Cao Jun, Peng Li-Qing, Xu Jing-Jing, Du Li-Jing, Zhang Qi-Dong
College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou 310036, China.
College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou 310036, China.
J Chromatogr A. 2016 Dec 16;1477:1-10. doi: 10.1016/j.chroma.2016.11.053. Epub 2016 Nov 25.
This study presents an effective method of using miniaturized matrix solid phase dispersion (MSPD) for the microextraction of inorganic iodine and iodinated amino acids from seaweed samples. Quantification of the target analytes was performed by ultrahigh performance liquid chromatography with UV detection. Molecular sieve (SBA-15) was chosen as the dispersing adsorbent with an ionic liquid (1-dodecyl-3-methylimidazolium bromide) as the elution solvent. The experimental conditions for the MSPD, such as the type of sorbent, ratio of sorbent to sample, type and concentration of the elution solvent, and grinding time were evaluated and optimized. Under the final working conditions, good recoveries were obtained in the range of 86.5-95.4%, with relative standard deviation values below 6.0% in all cases. The limits of detection and limits of quantitation were in the ranges of 3.7-16.7ng/mL and 12.4ng/mL, respectively. Compared with common ultrasound assisted extraction, the advantages of this green approach are low consumption of the sorbent and solvent, short extraction time and good selectivity, even in complicated matrices. The proposed SBA-15-based MSPD method was successfully applied to the microextraction of potassium iodide, 3-iodo-l-tyrosine, and 3,5-diiodo-l-tyrosine from kelp, nori and undaria pinnatifida, respectively.
本研究提出了一种利用小型化基质固相分散(MSPD)从海藻样品中微萃取无机碘和碘化氨基酸的有效方法。通过超高效液相色谱-紫外检测对目标分析物进行定量。选择分子筛(SBA-15)作为分散吸附剂,离子液体(1-十二烷基-3-甲基咪唑溴盐)作为洗脱溶剂。对MSPD的实验条件,如吸附剂类型、吸附剂与样品的比例、洗脱溶剂的类型和浓度以及研磨时间进行了评估和优化。在最终工作条件下,回收率良好,在86.5-95.4%范围内,所有情况下相对标准偏差值均低于6.0%。检测限和定量限分别在3.7-16.7ng/mL和12.4ng/mL范围内。与普通超声辅助萃取相比,这种绿色方法的优点是吸附剂和溶剂消耗低、萃取时间短且选择性好,即使在复杂基质中也是如此。所提出的基于SBA-15的MSPD方法成功应用于分别从海带、紫菜和裙带菜中微萃取碘化钾、3-碘-L-酪氨酸和3,5-二碘-L-酪氨酸。