Chen Yonggang, Meng Junhua, Zou Jili, An Jing
Department of Pharmacy, The Third Hospital of Wuhan, Wuhan, Hubei, 430060, People's Republic of China.
Biomed Chromatogr. 2015 Jun;29(6):869-75. doi: 10.1002/bmc.3367. Epub 2014 Oct 30.
Hordenine is an active compound found in several foods, herbs and beer. In this work, a novel sorbent was fabricated for selective solid-phase extraction (SPE) of hordenine in biological samples. The organic polymer sorbent was synthesized in one step in the plastic barrel of a syringe by a pre-polymerization solution consisting of methacrylic acid (MAA), 4-vinylphenylboronic acid (VB) and ethylene glycol dimethacrylate (EGDMA). The conditions for preparation were optimized to generate a poly(MAA-VB-EGMDA) monolith with good permeability. The monolith exhibited good enrichment efficiency towards hordenine. By using tyramine as the internal standard, a poly(MAA-VB-EGMDA)-based SPE-HPLC method was established for analysis of hordenine. Conditions for SPE, including volume of eluting solvent, pH of sample solution, sampling rate and sample volume, were optimized. The proposed SPE-HPLC method presented good linearity (R(2) = 0.9992) within 10-2000 ng/mL and the detection limits was 3 ng/mL, which is significantly more sensitive than reported methods. The method was also applied in plasma and urine samples; good capability of removing matrices was observed, while hordenine in low content was well extracted and enriched. The recoveries were from 90.6 to 94.7% and from 89.3 to 91.5% for the spiked plasma and urine samples, respectively, with the relative standard deviations <4.7%.
去甲乌药碱是一种存在于多种食物、草药和啤酒中的活性化合物。在本研究中，制备了一种新型吸附剂，用于生物样品中去甲乌药碱的选择性固相萃取（SPE）。该有机聚合物吸附剂由甲基丙烯酸（MAA）、4-乙烯基苯硼酸（VB）和乙二醇二甲基丙烯酸酯（EGDMA）组成的预聚合溶液在注射器的塑料筒中一步合成。优化了制备条件，以生成具有良好渗透性的聚（MAA-VB-EGDMA）整体柱。该整体柱对去甲乌药碱表现出良好的富集效率。以酪胺为内标，建立了基于聚（MAA-VB-EGDMA）的固相萃取-高效液相色谱法（SPE-HPLC）用于去甲乌药碱的分析。对固相萃取条件进行了优化，包括洗脱溶剂体积、样品溶液pH值、进样速率和样品体积。所提出的固相萃取-高效液相色谱法在10 - 2000 ng/mL范围内呈现良好的线性（R² = 0.9992），检测限为3 ng/mL，比已报道的方法灵敏度显著更高。该方法还应用于血浆和尿液样品；观察到其具有良好的去除基质能力，同时低含量的去甲乌药碱能被良好地萃取和富集。加标血浆和尿液样品的回收率分别为90.6%至94.7%和89.3%至91.5%，相对标准偏差<4.7%。
