Mutual Citation

Chromatography, Vol.22 No.2(2001)

Mutual Citation

Chromatography and Related Techniques in China:
a Status Report in 1998-1999
Zhang Yukui, Zhang Qinghe, Zhang Weibing and Xu Guowang
Dalian Institute of Chemical Physics, the Chinese Academy of Scientific, Dalian, 116011, China

Abstract
A overview of the developments of chromatography and related techniques in China during the period of 1998-1999. Specific topic areas covered include gas chromatography (GC), high-performance liquid chromatography (HPLC), capillary electrophoresis (CE) and capillary electrochromatography (CEC), solid phase extraction (SPE) and solid phase microextraction (SPME).
Keywords: chromatography and related techniques, review, status report.

2. Theory and Optimization

1. Introduction
The research on and application of chromatography and related

Geng Xingdu et al. investigated the matching relation between

techniques is one of the most active areas of analytical chemistry in

the number of experimental points and that of parameters of reten-

China. Almost all aspects of chromatography and related tech-tion equations employing two, three and four parameters of theniques currently used in the world are involved. We have reviewed

stoichiometric displacement model for the retention (SDM-R) of

the status of chromatography and related techniques in China [1,2].

homologue in liquid chromatography [3]. They have studied theIn this period, two symposia on chromatography and related tech-

convergent phenomenon of homologues in reversed phase liquidthniques were held. They were the 12 National Symposium onchromatography according to the stoichiomatric displacement

Chromatography (NSC XII) and 8th Beijing Conference and Exhi-model for retention. A general equation was derived for calculating

bition on Instrumental Analysis (BCEIA VIII). Table 1 lists thethe coordinates of the convergent point. The physical meaning of

distribution of the papers on various separation modes published in

the coordinates was discussed from the point of view of thermody-

international journals, Chinese periodicals and the two national

namics. The derived equation was compared and found to fit very

symposia by Chinese scientists during December 1998 through De-

well [4] with experimental data in the mobile phase.

cember 1999. It can be seen that liquid chromatography plays the

The retention equation and the relationship between retention

most important role in the separation science in China. The number

parameters and the parameters of molecular structure deduced byof papers about CE and CEC has increased obviously in comparing

Zou Hanfa et al. from statistic thermodynamics in reversed phaseto that in 1996-1997 [2].

liquid chromatography. It has been used to explain the difference inTable 1. Distribution of the papers in 30 periodicals and two symposia on chromatography and related techniques

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Chromatography, Vol.22 No.2(2001)

selectivity toward a particular species of 16 polycyclic aromatic

3, 4, 5 and 6 chlorine substituted compounds including more thanhydrocarbons (PAHs). They found that each pair of binary solvents

ten kinds of isomerides of polychlorinated dioxin (PCDD), Artifi-

methanol/water, acetonitrile/water and isopropanol/water has its

cial neutral network (ANN) was used to relate the molecular struc-own unique selectivity[5].In another paper, they discussed theoreti-

ture and retention time of PCDD [14]. Lin Leming et al. predicted

cally and experimentally the delay and dispersion of mobile phase

the retention values in thin layer chromatography by using back-in the gradient elution of HPLC [6].

propagation artificial neutral networks (ANNs) and the multi-

Bian Liuzhan et al. studied the thermodynamic behavior forparameter regression analysis with topological indexes. The rathersome proteins and small molecules in hydrophobic interaction

good correlation for 15 amino acids and 24 phenols and aniline de-chromatography in the temperature range from 21-80. The thermo-

rivatives were obtained [15]. Tang Wanying [16] and Zhang

dynamic parameters of these proteins were determined by using

Suping [17] have predicted the chromatographic retention value by

van’t Hoff relationship (lnk’-1/T). The conformational change ofgray model parameters. Wang Lianshen published two papers con-the proteins was judged in chromatographic process by using thecerning the relationship between the retention values and the mo-

obtained standard entropy charge and free energy [7]. Liang Heng

lecular structure of pollutants such as indole compounds and het-

established the separation model of CE based on nonequilibrium

erocyclic nitrogen compounds in liquid chromatography [18,19].

thermodynamics separation theory. By taking the operating voltage

The QSAR in TLC has been reviewed by Wang Q. et al. [20].

as controllable parameter and the net separation entropy of solute

Wang Hong established the systematic optimization for thesystem as objective function, the optimizing control orbit can be

MEKC separation of PTC-amino acids by using a dynamic scout-obtained by optimal design of the separation system, [8].

ing optimization method-controlled weighted centroid variable size

Zhang Lefeng presented a new method for the calculation of

simplex algorithm [21]. Wang Jingqing [22] and Lin Xuan [23] ap-

thermodynamic parameters based on two or more retention times

plied pattern recognition method and artificial neural network tounder different temperature conditions in gas chromatography.

solve the optimization of operating conditions in HPLC. Zhang

These thermodynamic parameters can predict retention time underWeibing theoretically discussed the relationship of retention of

any other temperature conditions [9].

compounds in multiple injection. The results showed that the ca-

Jiao Qingcai derived a few linear retention equations including

pacity factors of two solutes in a sample and the interval between

the various chromatographic parameters (for example, column tem-the two injections were the main factors affecting the separation

perature, composition of mobile phase, number of carbon atoms of[24].

the solute molecules, solvent molecules and alkylligand on bonded

In comparing with that of 1996-1997, the number of papers

phase surface) by using thermodynamic method based on both theabout resolution of overlapping chromatographic peaks has in-displacement adsorption multi-interaction model in reversed-phasecreased obviously. These methods included the window factor

liquid chromatography and the Martin equation. Both the linear re-analysis technique [25], wavelet transform [26], orthogonal projec-

tention rules and the experimental phenomena could be explained

tions [27] and fast Fourier transform [28]. Wang Lishi comparedby these equations. The other linear retention rules which were not

the results of wavelet smoothing and wavelet denoising for proc-

reported in literatures have also been predicted and verified experi-

essing CE signals. They found that the signal peaks are broadened

mentally [10].

and shortened by using wavelet smoothing, however, the peaks are

The kinetic origin of the profile was further investigated based

well described by using wavelet denoising [26]. Chen Dizhao et al.

on the idea of relaxation theory in the mobile phase by a way ofdeveloped the heuristic evolving latent projections (HELP) and an-

jumping process. The mathematical expression of profile wasnihilation of rank and resolution by projection (AR-RP). The ap-

gained. The form of profile was also discussed digitally with theproach have been successfully applied to the qualitative and quanti-

computer solution and compared with the experimental results

tative analysis of complete real multicomponent system with phe-

[11,12]. Dai Chaozheng studied the dynamic process of electro-

nols and PAHs [29].

chromatography and compared with that of HPLC. A general plate
3. Gas Chromatographyheight equation has been derived to express the effect of axial dispersion in the CEC process, mass transfer resistance at the mobile

Wu Caiying’s group has published several papers on the prepa-

phase, kinetic resistance associated with the reversible binding ofration and characterization of new stationary phases for capillary

eluite by the stationary phase and the temperature distribution ef-

gas chromatography such as crown ether capped cyclodextrine,

fect [13].

fulleropyrrolidine functionalized polysiloxane, derivatives of calix-

Zhao et al. investigated the molecular structure and feature se-arene and mixed stationary phases [30-34]. The polarity, chemical

lection for 76 kinds of homologues (1 to 8 chlorine substituent) forstability and thermostability of the stationary phase have been

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Chromatography, Vol.22 No.2(2001)

Zhang Yukui, Zhang Qinghe, Zhang Weibing and Xu Guowang

evaluated.

disubstituted benzene isomers was better than that on each of theZhou Liangmo have extensively studied the retention mecha-functional bonded silica stationary phase. The 3- (Aza-18-crown-6)

nism in the separation of chiral compounds on the bonded cy-

propylsilyl and calixa [4] rene bonded silica stationary phases wereclodextrine stationary phase in GC [35,36]. Yuan Liming et al.

synthesized also [52-54]. Zhang Qinghe et al. prepared porous zir-separated ethylbenzene/benzene, o-xylene/benzene, styrene/ben-conia, silica-zirconia and magnesia-zirconia particles by sol-gel

zene and styrene/toluene on the mixed stationary phases composed

process. The physical and chemical properties and chroma-of perpentylated bata-cyclodextrin and AgNO3, perpentylated beta-

tographic character were studied [55,56].

cyclodextrin and TlNO3, Benton-34 and AgNO3 in GC. The posi-

Zhou Liangmo et al. described the recent advances of mem-tive or negative synergistic effects was investigated extensively

brane chromatography in liquid chromatography [57]. The group of[37-39]. A mesoporous molecular sieve of the HMS type was pre-Zou Hanfa has prepared several membrane medium with different

pared and its applications as adsorbent for gas-solid chromatogra-

functional groups. The column efficiency and the column pressure

phy were evaluated by probing system as C 1-C 15 paraffins mix-

drop [58,59] have been studied. Shang Zhenghua prepared an affin-tures, aromatic hydrocarbons, alcoholes, halohydrocarbons and ke-

ity material for endotoxin removal from nylon 66 microfiltration

tones. The results indicated the mesoporous molecular sieve ad-

membrane. The results of immobilization of histidine ligand on thesorbent have unique features in comparing to the conventional

membrane with different activation agents were compared andmicro-molecular sieve and porous polymer adsorbents [40].

evaluated [60].

Most of the GC papers focused on the applications of GC to

Most of the HPLC papers focused on the applications of HPLC

environmental, medical and natural plant analyses. Xu Guowang etanalysis to medicine and clinic. New development and its applica-

al. monitored aldehydes and ketones pollutants in the gas of fixed

tions on biochemical research of affinity and hydrophobic interac-pollution source [41], Zhang Xiangming et al. determined the emis-tion chromatography (HIC) have been reviewed [61,62]. The num-sion amount of aromatics in exhaust gases from paint industry [42].

ber of papers about HPLC in medical analysis is about 60% of the

Li et al. analyzed the medicine by using GC [43].

published in the Journal of Yaowu Fenxi Zazhi during 1998-1999.
The applications of ion chromatography have many reports inthe past two years [63-65].

4. High Performance Liquid Chromatography
Preparation of liquid chromatographic columns has attracted at-

5. Capillary Electrophoresis and Electrochromatography

tention from several groups in China. Zhou Liangmo prepared thehighly efficient rod-shape poly (methacrylic acid-co-styrene-co-

Several reviews summarized the current state of the theory anddivinylbenzene) column by an in-situ free-radical polymerization

practice of capillary electrophoresis, e.g. the electroosmosis [66],in column. Aromatic acids and polycyclic aromatic hydrocarbons

temperature effect and temperature gradient technique [69], affinity

were separated [44]. Geng Xingdu prepared poly (acrylamide-co-[68] and non-aqueous capillary electrophoresis [69]. The applica-

butyl methacrylate-co-N, N’-methylenebisacrylamide) hydrophobic

tions of capillary electrophoresis have summarized in several re-interaction chromatographic continuous rod column in situ by di-views on environmental analysis [70], Chinese traditional medicine

rect polymerization of monomer mixture and porogenic solvents in[71], polysaccharides [72], alkaloid [73], toxin [74], DNA [75],stainless tube. This column could be used in separation and in thespeciation analysis [76] and chiral enantiomers [77].
Lin Bingcheng et al. developed a novel buffer based on low

study of retention mechanism of proteins [45].
Wang Jingfang et al. prepared molecular imprinting polymers

molecular weight hydroxypropylmethylcellulose to separation(MIPs) against Cbz-L-Ser, Cbz-L-Ala and Cbz-L-Pro utilizing

DNA fragments. The influence of additives such as urea and man-acrylamide plus 2-vinylpyridine as combined basic functional

nitol was investigated. The possible mechanism for the separation

monomers and evaluated in HPLC mode. The polymer sphericalof DNA fragments was also discussed [78]. Chen Yi et al. sepa-

stationary phase for HPLC have been prepared by different groups

rated basic protein using a homemade electric field modulated cap-

[46-48]. Cheng Liren et al. have prepared the chiral stationary

illary electrophoresis, which can offer both radial and axial electricphase coated cellulose derivatives, polymer coated silica and cross-fields with only one high power supply. The adsorption of protein

linked polymer HPLC stationary phase [49-51].

molecules onto the tubing wall can be regulated by the application

Da Shilu et al. have prepared some mixed functional HPLC sta-of a radial voltage : as the band broadening decreases with the in-tionary phases containing aza crown and beta-cyclodextrin, 8-

crease of the radial voltage. This implied that it may be possible toquinolinol derivatized beta-cyclodextrin bonded silica via continu-

dynamically control the adsorption of protein molecules on silica

ous solid-liquid reaction method. The results showed that the sepa-

surface [79,80]. Chen Jieke et al. reported the use of home-maderation ability of the new mixed functional stationary phase forCE with amperometric detection system to the analysis of neuro-

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transmitters in a single sympathetic nerve cell of rat. Isoproterenol

Zou Hanfa et al. summarized the current state of open tubular

was selected to be the internal stand and for the determination ofcapillary electrophoresis [120]. The methods for preparation of thenorepinephrine and epinephrine in a single sympathetic nerve cellcoated capillary used in CE have been reviewed [121]. Fu Ruonong[81]. In another paper, they developed a sensitive, rapid and a accu-

et al. prepared the open tubular capillary electrochromatography

rate method to analyze of the amine acid neurotransmitters in dor-column by using sol-gel process [122]. Liu Xiaoda et al. prepared asal root ganglion of art by using CE with a laser-induced

cross-linked polyacrylamide coated capillary by radiation-induced

fluorescence-charge coupled device and fluorescein isothiocyanate

with basic buffers [123]. High performance linear polyacrylamide[82]. A capillary electrophoresis-laser induced fluorescence-

capillary gel electrophoresis columns were prepared and character-intensified charged coupled device system was used for the high-ized by Shi Wei et al. [124].

sensitivity analysis of two important nature amino sugar, glu-

Liu Zheng et al. studied the relationship between retention

cosamine, galactosamine and glucosaminic acid [83]. Che Fa-Yun

value in micellar electrokinetic chromatography and LogP. The ef-

et al. analyzed 8-aminonaphthalene-1, 3, 6-trisulfonate derivatizedfect of organic modifier on the capacity factors of solutes haveoligosaccharides by CE electrospray ionization quadrupole ion trap

been examined too [125,126]. Zhang Lihua found the main factors

MS, and they have studied the distribution of ovalbumin glyco-

contributing to the retention of solutes in reversed phased capillaryforms by CE [84]. The applications of CE in medicine and naturalelectrochromatography were the solute size and the ability of solute

plant, some example are listed in Table 2.

to accept hydrogen bond [127].

To measure the free concentration of verapamil (a basic drug)

The detection of capillary electrophoresis was another hot

enantiomers in the binding system of human serum albumin

topic. Fang Yuzhi analyzed theoretically the factors affecting zone

(HSA), Lin Bingchen et al. established a capillary electrophoresis

broadening in capillary electrophoresis-amperometric detection at

method, liquid precolumn, and the method was examined system-disk-shaped electrode. A model equation about it was given. The

atically. The method was used to determine the binding constants

effect of injection time of sample, separation voltage and dead vol-of the basic racemic drug, verapamil to human serum albumin un-ume of the detector on zone broadening was experimentally exam-

der drug-HAS binding equilibrium [110,111]. Luo Guoan deter-

ined, and the model equation derived for the zone broadening wasmined the binding constant between fluorescein isothiocyanate la-verified [128]. Wang Erkang et al. described a new electrochemical

beled bovine serum albumin and its monoclonal antibody using thecell assembly possessing advantages of easier construction and op-

ligand separation mode of affinity capillary electrophoresis with la-eration, and good reproducibility. The construction and operation

ser induced fluorescenece detection [112]. On-line concentration

was demonstrated to be reliable and precise by examining the re-technique of capillary electrophoresis was studied by Ou Qingyu

produciblity, the concentration range of linearity and detection[113] and Sun Jingzheng [114], separately.

limit for phenols and catecholamines with the cell [129]. Wang

Capillary electrochromatography, which represents a hydrid of

Lishi et al. described the development of a scanning voltammetricchromatographic and electrophoretic techniques, has experienced

detector for CE. The scanning electrode potential waveform gen-dramatic growth in the past two years. Many papers have been pub-eration and the current signal acquisition were controlled by a mi-lished during the covered period dealing with the theory and prac-crocomputer interfaced with a home-made card witch is equipped

tice of CEC. The separation mechanism of CEC have been studied

with 12 bit digital-analog converter (D/A) and a 12 bit analog-

by several groups [115,116]. Fu Ruonong et al. discussed the effectdigital converter (A/D). The methods of potential control and sig-of double layer overlap on the performance and electroosmotic ve-

nal acquisition are discussed [130]. Chen Yi et al. established alocity in the packed capillary CEC. The theory analysis on the dou-

novel CE system which offered several ways to control electroos-ble layer overlap in the packed CEC was described. The results

mosis by electric field. The main feature of the system was a spe-

showed that the packing structure and the homogeneity of thecially fabricated capillary-cartridge unit, with which they canpacked bed were the internal factor that resulted in the emergenceachieve CE separation and electroosmosis control using flexibleof the double layer overlap in the packed CEC [117]. In the anothersilica capillary and only one high-voltage power supply [131]. Lin

paper, they studied the chromatographic behavior pressurized flow-

Bingchen et al. complied a computer program to work out the ray

driven electrochromatography. The experimental results were dis-tracing of UV detector of HPCE. Based on results obtained by cal-cussed in relation to theoretical considerations [118]. Zhang Lihua

culation, some practical methods for adjusting the distance between

et al. proposed a new method for shorten the retention time of sam-lens and capillary were provided to make the UV detector to work

ples in CEC by a commercial CE instrument with the ability toon optimal conditions [132].

change the mobile phase vials automatically. The method wasproved to have quite good reproducibility [119].

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Chromatography, Vol.22 No.2(2001)

Zhang Yukui, Zhang Qinghe, Zhang Weibing and Xu Guowang

Table 2. The applications of capillary electrophoresis and capillary electrochromatography in analysis of drugs nature plants

time and the stronger affinity to both polar and nonpolar com-

6. Others
Wang Zhenyu prepared the solid-phase coating with hydroxy-pounds. The ideal results was obtained for the enviromental sam-terminated poly (dimethylsiloxane) in SPME. The coating pos-ples [133]. Zhang Daoning et al. have compared the SPME andsessed higher thermal stability shorter extraction and desorption

SPE to enrich organochloride compounds in water samples and

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Yukui. Chemical J. Chinese University, 1998, 19(10), 1556

analyzed by GC with electron capture detector. The results showed[7]that SPME was a faster and more effective method in sample

Bian Liuzhan, Chen Guoliang, Li Rong, Li Huanru. Acta
Chimica Sinica, 1998, 56: 807

preparation. Several commercial solid phases in extraction of mod[8]erately polar organic compounds were compared and the results in-

Li Yanping, Yu Lie, Xie Youbo, Liang Hen. Acta Chimica
Sinica, 1999, 57(3), 281

dicated that polyacrylated was the best [134]. Wang Yiru et al. ana[9]lyzed naphthalene, 1-nitronaphthalene and 2-nitronaphthalene by
SPME with 100 µm polydimethylsiloxane and GC-ITD detection

Chen Jiping, Zhang Lefeng, Tian Yuzeng. Sepu, 1998, 16(1), 6-12

and the limits of the three compounds were 0.25, 0.30 and 0.20 µg.

[10] Jiao Qingcai, Liu Qian, Chen Yaozu. Acta Chimica Sinica,
1999, 57(3), 281

L-1, respectively [135]. Zou Hanfa et al. determinated the aromatic[11] Zhang W B, Proceedings of international Eight Beijing Con-

amines in the waste water by SPE and HPLC [136].

ference and Exhibition on instrumental Analysis, Oct.25-28,

You Jing et al. reviewed the applications of supercritical fluid

1999, Beijing

extraction (SFE) on environmental sample analysis. Li Hua reviewed the development and application of SFC in enantiomers[12] Zhang Weibing, Li Ruijiang, Xu Guowang, Hong Qongfa,

separation. The separation modes and choices of experimental con-

Zhang Yukui. Fenxikexuexuebao, 1999, 15(3), 199

dition were discussed also [137]. Du Qizhen et al. determined the[13] Dai Chaozhen, Sepu, 1999, 17, 514

retention percentages of the stationary phase at various flow rates[14] Zhao Ruihuan, Yue Bingfang, Shan Yichu, Zou Hanfa,
Zhang Yukui. Sepu, 1999, 17(2), 112-114

of fifteen two-phase solvent systems in three types of counter-[15] Wang Yuesong, Zhang Jun, Lin Leming. Sepu, 1999, 17(2),current chromatographic apparatus equipped with small middle and14-17; 18-20

large-bore colied columns [138]. Cao Xueli et al. separated and pu-[16] Tang Wanying, Zhou Shenfan, Yang Linxiao, Sepu, 1998,

rified the isoflavones from Pueraria Lobata by high-speed counter-16(2), 95-99

current chromatography [139]. Wang Hong reviewed the recent development in principle and applications of optical chromatography,[17] Zhang Suping, Song Zhaolin, Len Jing, Zhang Xiaodan,

and they theoretically studied the relationship between the particle

Zhou Shanhua. Chemical J. Chinese University, 1999, 20(10), 1581

radius with the intensity of the applied laser radiation force using a[18] Li L, Yang H, Ding Y, Wang L, Zhang Z, J. Liq. Chrom &ray-optics model by analyzing the force-status of the separated par-Rel. Technol., 1999, 22(6) , 897-907

ticles in the mobile phase [140]. Guan Yafen analyzed the heavy[19] Dai J, Yao S, Ding Y, Wang L, J. Liq. Chrom & Rel. Tech-oils from petrochemical industry by an on-line coupled packed cap-nol., 1999, 22 (15) , 2271-2282

illary HPLC and high temperature capillary gas chromatography[20] Wang Q S, Zhang L, Liq. Chrom & Rel. Technol., 1999, 22[141,142].

(1) , 1-

In conclusion, chromatographers of China have obtained great[21] Wang Hong, Hu Hanfang, Shang Sufeng, Ding Tianhui, Gu

achievements in chromatography and related techniques, especially, capillary electrophoresis, which have been studied exten-

Junlin, Fu Ruonong. Sepu, 1998, 16, 293

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[24] Zhang Weibing, Xu Guowang, Li Ruijiang, Zhang Yukui.
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