Ran Fanpeng, Liu Hongmei, Wang Xiaoqi, Guo Yong
School of Chemical and Biological Engineering, Lanzhou Jiaotong University, Lanzhou 730000, China; CAS Key Laboratory of Chemistry of Northwestern Plant Resources, Lanzhou Institute of Chemical physics, Chinese Academy of Sciences, Lanzhou 730000, China.
School of Chemical and Biological Engineering, Lanzhou Jiaotong University, Lanzhou 730000, China.
J Chromatogr A. 2017 Jul 21;1507:18-24. doi: 10.1016/j.chroma.2017.05.018. Epub 2017 May 8.
A novel material consisting of molybdenum disulfide (MoS) nanosheet that self-assemble into flower-like microspheres which aggregate to form a monolithic matrix with a micro or nano-scaled mesopore structure was successfully synthesized and used as an efficient sorbent for solid-phase extraction (SPE) due to its large specific adsorption area and good stability. The extraction properties of the as-prepared sorbent were evaluated by high-performance liquid chromatography with variable wavelength detection (HPLC-VWD) by analyzing four flavonoids (apigenin, quercetin, luteolin, and kaempferol). Under optimal conditions, the LODs and LOQs were found to be in the ranges of 0.1-0.25 and 0.4-0.5μgL, respectively, and wide linear ranges were obtained with correlation coefficients (R) ranging from 0.9991 to 0.9996. Compared with commercial C18 and Alumina-N sorbents, the as-prepared sorbent showed high extraction efficiency at different concentrations of flavonoids. After 100 uses, the extraction ability of the self-assembled MoS nanosheet monolithic sorbent had no evident decline, denoting a long service life. Finally, the SPE-HPLC-VWD method using the as-prepared sorbent was applied to flavonoid analysis in beverage samples with satisfactory results.
成功合成了一种由二硫化钼（MoS）纳米片组成的新型材料，该纳米片自组装成花状微球，这些微球聚集形成具有微米或纳米级介孔结构的整体基质，由于其较大的比吸附面积和良好的稳定性，该材料被用作固相萃取（SPE）的高效吸附剂。通过高效液相色谱可变波长检测（HPLC-VWD）分析四种黄酮类化合物（芹菜素、槲皮素、木犀草素和山奈酚），对所制备吸附剂的萃取性能进行了评估。在最佳条件下，检测限（LOD）和定量限（LOQ）分别在0.1-0.25和0.4-0.5μg/L范围内，获得了较宽的线性范围，相关系数（R）在0.9991至0.9996之间。与市售C18和氧化铝-N吸附剂相比，所制备的吸附剂在不同浓度的黄酮类化合物下均表现出较高的萃取效率。经过100次使用后，自组装MoS纳米片整体吸附剂的萃取能力没有明显下降，表明其使用寿命长。最后，将使用所制备吸附剂的SPE-HPLC-VWD方法应用于饮料样品中的黄酮类化合物分析，结果令人满意。
