分子印迹-基质固相分散-高效液相色谱法测定血液中苯磺酸氨氯地平
Determination of Amlodipine Besylate in Blood by HPLC Combined with Molecular Imprinting Matrix Solid Phase Dispersion
摘 要
采用分子印迹-基质固相分散-高效液相色谱法(MI-MSPD-HPLC)测定血液中痕量苯磺酸氨氯地平。制备苯磺酸氨氯地平分子印迹聚合物,以此为基质固相分散剂与样品混合均匀,风干后装柱,用甲醇洗脱苯磺酸氨氯地平。洗脱液在Inertsil DOS-SP分离柱上分离,以甲醇-乙腈-水(70+22+8)混合液为流动相进行洗脱,检测波长为237 nm。氨氯地平的线性范围为1.7~20.0 μg·L-1,检出限(3S/N)为0.5 μg·L-1,测定下限(10S/N)为1.7 μg·L-1。对空白血液样品进行加标回收试验,回收率在91.0%~109%之间,测定值的相对标准偏差(n=5)在3.7%~4.8%之间。方法可用于测定血液中的苯磺酸氨氯地平。
印迹聚合物
基质固相分散
苯磺酸氨氯地平
血液
HPLC
Molecularly imprinted polymers
Matrix solid-phase dispersion
Amlodipine besylate
Blood
Abstract
A method of HPLC combined with molecular imprinting matrix solid phase dispersion was applied to determine amlodipine besylate in blood.Molecularly imprinted polymer for amlodipine besylate was synthesized and mixed with the sample, used as matrix solid phase dispersing agent. After air-drying, the mixture was used as filter for packing column, and amlodipine besylate was eluted from the column by methanol.The eluent was separated on an Inertsil DOS-SP column using a mixture of methanol-acetonitrile-water (70+22+8) as mobile phase. UV absorbance was measured at 237 nm. The linearity range of amlodipine besylate was 1.7-20.0 μg·L-1, with detection limit (3S/N) of 0.5 μg·L-1 and lower limit of determination (10S/N) of 1.7 μg·L-1. The recovery rates measured by standard addition method were in the range of 91.0%-109%, with RSD (n=5) of 3.7%-4.8% . The method was used for measurement of amlodipine besylate in blood.
中图分类号 O657.7
所属栏目 工作简报
基金项目 河南省科学技术厅基金项目(132300410167;122102310497);焦作市科技局科技计划项目(201217)
收稿日期 2014/3/15
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备注许文静(1966-),女,河南焦作人,副教授,硕士,主要从事聚合物合成及应用研究。
引用该论文: XU Wen-jing,ZHANG She-li,ZHANG Wen-sheng. Determination of Amlodipine Besylate in Blood by HPLC Combined with Molecular Imprinting Matrix Solid Phase Dispersion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(4): 446～449
许文静,张社利,张文生. 分子印迹-基质固相分散-高效液相色谱法测定血液中苯磺酸氨氯地平[J]. 理化检验－化学分册, 2015, 51(4): 446～449
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【3】赖可,晁若冰,李楠,等.HPLC测定复方氨氯地平胶囊的含量［J］.华西药学杂志, 2010,25(6):748-749.
【4】NAFISUR R, MANISHA S, MD N H. Application of oxidants to the spectrophoto-metric determination of amlodipine besylate in pharmaceutical formulations［J］. IL Farmaco, 2004,59(11):913-919.
【5】胡在林.反相高效液相色谱法测定氨氯地平胶囊的含量和有关物质［J］.中国药业, 2011,20(12):28-29.
【6】李志伟,赵云超,齐建敏.高效毛细管电泳法测定缬沙坦氨氯地平［J］.河北大学学报:自然科学版, 2012,32(2):149-153.
【7】张琰,杨蕾,刘梅,等.苯磺酸氨氯地平片在健康人体的药动学及生物等效性评价［J］.第四军医大学学报, 2006,27(2):172-175.
【8】杨秋玲,李丹,权新军,等.基质固相分散-毛细管电泳法测定柚果皮中柚皮苷的质量浓度［J］.吉林大学学报:理学版, 2011,49(5):954-956.
【9】郑屏,盛旋,余晓峰,等.基质固相分散液相色谱法检测辣椒产品中的黄曲霉毒素［J］.色谱, 2006,24(1):62-64.
【10】HAN M, KANE R, GOTO M, et al. Discriminate surface molecular recognition sites on a microporous substrate: a new approach［J］. Macromolecules, 2003,36(12):4472-4477.
【11】MA Yue, ZHANG Ying, ZHAO Man, et al. Efficient synthesis of narrowly dispersed molecularly imprinted polymer microspheres with multiple stimuli-responsive template binding properties in aqueous media［J］. Chem Commun, 2012,48:6217-6219.
【12】SERGEYEVA T A, GORBACH L A, PILETSKA E V, et al. Colorimetric test-systems for creatinine detection based on composite molecularly imprinted polymer membranes［J］. Analytica Chimica Acta, 2013,770:161-168.
【13】黄红萍,游勇基.分子印迹固相萃取-液相色谱法测定喘息灵胶囊中盐酸克仑特罗的含量［J］.药物分析杂志, 2012,32(2):233-236.
【14】黄华斌,庄峙厦,赵丽,等.分子印迹固相萃取技术-高效液相色谱法测定奶制和饲料中三聚氰胺含量［J］.理化检验-化学分册, 2014,50(10):1286-1290.
【15】冯银巧,周如金,唐玉斌,等.分子印迹技术在固相萃取中的应用［J］.理化检验-化学分册, 2011,47(1):125-128.
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