Uniformly sized molecularly imprinted polymer for atropine and its application to the determination of atropine and scopolamine in pharmaceutical preparations containing scopolia extract
Uniformly sized molecularly imprinted polymer for atropine and its application to the determination of atropine and scopolamine in pharmaceutical preparations containing scopolia extract
复制标题
DOI：
10.1016/j.jpba.2004.10.017
复制
发表时间：
2005-02-23
影响因子：
3.4
通讯作者：
Haginaka, J
中科院分区：
文献类型：
--
作者：
Nakamura, M;Ono, M;Haginaka, J
制备了一种均匀尺寸的阿托品分子印迹聚合物（MIP）。以2-（三氟甲基）丙烯酸和乙二醇二甲基丙烯酸酯为功能单体和交联剂，采用多步溶胀法和热聚合法制备了MIP。选择性因子，定义为分子印迹和非印迹聚合物的保留因子(k)之比，k（印迹）/k（非印迹），阿托品在MIP上的选择性因子为2.2。所获得的MIP可用于一种商业胃肠道药物中托烷类生物碱（阿托品和东莨菪碱）的色谱柱切换高效液相色谱测定，该色谱柱由所有MIP材料作为前柱组成。和一个传统的阳离子交换分析柱。在柱前提取的阿托品保留时间处观察到干扰峰。但在本研究的分析条件下（加载0.2杯阿托品），由于其峰面积小于标准溶液阿托品峰面积的0.5%，因此在测定阿托品时，这种干扰可以忽略不计。另一方面，东莨菪碱的保留时间没有出现干扰峰。阿托品和东莨菪碱的校准曲线分别在0.02 ~ 0.9杯子/ml （r = 0.9999）和0.003 ~ 0.09杯子/ml （r = 0.9998）范围内呈线性关系。安慰剂制剂样品中阿托品和东莨菪碱的平均回收率分别为98.9%和99.9%。两种成分的日内精密度（相对标准偏差，rsd(%)）均小于2.0%。将优化后的色谱柱切换系统成功地应用于某商品胃肠道药物中阿托品和东莨菪碱的含量测定。(C) 2004 Elsevier B.V.版权所有
A uniformly sized molecularly imprinted polymer (MIP) for atropine has been prepared. The MIP was prepared using 2-(trifluoromethyl) acrylic acid and ethylene glycol dimethacrylate as a functional monomer and cross-linker, respectively, by a multi-step swelling and thermal polymerization method. The selectivity factor, which is defined as the ratio of the retention factors (k) on the molecularly imprinted and non-imprinted polymers, k(imprinted)/k(non-imprinted), was 2.2 for atropine on the MIP. The obtained MIP was applied for the determination of tropane alkaloids (atropine and scopolamine) in a commercial gastrointestinal drug by a column-switching HPLC system, consisting of all MIP material as a pre-column. and a conventional cation-exchange analytical column. An interference peak was observed at the retention time of atropine derived from pre-column. However, since the peak area was less than 0.5% the peak area of atropine of a standard solution under the analytical conditions of this study (0.2 mug of atropine was loaded), this interference was negligible in the determination of atropine. On the other hand, no interference peak was observed at the retention time of scopolamine. Calibration curves of atropine and scopolamine showed food linearity in the range of 0.02-0.9 mug/ml (r = 0.9999) and 0.003-0.09 mug/ml (r = 0.9998), respectively. The mean recoveries of atropine and scopolamine from a placebo pharmaceutical preparation sample were 98.9 and 99.9%, respectively. The intra-day precision (measured by relative standard deviation, R.S.D. (%)) of both ingredients was less than 2.0%. The optimized column-switching system was applied successfully to the determination of atropine and scopolamine in a commercial gastrointestinal drug. (C) 2004 Elsevier B.V. All rights reserved.