标准偏差≤11%)和选择性。通过分析 ERM-BC211(大米,砷形态)认证参考材料验证了准确性,并且该方法成功应用于商业大米样品。