CAJ | 학술논문

以邻苯二甲酸二辛酯（ DOP）为虚拟模板分子，α-甲基丙烯酸（ MAA）为功能单体，乙二醇二甲基丙烯酸酯（ EDMA）为交联剂，采用沉淀聚合法制备了对邻苯二甲酸二（2-丙基庚）酯（ DPHP）具有高选择性的分子印迹聚合物（ MIP）。用紫外分光光度法探索了不同功能单体与模板分子的结合能力，与功能单体丙烯酸（ AA）相比，MAA 与DOP的结合能力更强，其最佳结合的物质的量比为6：1。考察 MIP 对 DOP、DPHP、邻苯二甲酸二甲酯（ DMP）、邻苯二甲酸二丁酯（ DBP）的选择吸附性能，发现该聚合物对 DPHP具有更高的选择吸附性。以制备的聚合物为固相萃取填料，结合 HPLC分析，考察了淋洗剂与洗脱剂的种类和用量对 DPHP 回收率的影响。将 DPHP 甲醇溶液加载至萃取柱后用1 mL甲醇-水（1：9，v/v）淋洗，5 mL甲醇-乙酸（9：1，v/v）洗脱，DPHP在分子印迹固相萃取（ MI-SPE）柱上的回收率达到96.8％，而在非印迹固相萃取（ NISPE）柱上的回收率仅为52.9％。将建立的 MISPE-HPLC方法应用于测定兔口服 DPHP后不同时间点兔血清中 DPHP的浓度，发现其血药浓度的最大值为5.88μg/mL，达峰值时间为4 h，DPHP加标回收率为90.0％~92.0％，相对标准偏差小于5％。
이린분이갑산이신지（ DOP）위허의모판분자，α-갑기병희산（ MAA）위공능단체，을이순이갑기병희산지（ EDMA）위교련제，채용침정취합법제비료대린분이갑산이（2-병기경）지（ DPHP）구유고선택성적분자인적취합물（ MIP）。용자외분광광도법탐색료불동공능단체여모판분자적결합능력，여공능단체병희산（ AA）상비，MAA 여DOP적결합능력경강，기최가결합적물질적량비위6：1。고찰 MIP 대 DOP、DPHP、린분이갑산이갑지（ DMP）、린분이갑산이정지（ DBP）적선택흡부성능，발현해취합물대 DPHP구유경고적선택흡부성。이제비적취합물위고상췌취전료，결합 HPLC분석，고찰료림세제여세탈제적충류화용량대 DPHP 회수솔적영향。장 DPHP 갑순용액가재지췌취주후용1 mL갑순-수（1：9，v/v）림세，5 mL갑순-을산（9：1，v/v）세탈，DPHP재분자인적고상췌취（ MI-SPE）주상적회수솔체도96.8％，이재비인적고상췌취（ NISPE）주상적회수솔부위52.9％。장건립적 MISPE-HPLC방법응용우측정토구복 DPHP후불동시간점토혈청중 DPHP적농도，발현기혈약농도적최대치위5.88μg/mL，체봉치시간위4 h，DPHP가표회수솔위90.0％~92.0％，상대표준편차소우5％。
The molecular imprinted polymer(MIP)with high selectivity to di(2-propylheptyl) phthalate( DPHP ) was synthesized by precipitation polymerization with dioctyl phthalate ( DOP)as dummy template,methacrylic acid( MAA)as functional monomer and ethylene gly-col dimethacrylate( EDMA)as cross-linker. The binding ability of the template and functional monomer was investigated by UV spectrometry. Compared with the functional monomer acrylic acid( AA),MAA showed stronger binding capacity to DOP and the best combination mole ratio of 6 :1. The selective adsorption performance of MIP for DOP,DPHP,dimethyl phthalate ( DMP)and dibutyl phthalate( DBP)was investigated using the prepared MIP as high perform-ance liquid chromatographic column packing. It was found that the prepared MIP showed higher retention ability and selectivity for DPHP. Using the prepared MIP as a solid-phase extraction (SPE)sorbent(MISPE),the effects of the type and amount of washing solvent and elution solvents on the recovery of DPHP were investigated. After optimization of MISPE profile,the DPHP extraction recovery of 96. 8% was obtained when the following procedures were applied to MISPE cartridge:conditioning with 2 mL methanol,loading with 1 mL methanol,washing with 1 mL methanol-water(1:9,v/v),eluting with 5 mL methanol-acetic acid(9:1,v/v). The recovery of DPHP on non-imprinted polymer( NIP)cartridge was only 52. 9%. The developed MISPE-HPLC method was applied to determine the concentrations of DPHP in rabbit serum at different time points after oral administration. It was found that the maximal concentration (cmax)and time(tmax)were 5. 88μg/mL and 4 h,respectively. The recoveries of spiked DPHP in rabbit serum ranged from 90. 0% to 92. 0% with the relative standard deviations less than 5%.