开管毛细管电色谱分析3种解热镇痛药物  

Analysis of three antipyretic analgesic drugs by open-tubular capillary electrochromatography

作　　者：刘丽丽[1,3] 乔娟 张红医[3] 齐莉 LIU Lili;QIAO Juan;ZHANG Hongyi;QI Li(Key Laboratory of Analytical Chemistry for Living Biosystems, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190, China;School of Chemical Sciences, University of Chinese Academy of Sciences, Beijing 100049, China;College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China)

机构地区：[1]中国科学院化学研究所活体分析化学院重点实验室,北京100190 [2]中国科学院大学化学科学学院,北京100049 [3]河北大学化学与环境科学学院,河北保定071002

出　　处：《色谱》2020年第9期1107-1114,共8页Chinese Journal of Chromatography

基　　金：国家自然科学基金(21727809);中国科学院项目(2007CB714504)。

摘　　要：针对生物体液样品开展药物的绿色高效毛细管电泳分离分析具有重要的研究意义。该研究以3种解热镇痛药(4-氨基安替比林、氨基比林及非那西汀)为研究对象,以嵌段聚合物为涂层,建立了药物的开管毛细管电色谱(OT-CEC)分析新策略。首先,采用活性/可控自由基可逆加成-断裂链转移聚合方法,合成制备得到了两亲性嵌段聚合物-聚(苯乙烯-甲基丙烯酸缩水甘油酯)(P(St-GMA)),并将其涂覆到毛细管内壁;其次,通过考察影响OT-CEC分离效率的关键因素,包括嵌段聚合物的聚合时间、涂覆毛细管嵌段聚合物的浓度、电泳运行缓冲液的种类和pH值、有机溶剂添加剂等,优化了3种解热镇痛药物的OT-CEC分离条件;最终发现,不需添加任何有机溶剂及表面活性剂,仅采用50.0 mmol/L乙酸钠-乙酸(pH 5.7)作为OT-CEC的缓冲溶液,就能实现3种解热镇痛药物的基线分离。在8.0~2.5×10^3μmol/L范围内,分析物峰面积与其对应的浓度呈现良好的线性关系,相关系数(R^2)均大于0.995,检出限为1.0~2.5μmol/L。结果表明:P(St-GMA)在溶液中自组装所形成的类表面活性剂胶团结构增强了两亲性嵌段聚合物与解热镇痛药物之间的相互作用,显著提升了解热镇痛药物的OT-CEC分离效率。该工作不仅为制备新型聚合物及调控嵌段聚合物的自组装行为提供了研究思路,也展示了两亲性嵌段聚合物在药物的绿色OT-CEC分析中的实际应用潜力。The advantages of capillary electrophoresis,such as small sample consumption,high separation efficiency,and multiple separation modes,have been known for decades.However,exploring unique capillary electrophoresis techniques for the analysis of fluid drugs in living bio-systems remains an important and urgent task.Owing to the similar structures and mass-to-charge ratios of antipyretic analgesic drugs,efficient baseline separation of these analytes by capillary zone electrophoresis method cannot be easily achieved.Micellar electrokinetic chromatography can improve the baseline separation of these drugs,but the substantial amounts of non-volatile surfactants(such as sodium dodecyl sulfate,sodium dodecyl sulfonate,sodium deoxycholate and cetylammonium bromide)in running buffer solutions would pollute the ion source during mass spectrometric analysis.For this reason,it is difficult to analyze unknown drugs by capillary electrophoresis-electrospray ionization-mass spectrometry.To overcome these drawbacks,much attention has been paid to capillary electrochromatography(CEC)because combines the high separation efficiency of capillary electrophoresis with the high selectivity of high performance liquid chromatography(HPLC).Recent challenges encountered in open-tubular capillary electrochromatography(OT-CEC)expanding the range of suitable functional polymer monomers and improvement of the separation efficiency by tuning the characteristics of the polymer coatings without using any organic solvent additives.In this study,a protocol based on OT-CEC using a block co-polymer coating is proposed for the analysis of three test antipyretic analgesic drugs(4-aminoantipyrine,antipyrine and phenacetin),without adding organic solvents and surfactants in the running buffer solutions.First,an amphiphilic block co-poly(styrene-co-glycidyl methacrylate)(P(St-GMA)),was synthesized by reversible addition-fragmentation chain transfer polymerization under mild conditions.Then,P(St-GMA)was coated onto the capillary surface,and an OT-CEC analy

关 键 词：开管毛细管电色谱 两亲性嵌段聚合物 解热镇痛药物 

分 类 号：O658[理学—分析化学]