Ariani Marisa Dwi, Zuhrotun Ade, Manesiotis Panagiotis, Hasanah Aliya Nur
Pharmaceutical Analysis and Medicinal Chemistry Department, Faculty of Pharmacy, Universitas Padjadjaran Sumedang Bandung 45463 West Java Indonesia
Pharmacy Biology Department, Faculty of Pharmacy, Universitas Padjadjaran Sumedang Bandung 45463 West Java Indonesia.
RSC Adv. 2024 Apr 25;14(19):13521-13534. doi: 10.1039/d4ra01018c. eCollection 2024 Apr 22.
rhizome is traditionally used as a treatment for various diseases. Ethyl -methoxycinnamate (EPMC), which constitutes up to 31.77% of the total essential oil, is the main/marker compound. EPMC is responsible for various pharmacological activities of rhizome. According to the existing research, the isolation yield of EPMC is still meager, namely 0.50-2.50%; thus, a new EPMC isolation method is needed to produce better results. In this study, after determining the association constant and obtaining the Jobs plot between methacrylate derivative monomers and EPMC, a molecularly imprinted polymer for solid phase extraction (MI-SPE) was synthesized through bulk polymerization with EPMC as a template, methacrylic acid as a monomer, TRIM/EDGMA as a crosslinker in a ratio of 1 : 4 : 20 (MIP1) or 1 : 7 : 20 (MIP2). BPO was used as an initiator and -hexane was used as a porogen. The synthesis of the NIP was also conducted using the same ratio but without the template. The MIPs were then characterized using Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) measurements, and their analytical performance was evaluated through adsorption capacity and selectivity. The results indicate that MIP2 exhibits better analytical performance with an adsorption capacity value of 0.0813 mg g. The selectivity of MIP2 was tested using EPMC analog compounds, namely ethyl cinnamic (EC), cinnamaldehyde (CD), and kaempferol (KF), with imprinting factor (IF) values of 17.436, 1.539, and 0.06, respectively. Lastly, MIP2 was applied to the SPE cartridge for the isolation of EPMC from rhizome extract, and showed a percentage recovery of 82.40% for the ethanol extract, 68.05% for the ethyl acetate extract, and 65.27% for the -hexane extract. MI-SPE 2 gives high purity results for the ethanol, ethyl acetate, and -hexane extracts, with purities of 97.00%, 97.63%, and 99.59%, respectively. These results indicate that the MI-SPE technique shows great potential as a new method for isolating EPMCs with high yield and purity.
根茎传统上被用于治疗各种疾病。乙基 - 甲氧基肉桂酸酯(EPMC)占总精油的比例高达31.77%,是主要/标志性化合物。EPMC具有根茎的多种药理活性。根据现有研究,EPMC的分离产率仍然很低,即0.50 - 2.50%;因此,需要一种新的EPMC分离方法以获得更好的结果。在本研究中,在确定了甲基丙烯酸酯衍生物单体与EPMC之间的缔合常数并获得Job曲线后,以EPMC为模板、甲基丙烯酸为单体、TRIM/EDGMA为交联剂,按1∶4∶20(MIP1)或1∶7∶20(MIP2)的比例通过本体聚合法合成了用于固相萃取的分子印迹聚合物(MI-SPE)。使用过氧化苯甲酰(BPO)作为引发剂,正己烷作为致孔剂。非印迹聚合物(NIP)也采用相同比例合成,但不使用模板。然后使用傅里叶变换红外光谱(FTIR)、扫描电子显微镜(SEM)和布鲁诺尔-埃米特-泰勒(BET)测量对MIP进行表征,并通过吸附容量和选择性评估其分析性能。结果表明,MIP2表现出更好的分析性能,吸附容量值为0.0813 mg/g。使用EPMC类似化合物,即肉桂酸乙酯(EC)、肉桂醛(CD)和山奈酚(KF)测试了MIP2的选择性,印迹因子(IF)值分别为17.436、1.539和0.06。最后,将MIP2应用于SPE柱,用于从根茎提取物中分离EPMC,乙醇提取物的回收率为82.40% , 乙酸乙酯提取物的回收率为68.05%,正己烷提取物的回收率为65.27%。MI-SPE 2对乙醇、乙酸乙酯和正己烷提取物给出了高纯度结果,纯度分别为97.00%、97.63%和99.59%。这些结果表明,MI-SPE技术作为一种高产率和高纯度分离EPMC的新方法具有巨大潜力。