Hassanpour-Sabet Roghayeh, Seyfinejad Behruoz, Marzi Khosrowshahi Elnaz, Nemati Mahboob, Afshar Mogaddam Mohammad Reza, Jouyban Abolghasem
Food and Drug Safety Research Center, Tabriz University of Medical Sciences Tabriz Iran
Pharmaceutical Analysis Research Center and Faculty of Pharmacy, Tabriz University of Medical Sciences Tabriz Iran
RSC Adv. 2022 Oct 10;12(44):28728-28737. doi: 10.1039/d2ra02916b. eCollection 2022 Oct 4.
Dispersive solid-phase extraction (DSPE) was developed for the extraction of vanillylmandelic acid (VMA) in urine samples prior to capillary electrophoresis with diode array detection (CE-DAD). Extraction of VMA by DSPE was carried out by direct addition of 7.5 mg of synthesized amino-functionalized UiO-66 (Zr) metal-organic framework adsorbent into the 5 mL sample solution (pH 4.0), followed by sonication and centrifugation. The supernatant layer was discarded, then the sedimented adsorbent was eluted using borate buffer (75 mM, pH 10). Effective extraction parameters including the amount of adsorbent, sample pH, adsorption and desorption time, type, volume and pH of eluent, and type of adsorbent dispersion method were systematically investigated. Under the optimized conditions, linearity of the method was from 40 to 2000 μg L with a correlation coefficient over 0.9948. The method detection and quantification limits were 12 and 40 μg L, respectively. The relative standard deviations for intra-and inter-day precision were 2.4 and 2.8% ( = 5), respectively. The extraction recovery and enrichment factor values were 90% and 9.0 respectively.
分散固相萃取(DSPE)用于在采用二极管阵列检测的毛细管电泳(CE-DAD)之前对尿液样本中的香草扁桃酸(VMA)进行萃取。通过将7.5 mg合成的氨基功能化UiO-66(Zr)金属有机骨架吸附剂直接加入5 mL样品溶液(pH 4.0)中,随后进行超声处理和离心,来实现DSPE对VMA的萃取。弃去上层清液,然后使用硼酸盐缓冲液(75 mM,pH 10)洗脱沉淀的吸附剂。系统研究了有效的萃取参数,包括吸附剂用量、样品pH值、吸附和解吸时间、洗脱剂的类型、体积和pH值以及吸附剂分散方法的类型。在优化条件下,该方法的线性范围为40至2000 μg/L,相关系数超过0.9948。方法的检测限和定量限分别为12和40 μg/L。日内和日间精密度的相对标准偏差分别为2.4%和2.8%(n = 5)。萃取回收率和富集因子值分别为90%和9.0。