Analytical and Bioanalytical Chemistry ( IF 3.8 ) Pub Date : 2018-10-03 , DOI: 10.1007/s00216-018-1406-y Guizhen Li , Kyung Ho Row
A ternary deep eutectic solvent (TDES) was used as both template and functional monomer in the synthesis of TDES-based molecularly imprinted polymers (TDES-MIPs). A meticulous miniaturized solid-phase microextraction (mini-SPME) method followed by high-performance liquid chromatography (HPLC) were used for the optimal speciation of 3,4-dihydroxybenzoic acid (3,4-DHBA) in the needle of a syringe system with response surface methodology (RSM). Under the optimal conditions for the determination of 3,4-DHBA (amount of adsorbent (2 mg), sample volume (1 mL), cycles for adsorption and desorption (6)), the actual extraction amount was 8.46 μg g−1. The limits of detection (LODs, S/N = 3) for 3,4-DHBA in Ilex chinensis Sims were 0.26–0.31 μg mL−1, and the intra-day and inter-day precision (relative standard deviations, n = 4) after spiking with 5 μg mL−1, 100 μg mL−1, and 200 μg mL−1 were both less than 4.21%. The meticulous method (TDES-MIP-mini-SPME) combined with RSM offers a significant advance over existing methods, because of the meticulous operation and excellent selectivity of 3,4-DHBA from complex samples.
中文翻译:
选择性提取3,4-二羟基苯甲酸。
在基于TDES的分子印迹聚合物(TDES-MIP)的合成中,将三元深共熔溶剂(TDES)用作模板和功能单体。细微的微型固相微萃取(mini-SPME)方法,然后用高效液相色谱(HPLC)用于注射器系统针头中3,4-二羟基苯甲酸(3,4-DHBA)的最佳形态使用响应面方法(RSM)。在确定3,4-DHBA的最佳条件下(吸附剂量(2 mg),样品量(1 mL),吸附和解吸循环(6)),实际提取量为8.46μgg -1。冬青树Sims中3,4-DHBA的检出限(LODs,S / N = 3)为0.26-0.31μgmL -1和日内和日间精密度(相对标准偏差,Ñ 用5μg毫升尖峰之后= 4)-1,100微克毫升-1,和200μg毫升-1均小于4.21%。细致的方法(TDES-MIP-mini-SPME)与RSM相结合,比现有方法有了重大进步,这是因为细致的操作和对复杂样品中3,4-DHBA的优异选择性。