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迎头法与微扰法测定 RP-HPLC 系统中吸附
等温线的比较
#
丛景香
1,2
,黄照昊
1
,李丹
1
,姜韦
1
,李雨晴
1*
基金项目:高等学校博士学科点专项科研基金新教师类资助课题(20122120120003)。辽宁科技大学省级
重点实验室开放基金资助课题(USTLKL 2012-04)
作者简介:丛景香(1979-),女,讲师,主要研究方向:制备色谱基本理论及应用. E-mail:
congjingxiang@126.com
(1. 辽宁科技大学化学工程学院应化系; 5
2. 辽宁科技大学精细分离工程中心)
摘要:反相高效液相色谱(RP-HPLC)是广泛应用于精细化学品制备分离过程中的关键方
法之一。RP-HPLC 中吸附等温线的测定具有重要意义。本文以具有一定质量纯度的苯酚及
1-萘酚两组分作为目标物,分别采用迎头法和微扰法测定了目标物在 RP-HPLC 系统中的吸10
附行为,制备色谱柱采用匀浆法填充,固定相为 20μm C18,流动相为体积比为 17:3 的甲
醇-水溶液。应用单组分近似及迭代拟合给出了两组分的非线性 Langmuir 型吸附等温线。根
据两种方法测定的吸附等温线参数,采用数值方法计算了目标物的保留值,结果表明微扰法
测定结果更接近实测值。
关键词:吸附等温线;RP-HPLC;迎头法;微扰法 15
中图分类号:O656.3
Comparison of frontal analysis and perturbation method in
determination of adsorption isotherm in RP-HPLC system
Cong Jingxiang
1,2
, Huang Zhaohao
1
, Li Dan
1
, Jiang Wei
1
, Li Yuqing
1
20
(1. Department of Applied Chemistry, School of Chemical Engineering, University of Science and
Technology Liaoning;
2. Engineering Center of Fine Separation, University of Science and Technology Liaoning)
Abstract: Reversed phase high performance liquid chromatography (RP-HPLC) has been widely
used in the process of preparation and separation of fine chemicals. The determination of 25
adsorption isotherm is very important in RP-HPLC. The phenol and 1-naphthol were selected as
the targets in this paper; the frontal analysis and perturbation method were used to measure the
isotherms of phenol, 1-naphthol and their mixture in RP-HPLC. The preparative column was
packed with 20μm C18 by slurry method, and methanol-water (17:3, v/v) was used as the mobile
phase. Using one-component approximation and iterative fitting, the nonlinear Langmuiran 30
adsorption isotherms of the two components and their mixture were given. Based on the isotherm
parameters obtained by the two methods, the retention values of the targets were obtained by
numerical calculation, which shows that the values obtained by perturbation method were closer to
the measured values.
Key words: Adsorption isotherm; RP-HPLC; frontal analysis; perturbation method 35
0 引言
反相高效液相色谱(RP-HPLC)具有分离精度高、效率高、速度快、可常温操作等优
点,已广泛应用于食品、药品、化工产品、环境监测等领域,尤其是在精细化学品的制备分
离过程中,RP-HPLC 已成为必不可少的手段之一
[1]
。由于对目标产品产量的要求,制备色
谱往往需要增大进样量,因而产生非线性效应。而溶质的非线性色谱行为则主要通过测定吸40
附等温线,即 在一定温度下溶质分子在两相界面上进行的吸附过程达到平衡时它们在两相中
浓度之间的关系曲线来进行表征
[2]
。利用吸附等温线这一热力学性质,是了解组分在色谱柱