APPLICATIONS OF CERIUM BIS （MONOMYRISTY—LPHOSPHATE）ADSORBENT TO REVERSED PHASE LIQUID CHROMATOGRAPHY

The tetravalent metal salts of monoalkyl phosphates [M(O3POR)2]are a new kind of stationary phases of Chromatography-homogeneous bonded phases.This paper deals with the application of cerium bis(monomyristylphosphate)as support to reversed phase liquid chromatography.The results show that the best mobil phase is CH3CN:H2O=95:5.The good separation to the mixture containing six aromatic hydrocarbons and the determination of naphthalene in a group samples have been achieved.The regression analysis shows that detect limits,linearities and precision for six aromatic hydrocarbons are good.     

THE EFFECT OF pH VALUES OF MOBILE PHASE ON RETENTION BEHAVIOUR OF DISSOCIABLE SOLUTE IN REVERSED PHASE LIQUID CHROMATOGRAPHY (RPLC)

By using aqueous buffers of different pH values as the mobile phase the chromatography retentionbehaviours of some organic acids, bases and ampholytes on the column packed with hexadecyl dimethylsilanebonded stationary phase are investigated. According to the interaction of solute with stationary andmobile phases, and the dissociation equilibrium, the corresponding retention equations are derived. Thedissociation equilibrium constants of some separated compounds are calculated based on the experimentaldata and the derived equations. A comparison with the results of references has been made. Seven bio-chemical compounds which are important in clinic are separated efficiently.     

THE RELATIONSHIP BETWEEN RETENTION VALUES OF HOMOLOGUES AND THE COLUMN TEMPERATURE IN REVERSED－PHASE LIQUID CHROMATOGRAPHY

ＴＨＥ　ＲＥＬＡＴＩＯＮＳＨＩＰ　ＢＥＴＷＥＥＮ　ＲＥＴＥＮＴＩＯＮ　ＶＡＬＵＥＳ　ＯＦ　ＨＯＭＯＬＯＧＵＥＳ　ＡＮＤ　ＴＨＥ　ＣＯＬＵＭＮ　ＴＥＭＰＥＲＡＴＵＲＥ　ＩＮ　ＲＥＶＥＲＳＥＤ－ＰＨＡＳＥ　ＬＩＱＵＩＤ　ＣＨＲＯＭＡＴＯＧＲＡＰＨＹＴＨＥ...     

INFLUENCE OF THE ELUENT COMPOSITION ON RETENTION IN REVERSED PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC)

It is proved for the first time by means of measuring the retention values of 16 compounds that the relationship between solute retention and composition of eluent MeOH/H_2O in reversed phase (RP) system can be described with the equation In k'=b_0 b_1C_B b_2lnC_B which was drawn on the basis of liquid-solid chromatography (LSC) mode. The brief discussion about the several constants in the equation has been done.     

PREPARATION AND EVALUATION OF SMALLBORE REVERSED PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC COLUMN

A smallbore chemically bonded alkyl stationary phase column of 2 mm I. D.(inner diameter) and 15 cm in length having an efficiency of 6400—7600 theoretical plates has been developed. The column officicncy is nearly the same as that of routine analytical column of 4.6—5.0 mm I. D. The amount of cluant used for the smallbore column, however, is less than about one fifth that for the ordinary columns.Using the reaction of monochlorosilane with 5 μm accumulated silica bead produced in Qingdao Ocean Chemical Factory instead of trichlorosilane and irregular silica gel, we have. prepared a nonpolar chemically bonded phase packing which has a higher carbon content and more obvious hydrophobicity. Moreover, the reproducibility of the preparation is better.The equipment and assembly necessary for getting high efficiency with the smallbore column are discussed briefly. Using Model SW-1 smallbore column HPLC instrument developed in the institute with the Model K-1 column fittings and injector, the detector with     

STUDY ON ORGANIC LIGHT—RARE—EARTH ADSORBENT—CERIUM BIS（OCTYLPHOSPHATE）

The tetravalent metal salts of monoalkyl phosphates[M(R-OPO3)2] are a new kind of stationary phases of chromatography-homogeneous bonded phases.The studies on preparation,structure and gas chromatographic efficiency of cerium bis (octylphosphate) (COPP) are reported in this paper. By using chemical analysis,infrared spectra,x-ray diffraction analysis ,the strong evidence that COPP has a layered structure of the α-zirconium phosphate type was demonstrated,the repetitive unit is C8H17OPO3CeO3POC8H17 and there is a little bending or interpenetration of the alkyl chains within the layers.The thermogravimetic analysis of the COPP indicated that it has much more thermalstability than silica-based packings.The thermodynamic parameters ΔH and molecular connectivity indexes x′ for the adsorption of several dozen compounds on the COPP have also been determined by gas chromatographic method,and the fine linearity between them was shown.     

THYMINE BONDED-STATIONARY PHASE FOR HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

A new type of HPLC stationary phase containing thymine derivative wassuccessfully prepared.It was found to give selective separation of nucleic acidbases and several purine derivatives,such as caffeine and theophylline.Theretention behaviour and elution order of the solutes were interpreted in terms ofmolecular structure.     

PREPARATION OF CHITOSAN COATED METAL AFFINITY CHROMATOGRAPHY ADSORBENT

1NTRODUCTIONImmobilizedmetalionaffinitychromatography(IMAC)hasattractedconsiderableattentioninthepurificationofproteinssincePorathfirstlyuseditin1975Llj.IMAChassomeadvantagescomparingtootheraffinitychromatography.Forexample,IMACcanbeoperatedatanhighionstrengthandtheligandsuchasC.2 ischeapandstable.TheconventionalIMACadsorbentswereproducedbyreactingiminodiaceticacid(IDA)withpolysaccharidesuchasagaroseandthentheaffinityligandC.2 waschelatedtothe.d...b..t[2].Thepreparationwasexpensi…     

STUDY OF DERIVATIZATION OF PROTEIN WITH A EUROPIUM CHELATE AND APPLICATION TO HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

A europium chelate of 5-chlorosulfoyl-2-thenoyltrifluoroacetone(CTTA)was investigated for precolumn derivatization ofprotein for high performance liquid chromatography.This new label was highlyfluorescent and suitable for time-resolved fluorometric detection.Thedetective limit of protein is less than 0.3ug in sample with a volume of100ul.Theoretically,the new label can also be used in gel electrophoresisand protein blotting.     

INTERSECTION POINT RULE OF THE RETENTION VALUE AND MOBILE PHASE COMPOSITION OF THE HOMOLOGUES IN REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

Based on the intersection point rule of the retention value and normal boiling point of homologues in reversed-phase high-performance liquid chromatography(RPLC), the intersection point rule of the retention value of homologues and mobile phase composition has been derived, and was testified by a lot of experimental data from the literature. With this newly proposed equation, we can use the retention value of the compound in one mobile phase composition to predict its retention value in any other mobile phase composition. For fourteen groups of homologues in five mobile phase compositions on five Kinds of columns, the overall average absolute error of 721 data sets is 2.8%.     

A UNIFIED RETENTION MODEL OF SOLUTE IN LIQUID CHROMATOGRAPHY

Based on six thermodynamic equilibria,a unified retention model of solute in liquidchromatography(LC)is first proposed.The unified model was tested and proved to be valid for a LC sys-tem with mobile phase consisting of a complete range of multiple,ternary or binary components and eachkind of LC except size exclusion chromatography.In addition,so long as making some assumptions andmathematical conversions,the expressions of various popular models in LC can be derived by using theunified model.     

CELLULOSE MEMBRANE USED AS STATIONARY PHASE OF MEMBRANE AFFINITY CHROMATOGRAPHY

ＣＥＬＬＵＬＯＳＥＭＥＭＢＲＡＮＥＵＳＥＤＡＳＳＴＡＴＩＯＮＡＲＹＰＨＡＳＥＯＦＭＥＭＢＲＡＮＥＡＦＦＩＮＩＴＹＣＨＲＯＭＡＴＯＧＲＡＰＨＹ￥ＷｅｉＧＵＯ；ＺｈｅｎＨｕａＳＨＡＮＧ；ＹｉＮｉａｎＹＵａｎｄＬｉａｎｇＭｏＺＨＯＵ（ＤａｌｉａｎＩｎｓｔｉ...     

SYNTHESIS AND PROPERTIES OF THERMOTROPIC LIQUID CRYSTALLINE COPOLYESTERS CONTAINING BIS（4－HYDROXYPHENYL）METHANONE（Ⅴ）

ＳＹＮＴＨＥＳＩＳＡＮＤＰＲＯＰＥＲＴＩＥＳＯＦＴＨＥＲＭＯＴＲＯＰＩＣＬＩＱＵＩＤＣＲＹＳＴＡＬＬＩＮＥＣＯＰＯＬＹＥＳＴＥＲＳＣＯＮＴＡＩＮＩＮＧＢＩＳ（４－ＨＹＤＲＯＸＹＰＨＥＮＹＬ）ＭＥＴＨＡＮＯＮＥ（Ⅴ）￥ＤｅＷｅｎＤＯＮＧ；ＹｕＳｈａｎＮ...     

SYNTHESIS AND PROPERTIES OF THERMOTROPIC LIQUID CRYSTALLINE COPOLYESTERS CONTAINING BIS（4－HYDROXYPHENYL）METHANONE（Ⅵ）

ＳＹＮＴＨＥＳＩＳＡＮＤＰＲＯＰＥＲＴＩＥＳＯＦＴＨＥＲＭＯＴＲＯＰＩＣＬＩＱＵＩＤＣＲＹＳＴＡＬＬＩＮＥＣＯＰＯＬＹＥＳＴＥＲＳＣＯＮＴＡＩＮＩＮＧＢＩＳ（４－ＨＹＤＲＯＸＹＰＨＥＮＹＬ）ＭＥＴＨＡＮＯＮＥ（Ⅵ）ＳＹＮＴＨＥＳＩＳＡＮＤＰＲＯＰＥＲ...     

COVALENTLY BONDING CHIRAL POLYURETHANE ON AMINATED SILICA GEL： A NEW STRATEGY TO PREPARE CHIRAL STATIONARY PHASE FOR HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

Two polyurethanes of different molecular weights were prepared by the copolymerization of phenyl diisocyanate and diisopropyl tartrate. The polyurethanes having terminal isocyanate groups were reacted with 3-aminopropyl silica gel to afford two chiral stationary phases. The Mn of the two polyurethanes were 4057 g/mol and 6442 g/mol. The polyurethanes and the corresponding chiral stationary phases were characterized by FT-IR, 1H NMR and elemental analysis. The loading capacities of the polyurethanes on silica gel were 0.68 mmol units/g and 0.61 mmol units/g, respectively. The separation performance and the influence of additives, triethylamine and trichloroacetic acid, on the separation of chiral compounds were investigated by HPLC. The chiral stationary phase prepared from polyurethane with Mn of 4057 g/mol demonstrated better enantioseparation capability than that with Mn of 6442 g/mol. Additionally, it was found that the addition of triethylamine and trichloroacetic acid in the mobile phases significantly improved the enantioseparation for these two chiral stationary phases.     

PURIFICATION OF Cd-BINDING PROTEIN FROM MAIZE ROOTS BY REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

An efficient procedure of purification of Cd-binding protein in roots of maize has been established. Young seedlings of maize were exposed to a medium containing CdCl2 to induce the production of Cd-binding protein in their roots. The protein was purified after heat treatment by ion-exchange chromatography and reverse-phase HPLC. The resulting protein was identified as a purified product by N-terminal amino acid with the dansyl method. Its molecular weight was 3200 dalton, the cysteine content was 29.5%, about 3 Cd atoms were bound to one molecule of the protein and the Cd : cystine ratio was 1 : 2.3. According to its character, this protein could be a kind of plant metallothionein-like protein.     

SYNTHESIS OF N－ARYL－4－METHYLPHENOXYACETAMIDES BY MEANS OF LIQUID－LIQUID PHASE TRANSFER CATALYSIS

ＳＹＮＴＨＥＳＩＳ ＯＦ Ｎ－ＡＲＹＬ－４－ＭＥＴＨＹＬＰＨＥＮＯＸＹＡＣＥＴＡＭＩＤＥＳ ＢＹ ＭＥＡＮＳ ＯＦ ＬＩＱＵＩＤ－ＬＩＱＵＩＤ ＰＨＡＳＥ ＴＲＡＮＳＦＥＲ ＣＡＴＡＬＹＳＩＳ￥ＴａｉＢａｏＷＥＩ；ＪｉＣｈｏｕＣＨＥＮ；ＹｏｕＭｉｎｇ...