Hasanah Aliya Nur, Maelaningsih Firdha Senja, Apriliandi Fadli, Sabarudin Akhmad
Pharmaceutical Analysis and Medicinal Chemistry Department, Faculty of Pharmacy, Universitas Padjadjaran, Jalan Raya Bandung Sumedang KM 21, 5, Sumedang, Indonesia.
Chemistry Department, Universitas Brawijaya, Malang, Indonesia.
J Anal Methods Chem. 2020 Feb 28;2020:3027618. doi: 10.1155/2020/3027618. eCollection 2020.
A monolithic imprinted atenolol column was constructed by in situ polymerisation using a methacrylic acid monomer and a 1 : 1 (v/v) porogen of propanol: toluene with two template: monomer: crosslinker combinations, namely, MIP 1 (1 : 4 : 20) and MIP 2 (1 : 5 : 20). Physical characterisation of the monolithic columns consisted of permeability testing, Fourier transform infrared (FTIR) testing, surface area analysis (SAA), and scanning electron microscopy (SEM). The permeability value of four monolithic columns was in the good category: MIP 1 (24.01 mD), NIP 1 (56.43 mD), MIP 2 (23.03 mD), and NIP 2 (14.47 mD). The polymerisation process of these four monolithic imprinted columns was carried out perfectly, as shown by the absence of vinyl groups (1000 cm and 900 cm) during FTIR testing. Based on SAA testing, the pores of the four polymers were classified as mesopores. The best monolithic column was MIP 1, as seen from the intercolumn and intracolumn reproducibility values and a % RSD <2.0%. The MIP 1 column was selective towards atenolol, as seen from the selectivity factor, imprinting factor (IF), and resolution (Rs) values. The IF values of MIP 1 were atenolol (204.62), metoprolol (3.36), and propranolol (1.27). The Rs value between atenolol and the analogue compounds was 7.23. The MIP 1 column can be used for the analysis of atenolol in blood serum samples with an average percentage recovery rate of 94.88 ± 4.43%.
采用甲基丙烯酸单体以及丙醇与甲苯体积比为1:1的致孔剂，通过原位聚合制备了整体式印迹阿替洛尔柱，使用了两种模板:单体:交联剂组合，即MIP 1(1:4:20)和MIP 2(1:5:20)。整体柱的物理表征包括渗透性测试、傅里叶变换红外(FTIR)测试、比表面积分析(SAA)和扫描电子显微镜(SEM)。四根整体柱的渗透值处于良好类别:MIP 1(24.01 mD)、NIP 1(56.43 mD)、MIP 2(23.03 mD)和NIP 2(14.47 mD)。这四根整体式印迹柱的聚合过程进行得很完美，FTIR测试中未出现乙烯基(1000 cm和900 cm)证明了这一点。基于SAA测试，这四种聚合物的孔被归类为中孔。从柱间和柱内重现性值以及%RSD<2.0%可以看出，最佳的整体柱是MIP 1。从选择性因子、印迹因子(IF)和分离度(Rs)值可以看出，MIP 1柱对阿替洛尔具有选择性。MIP 1的IF值分别为阿替洛尔(204.62)、美托洛尔(3.36)和普萘洛尔(1.27)。阿替洛尔与类似化合物之间的Rs值为7.23。MIP 1柱可用于分析血清样本中的阿替洛尔，平均回收率为94.88±4.43%。
