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1.
Journal of Pharmaceutical Analysis ; (6): 421-429, 2023.
Article in Chinese | WPRIM | ID: wpr-991155

ABSTRACT

Chiral metal-organic frameworks(CMOFs)with enantiomeric subunits have been employed in chiral chemistry.In this study,a CMOF formed from 6-methoxyl-(8S,9R)-cinchonan-9-ol-3-carboxylic acid(HQA)and ZnCl2,{(HQA)(ZnCl2)(2.5H2O)}n was constructed as a chiral stationary phase(CSP)via an in situ fabrication approach and used for chiral amino acid and drug analyses for the first time.The{(HQA)(ZnCl2)(2.5H2O)}n nanocrystal and the corresponding chiral stationary phase were systematically characterised using a series of analytical techniques including scanning electron microscopy,X-ray diffraction,Fourier transform infrared spectroscopy,circular dichroism,X-ray photoelectron spectros-copy,thermogravimetric analysis,and Brunauer-Emmett-Teller surface area measurements.In open-tubular capillary electrochromatography(CEC),the novel chiral column exhibited strong and broad enantioselectivity toward a variety of chiral analytes,including 19 racemic dansyl amino acids and several model chiral drugs(both acidic and basic).The chiral CEC conditions were optimised,and the enantioseparation mechanisms are discussed.This study not only introduces a new high-efficiency member of the MOF-type CSP family but also demonstrates the potential of improving the enantiose-lectivities of traditional chiral recognition reagents by fully using the inherent characteristics of porous organic frameworks.

2.
Journal of Pharmaceutical Analysis ; (6): 323-339, 2023.
Article in Chinese | WPRIM | ID: wpr-991147

ABSTRACT

Capillary electrochromatography(CEC)plays a significant role in chiral separation via the double sepa-ration principle,partition coefficient difference between the two phases,and electroosmotic flow-driven separation.Given the distinct properties of the inner wall stationary phase(SP),the separation ability of each SP differs from one another.Particularly,it provides large room for promising applications of open tubular capillary electrochromatography(OT-CEC).We divided the OT-CEC SPs developed over the past four years into six types:ionic liquids,nanoparticle materials,microporous materials,biomaterials,non-nanopolymers,and others,to mainly introduce their characteristics in chiral drug separation.There also added a few classic SPs that occurred within ten years as supplements to enrich the features of each SP.Additionally,we discuss their applications in metabolomics,food,cosmetics,environment,and biology as analytes in addition to chiral drugs.OT-CEC plays an increasingly significant role in chiral separation and may promote the development of capillary electrophoresis(CE)combined with other instruments in recent years,such as CE with mass spectrometry(CE/MS)and CE with ultraviolet light detector(CE/UV).

3.
Journal of Pharmaceutical Analysis ; (6): 209-215, 2023.
Article in Chinese | WPRIM | ID: wpr-991136

ABSTRACT

Here,a styrene-based polymer monolithic column poly(VBS-co-TAT-co-AHM)with reversed-phase/hydrophilic interaction liquid chromatography(RPLC/HILIC)bifunctional separation mode was success-fully prepared for capillary electrochromatography by the in situ polymerization of sodium p-styrene sulfonate(VBS)with cross-linkers 3-(acryloyloxy)-2-hydroxypropyl methacrylate(AHM)and 1,3,5-triacryloylhexahydro-1,3,5-triazine(TAT).The preparation conditions of the monolith were optimized.The morphology and formation of the poly(VBS-co-TAT-co-AHM)monolith were confirmed by scanning electron microscopy(SEM)and Fourier transform infrared spectroscopy(FT-IR).The separation perfor-mances of the monolith were evaluated systematically.It should be noted that the incorporation of VBS functional monomer can provide π-π interactions,hydrophilic interactions,and ion-exchange in-teractions.Hence,the prepared poly(VBS-co-TAT-co-AHM)monolith can achieve efficient separation of thiourea compounds,benzene series,phenol compounds,aniline compounds and sulfonamides in RPLC or HILIC separation mode.The largest theoretical plate number for N,N'-dimethylthiourea reached 1.7×105 plates/m.In addition,the poly(VBS-co-TAT-co-AHM)monolithic column showed excellent reproducibility and stability.This novel monolithic column has great application value and potential in capillary electrochromatography(CEC).

4.
Bol. latinoam. Caribe plantas med. aromát ; 21(4): 548-560, jul. 2022. ilus, tab, graf
Article in English | LILACS | ID: biblio-1527072

ABSTRACT

Yerba mate ( Ilex paraguariensis ) produces several secondary metabolites of interest to the phar maceutical industry, such as chlorogenic acids and methylxanthines. These compounds have been produced in vitro by callus culture from different species. However, for I. paraguariensis , no studies upon the production of these compounds in vitro have been p erformed to date. In this work, we show that the concentration of secondary metabolites from I. paraguariensis callus is possible and highly dependent on the callus growth phase. We observed that the best phase for the production of secondary compounds in calli of yerba mate is the stationary growth phase on both genotypes tested. In this phase, higher levels of phenolic compounds, chlorogenic acid and 3,5 - dicaffeoylquinic acid and greater antioxidant activity were observed. Chlorogenic acid and 3,5 - dicaffe oylquinic acid presented positive correlation with antioxidant activity. For the first time, secondary compounds were reported in yerba mate calli cultivated in vitro .


La yerba mate ( Ilex paraguariensis ) produce varios metabolitos secundarios de interés para la industria farmacéutica, como los ácidos clorogénicos y las metilxantinas. Estos compuestos se han producido in vitro mediante cultivo de ca llos de diferentes especies. Sin embargo, para I. paraguariensis , hasta la fecha no se han realizado estudios sobre la producción de estos compuestos in vitro . En este trabajo, mostramos que la concentración de metabolitos secundarios desde callos de I. pa raguariensis es posible y altamente dependiente de la fase de crecimiento del callo. Observamos que la mejor fase para la producción de compuestos secundarios en callos de yerba mate es la fase de crecimiento estacionario en ambos genotipos probados. En es ta fase se observaron niveles más altos de compuestos fenólicos, ácido clorogénico y ácido 3,5 - dicafeoilquínico y una mayor actividad antioxidante. El ácido clorogénico y el ácido 3,5 - dicafeoilquínico presentaron correlación positiva con la actividad antio xidante. Por primera vez, se reportaron compuestos secundarios en callos de yerba mate cultivados in vitro .


Subject(s)
Ilex paraguariensis , Genotype , Antioxidants
5.
Journal of Pharmaceutical Analysis ; (6): 509-516, 2022.
Article in Chinese | WPRIM | ID: wpr-955464

ABSTRACT

Homochiral metal-organic frameworks(MOFs)have attracted considerable attention in many fields of research,such as chiral catalysis and chiral chromatography.However,only few homochiral MOFs can be effectively used in capillary electrochromatography(CEC)and their performances are far from adequate.In this study,we successfully synthesized achiral nanocrystalline MIL-53.A facile post-synthetic modi-fication strategy was then implemented to functionalize the product,yielding a homochiral MOF:L-His-NH-MIL-53.This MOF was then employed as a chiral coating in open-tubular CEC mode(OT-CEC),and,as such,it exhibited high enantioselectivities for several racemic drugs.The homochiral MOF and the fabricated capillary coating were systematically characterized using transmission electron microscopy,scanning electron microscopy(with energy-dispersive X-ray spectrometry),Fourier-transform infrared spectroscopy,X-ray diffractometry,thermogravimetric analysis,circular dichroism spectroscopy,Bru-nauer-Emmett-Teller surface area measurements,and X-ray photoelectron spectroscopy.This study is expected to provide a new strategy for the design and establishment of MOF-based chiral OT-CEC systems.

6.
Chinese Pharmaceutical Journal ; (24): 1289-1294, 2020.
Article in Chinese | WPRIM | ID: wpr-857629

ABSTRACT

OBJECTIVE: To establish a platelet cell membrane chromatographic model and investigate the retention behaviors of anti-platelet aggregation drugs on chromatographic column at different temperatures, and simulate the interactions between drugs and platelets under normal and febrile pathological conditions. METHODS: The platelet cell membrane chromatographic stationary phase was constructed by physical adsorption method. The column was packed with wet method. The protein content was determined by BCA protein concentration assay kit. The biological activity was determined by Na+, K+-ATPase assay kit. The chromatographic model was used to investigate the specificity of the column and the retention characteristics of drugs in the temperature range of 35.0-42.0℃. RESULTS: The activity of platelet ATPase was 0.214, and the concentration of platelet membrane protein was 0.340 9 mg•mL-1 before bonding and 0.080 5 mg•mL-1 after bonding. The retention characteristics of clopidogrel, dipyridamole and cilostazole on platelet cell membrane chromatographic column and blank silica gel column were quite different. The retention time of the three drugs on platelet cell membrane chromatographic column was the maximum at 36.0℃, and then decreased with the increase of temperature. CONCLUSION: A platelet cell membrane chromatographic model is successfully constructed, and the retention characteristics of antiplatelet aggregates at different temperatures are studied for the first time. The chromatographic retention behaviors of antiplatelet aggregates at normal and febrile body temperatures are simulated.

7.
Article | IMSEAR | ID: sea-185437

ABSTRACT

Chromatography can be described as a mass transfer process involving adsorption using a nonpolar stationary phase and a mobile polar phase titrating through the column. The active component of the column, the sorbent or the stationary phase , is typically a granular material made of solid particles (e.g. silica, polymers, etc.,). The component of the sample mixture are separated from each other by means of mobile phase and different degrees of interaction with the sorbent particles based on their relative polarity. In the present study we have extracted piperine from grounded pepper using different chemicals such as petroleum ether, acetone and methanol. Petroleum ether extraction showed higher piperine content of 9.12% than methanol and acetone 3.15% and 3.37% respectively.

8.
Malaysian Journal of Microbiology ; : 444-451, 2018.
Article in English | WPRIM | ID: wpr-751179

ABSTRACT

Aims@#YuiC is a stationary phase survival (Sps) protein from the Firmicute Bacillus subtilis that possesses muralytic activity to cleave bacterial cell-wall peptidoglycan. It has a small lytic transglycosylase (MltA) fold analogous to the resuscitation promoting factors (Rpfs) of Actinobacteria which have a hybrid of a mini lysozyme and soluble lytic transglycosylase (Slt35/70) fold. The present study aimed at identifying key residues of YuiC/Sps that are catalytically active and studying the effect of B. subtilis cell growth upon sps/yuiC deletion. @*Methodology and results@#Four forms of mutated yuiC were created through Site-directed, Ligase-Independent Mutagenesis Polymerase Chain Reaction (SLIM PCR) that include the substitutions of D129A, D151A, D162A and K102A. These individual mutated yuiC genes were cloned and expressed in the Escherichia coli BL21 (DE3) expression system and subsequently purified to homogeneity using affinity, cation exchange and size exclusion chromatography. The D129A variant was shown to be insoluble, indicating its role in maintaining the right protein folding of YuiC. The remaining three variants resulted in soluble proteins but were inactive on zymograms indicating that they may be responsible for catalysis. B. subtilis cells harbouring individual sps genes (yuiC, yabE, yocH and yorM) knocked out showed stationary phase defects and altered colony morphologies compared to the wild type. @*Conclusion, significance and impact of study@#This study has identified the key residues involved in catalysis of YuiC, which are the D151, D162 and K102. These are conserved in Sps domains. The catalytic mechanism of YuiC is similar to the mechanism reported for Neisseria gonorrhoeae MltA. sps/yuiC knock outs have implied that each sps/yuiC has a significant role on B. subtilis late growth stage. The B. subtilis YuiC/Sps model has given an insight into Sps functions in the final growth stage of the Firmicutes, which members include etiologic agents of anthrax, botulism and listeriosis. Inhibition of Sps protein may inactivate pathogen replication and facilitate entrance into a non-contagious dormant sporulation stage.

9.
Chinese Journal of Analytical Chemistry ; (12): 734-740, 2017.
Article in Chinese | WPRIM | ID: wpr-512384

ABSTRACT

2-(Dimethylamino)ethyl methacrylate and sodium monochloroacetate were employed to synthesize [2-(Methacryloyloxy)ethyl] dimethyl ammonium acetate (CBMA) functional monomer.CBMA was grafted on the surface of silica by surface initiated atom transfer radical polymerization (SI-ATRP) to obtain silica-CBMA hydrophilic interaction stationary phase.Three silica-CBMA stationary phases with different grafted density of CBMA monomer were synthesized in SI-ATRP progress by changing the concentration of CBMA under the same conditions.The ability to separate organic acid compounds of the synthesized silica-CBMA stationary phases was evaluated under different conditions, including effects of pH value, salt concentration and content of water of mobile phase on retention of solutes.The results showed that the stationary phases could effectively separate organic acid compounds in HILIC mode, which followed a mixed mode of chromatography of ion exchange and hydrophilic interaction.The retention of solutes decreased with the increases of salt concentration of mobile phase, which consistent with the characteristics of ion exchange;the pH value of mobile phase had significant influence on ionization of the stationary phase and solutes, i.e., the retention of solutes increased as the increasing of pH value of mobile phase.However, the retention of solutes decreased with the increasing of the content of water in mobile phase, which was the typical characteristic of HILIC.The method of hydrophilic interaction chromatography combined with silica-CBMA stationary phases could conveniently determinate the content of vitamin C and rutin in rutin tablets, providing a new method for the separation and determination of strong polar samples.

10.
Journal of Pharmaceutical Analysis ; (6): 156-162, 2017.
Article in Chinese | WPRIM | ID: wpr-618381

ABSTRACT

In the pharmaceutical industry, the analysis of atropisomers is of considerable interest from both scientific and regulatory perspectives. The compound of interest contains two stereogenicaxes due to the hindered rotation around the single bonds connecting the aryl groups, which results in fourpotential configurational isomers (atropisomers). The separation of the four atropisomers was achieved on aderivatized β-cyclodextrin bonded stationary phase. Further investigation showed that low temperatureconditions, including sample preparation (?70 °C), sample storage (?70 °C), and chromatographic separation (6 °C),were critical to preventing interconversion. LC-UV-laser polarimetric analysis identified peaks 1 and 2as a pair of enantiomers and peaks 3 and 4 as another. Thermodynamic analysis of the retention data indicatedthat the separation of the pairs of enantiomers is primarily enthalpy controlled as indicated by the positiveslope of the van't Huff plot. The difference in absolute Δ (Δ H), ranged from 2.20 kJ/mol to 2.42 kJ/mol.

11.
Mongolian Pharmacy and Pharmacology ; : 84-88, 2016.
Article in English | WPRIM | ID: wpr-631303

ABSTRACT

Introduction: High-performance liquid chromatography is one of the powerful qualitative and quantitative tech-niques, generally used for the analysis of pharmaceutical preparations. HPLC’s virtue lies in its versatility. We can use it to separate compounds of molecular weights from 54-450000Daltons. Amounts of material to be detected can vary from pictograms and nanograms to micrograms and milligrams to grams depends on which kind of detectors used for chromatographically separations. This article was prepared with an aim to review different aspects of HPLC, such as principle, types, and its applications. Keywords: High performance liquid chromatography, applications, mobile phase, stationary phase

12.
Braz. j. microbiol ; 46(3): 641-647, July-Sept. 2015. tab, ilus
Article in English | LILACS | ID: lil-755830

ABSTRACT

Dormancy models for Mycobacterium tuberculosis play important roles in understanding various aspects of tuberculosis pathogenesis and in the testing of novel therapeutic regimens. By simulating the latent tuberculosis infection, in which the bacteria exist in a non-replicative state, the models demonstrate reduced susceptibility to antimycobacterial agents. This minireview outlines the models available for simulating latent tuberculosis both in vitro and in several animal species. Additionally, this minireview discusses the advantages and disadvantages of these models for investigating the bacterial subpopulations and susceptibilities to sterilization by various antituberculosis drugs.

.


Subject(s)
Animals , Guinea Pigs , Mice , Rabbits , Antitubercular Agents/pharmacology , Disease Models, Animal , Latent Tuberculosis/pathology , Mycobacterium tuberculosis/growth & development , Tuberculosis, Pulmonary/pathology , Drug Resistance, Bacterial , Indicators and Reagents/pharmacology , Latent Tuberculosis/drug therapy , Latent Tuberculosis/microbiology , Macaca fascicularis , Mycobacterium tuberculosis/drug effects , Mycobacterium tuberculosis/metabolism , Oxazines/pharmacology , Tuberculosis, Pulmonary/drug therapy , Tuberculosis, Pulmonary/microbiology , Xanthenes/pharmacology , Zebrafish
13.
Chinese Pharmaceutical Journal ; (24): 2027-2030, 2014.
Article in Chinese | WPRIM | ID: wpr-860063

ABSTRACT

OBJECTIVE: To establish a fast and efficient HPLC method for the chiral separation of ondansetron hydrochloride and determination of the enantiomic impurity of (-)ondansetron(R)hydrochloride.

14.
Chinese Journal of Analytical Chemistry ; (12): 1002-1009, 2014.
Article in Chinese | WPRIM | ID: wpr-452469

ABSTRACT

A 6-azido-β-cyclodextrin was synthesized and derivatized with p-nitrophenyl isocyanate as chiral ligand. Following that the ligand was chemically bonded to mesoporous SBA-15 via a ‘Click Chemistry ’ reaction of the azido group with alkynyl group. A new p-nitrophenylcarbamoylatedβ-cyclodextrin bonded SBA-15 chiral stationary phase ( NPCSP ) for HPLC was obtained. The new stationary phase was first used to enantioseparate propranolol in human plasma under the polar organic solvent mode. The effects of methanol content , additive concentration of glacial acetic acid/triethylamine in mobile phase and the temperature on the enantioseparation were studied. The optimal chromatographic conditions were as follows: mobile phase was acetonitrile/methanol/glacial acetic acid/triethylamine (90:10:1. 25:2. 25, V/V), temperature 288 K, flow rate of 0. 5 mL/min, injection volume of 20 μL, detection wavelength at 290 nm. The resolution was 2. 04 with a short run time (< 15 min) under the above conditions. The composition of propranolol in plasma was quantitatively measured by HPLC-MS selected ion monitoring mode ( [ M +H ]+ m/z 260 . 10 ) with hydrochlorothiazide as internal standard. And linear range was 2. 5-250 μg/L and with a good linear relationship. The detection limit was 1 μg/L according to S/N=3. The experimental results showed that the chiral stationary phase exhibited excellent chiral separation ability to propranolol and the analysis method for propranolol in plasma was sensitive, accurate, simple and fast, which could be used for the determination of propranolol in plasma and pharmacokinetic studies.

15.
Chinese Journal of Information on Traditional Chinese Medicine ; (12): 17-21, 2014.
Article in Chinese | WPRIM | ID: wpr-444040

ABSTRACT

Objective To investigate the current situation of randomized controlled trials (RCTs) on the treatment of chronic obstructive pulmonary disease (COPD) in stationary phase with point application, and provide evidence for clinical practice. Methods Such databases as CNKI, VIP, and CBM were searched from the establishment date to October 2011 to collect the RCTs on the treatment of COPD in stationary phase with point application according to the predefined inclusion criteria. And the quality was assessed by using the Jadad scale, the revised CONSORT statement and other self-defined indexes. Results Among 32 included RCTs, 1 literature scored three points, 8 scored two points, 23 scored one point according to Jadad scale, and no RCT performed the allocation concealment. According to the CONSORT criteria, only one can be prompted randomized trials from the title of the article, 23 from abstracts, 2 literature showed how to determine the sample size, 7 described the method to generate random allocation sequence, only 1 literature mentioned blind method, 15 literature explicitly mentioned syndromes. Conclusion Currently, the methodology and reporting quality of studies on the treatment of COPD in stationary phase with point application are not good enough to provide reliable evidence for clinical practice, and we should improve the quality of our clinical research.

16.
Chinese Journal of Analytical Chemistry ; (12): 375-383, 2014.
Article in Chinese | WPRIM | ID: wpr-443775

ABSTRACT

An isatin derivative ofβ-cyclodextrin Schiff base was first synthesized by the condensation reaction between the carbonyl group of isatin and ethylenediamino group of the mono-substituted β-cyclodextrin. The Schiff base ligand was chemically linked to homemade ordered mesoporous SBA-15 silica gel via 3-( triethoxysilyl) propyl isocyanate coupling agent. In this way, a novel isatin derivative of β-cyclodextrin-bonded SBA-15 stationary phase ( ISCDP) was prepared for HPLC. Its chemical and physical parameters were characterized by infrared spectroscopy, mass spectroscopy, elemental analysis, thermogravimetric analysis, scanning electron microscopy, transmission electron microscopy, X-ray diffraction and BET specific surface area analysis. The basic chromatographic property of ISCDP was evaluated by using polar halogenated uracils and disubstituted benzene positional isomers as solute probes in reversed-phase chromatography. ISCDP was also used to enantioseparate twoβ-blocker drugs in polar organic mode and two dansyl amino acids in reversed-phase mode, respectively. The related chromatographic separation mechanism was also discussed. Above studies were expected to provide experimental basis for the practical application of ISCDP in the future. The results showed that the introduction of isatin indole ring could enhanced the reversed-phase chromatographic separation ability of ISCDP for halogenated uracils within 7 min. The new packing also exhibited high stereoselectivity for the position isomers of nitroaniline, aminophenol and benzenediol, in which the para isomers were finally eluted due to strong inclusion interaction between the isatin derivative of β-cyclodextrin ligand and the isomers. Meanwhile, the introduction of isatin indole ring could also improve the chiral separation ability of ISCDP. For example the fast enantioseparations of chiral β-adrenergic blockers and dansyl-amino acids on ISCDP were achieved within 20 min (Rs>1. 3). Obviously, besides hydrophobicity, various synergistic interactions could enhance the separation selectivities of the new stationary phase for chiral and achiral analytes, including dipole-dipole, hydrogen bonding,π-π and inclusion interactions. The ordered pore structure of SBA-15 facilitated to fast and efficient separation and analysis for drugs with good permeability and low mass transfer resistance.

17.
Journal of Pharmaceutical Analysis ; (6): 48-55, 2012.
Article in Chinese | WPRIM | ID: wpr-472262

ABSTRACT

The enantiomers separation of thirteen drugs collected in Ch.P2010 was performed on chiral stationary phase of cellulose ramification (chiralpak OD and chiralpak OJ) by high performance liquid chromatographic (HPLC) methods,which included ibuprofen (Cl),ketoprofen (C2),nitrendipine (C3),nimodipine (C4),felodipine (C5),omeprazole (C6),praziquantel (C7),propranolol hydrochloride (C8),atenolol (C9),sulpiride (C10),clenbuterol hydrochloride (C11),verapamil hydrochloride (C12),and chlorphenamine maleate (C13).The mobile phase consisted of isopropanol and n-hexane.The detection wavelength was set at 254 nm and the flow rate was 0.7 mL/min.The enantiomers separation of these thirteen racemates on chiralpak OD column and chiralpak OJ column was studied,while the effects of proportion of organic additives,alcohol displacer and temperature on the separation were studied.And the mechanism of some of racemates was discussed.The results indicated that thirteen chiral drugs could be separated on chiral stationary phase of cellulose ramification in normal phase chromatographic system.The chromatographic retention and resolution of enantiomers could be adjusted by factors including column temperature and the concentration of alcohol displacer and organic alkaline modifier in mobile phase.It was shown that the resolution was improved with reducing concentration of alcohol displacer.When concentration of organic alkaline modifier was 0.2% (v/v),the resolution and the peak shape were fairly good.Most racemates mentioned above had better resolution at column temperature of 25 ℃.When racemates were separated,the temperature should be kept so as to obtain stable separation results.

18.
Journal of China Pharmaceutical University ; (6): 151-155, 2010.
Article in Chinese | WPRIM | ID: wpr-480407

ABSTRACT

Novel aminopropyl-functionalized periodic mesoporous organosilicas (APMO) were successfully prepared by co-condensation of 1,2-bis (triethoxysilyl) ethane (BTSE) and 3-aminopropyltriethoxysilane (APTES) with the template of cationic surfactants cetyltrimethylammonium chlorine (C_(18)TAC) in basic medium.With the characterization measurements of powder X-ray diffraction (XRD),FT-IR and scanning electron microscopy (SEM) so on,APMO had such advantages as good monodisperse microshperes,uniformly orderd mesopore and large specific surface areas.These mesoporous materials were directly considered to be the chromatographic stationary phases and analyzed by HPLC evaluation.During the research,the as-prepared APMO column had better permeability and three polycyclic aromatic compounds realized separation.In addition,the as-prepared APMO column had certain advantages in fast analysis.

19.
Chinese Journal of Analytical Chemistry ; (12): 158-162, 2010.
Article in Chinese | WPRIM | ID: wpr-403825

ABSTRACT

A method for the rapid enantioseparation of five β-blocker drugs, including alprenolol, propranolol), mexiletine, metoprolol and pindolol was developed by a 5-cm short column packed with perphenylcarbamoylated β-cyclodextrin(CD) chiral stationary phase by HPLC. The results showed that except for alprenolol), the other 4 β-blocker drugs were completely separated using ACN-0.1% thriethylammonium acetate(TEAA), 40∶ 60, V/V, pH=4.0) as mobile phase. The 5-cm short CD-based column exhibited rapid separation ability to the above β-blocker drugs within 5 min, which indicated that the separation has high efficiency. According to the chemical structures of the β-blockers and their chromatographic behavior, related separation mechanisms were also discussed. The proposed method was rapid, effective and repeated.

20.
China Pharmacy ; (12)2007.
Article in Chinese | WPRIM | ID: wpr-533062

ABSTRACT

OBJECTIVE:To establish a HPLC-chiral stationary phase(CSP) for separating the enantiomers of lactic acid and determining the optical purity of lactic acid.METHODS:Lactic acid samples of different optical purity were determined by HPLC-CSP vs.optical rotation method.The enantiomers of lactic acid were separated on Chirex 3126(D)-penicillamine chiral column.The mobile phase consisted of copper sulfate solution-isopropyl alcohol (85∶15) at a flow rate of 0.6 mL?min-1.The detection wavelength was set at 254 nm.RESULTS:A baseline separation of the enantiomers of lactic acid was achieved with a separation factor of greater than 1.2.The calibration curve was linear in the range of 0.75~48.24 mg?mL-1 (r=0.999 3),RSD=1.21%.The determination results determined by HPLC-CSP were similar to those determined by optical rotation method.CONCLUSION:The established method is simple,reliable in results and reproducible,and it is applicable for the separation of the enantiomers of lactic acid and determination of the optical purity of lactic acid.

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