Journal of Liquid Chromatography &amp Related Technologies (J Liq Chrom Relat Tech)

Publications in this journal

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  Available from: ysu.edu

  Article: Ionic liquids in chromatography and capillary electrophoresis

  A M Stalcup, B Cabovska
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  ABSTRACT: One of the major challenges facing the chemical industry is the development of new, "green" technologies which reduce the environmental impact of manufacturing processes. Ionic liquids are emerging as a promising alternative to traditional organic solvents and are, thus, gener-ating considerable interest in a variety of areas. This review examines some of the unique properties of ionic liquids and their applications in analytical separations.
  Journal of Liquid Chromatography &amp Related Technologies ; 27:1082-6076.
• Article: RAPID AND SENSITIVE LIQUID CHROMATOGRAPHIC METHOD FOR DETERMINATION OF ETOPOSIDE IN PLASMA AND BIOLOGICAL SAMPLES

  Abida Raza, Akhtar Aman, Shumaila Bashir, Bashir Ahmad, Javaid Irfan, J. Dev Mehta, Hardyal S. Gill, Abad Khan, Mehboob Alam, Andreas G. Schätzlein
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  ABSTRACT: A simple, easy, fast, inexpensive and sensitive reversed phase HPLC method is developed for quantification of etoposide in plasma and biological samples. Separations are carried out using mobile phase consisting of acetonitrile and water (35:65, v/v) on phoenix C18 chromolith reverse phase analytical column protected by Phenomenex guard cartridge. Etoposide and teniposide (internal standard) are extracted from tissue samples with acetonitrile and chloroform. The eluent is monitored at 254 nm at the temperature of 45° C. The developed method exhibited linearity over an analytical range of the respective samples. Run time is only five minute using flow rate of 1.5 mL/minute with great precision and reproducibility. The peak-height ratio of etoposide with respect to internal standard is linear corresponding to its plasma concentration. The method was reliable as both intra-day and inter-day coefficient of variation was below 5%. It is observed that this method is sensitive and reliable. The described method will be applied toward etoposide pharmacokinetic and compartmental studies in mice.
  Journal of Liquid Chromatography &amp Related Technologies 02/2013;
• Article: Stability-Indicating Micellar Electrokinetic Chromatography Method for Determination of Finasteride in Pharmaceutical Preparations

  M. Gökhan ÇAĞLAYAN, İsmail Murat PALABIYIK, Feyyaz ONUR
  Journal of Liquid Chromatography &amp Related Technologies 02/2013; 36(6):781-791.
• Article: QUANTITATIVE ESTIMATION OF LUPEOL AND STIGMASTEROL IN COSTUS IGNEUS BY HIGH-PERFORMANCE THIN-LAYER CHROMATOGRAPHY

  K. Manjula a, K. Rajendran a, T. Eevera b & S. Kumaran a
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  ABSTRACT: In this article, simultaneous quantitative estimation of two biologically active triterpenoid compound Lupeol and a steroid compound, Stigmasterol, in Costus igneus stems was performed using high-performance thin-layer chromatography (HPTLC). TLC aluminum plates precoated with silica-gel 60 F254(20 cm�10 cm) were used with a mobile phase of n-Hexane: Ethyl acetate (80:20v=v) for lupeol, Toluene: Acetone: Acetic acid (8.9: 0.9: 0.2 v=v=v) for stigmasterol and densitometric determination of these compounds was carried out at 366 nm in reflectance=absorbance mode. The linear regression data for the calibration plots showed a good linear relationship with r¼0.99794 and r¼0.99291 for Lupeol and Stigmasterol, respectively. A recovery study was carried out to check the accuracy of the method. The average recovery of Lupeol and Stigmasterol was 100.16% and 99.94%, respectively. According to International Conference on Harmonization (ICH) guidelines, the method was validated for linearity, precision, accuracy, and recovery, limit of detection, limit of quantification, specificity, robustness, and ruggedness. The HPTLC method was found to be reproducible, accurate, and precise and could detect these two compounds at nanogram level from the stem of Costus igneus.
  Journal of Liquid Chromatography &amp Related Technologies 01/2013; 36:,:197–212.
• Article: Separation and Statistical Data Processing of Different Batches of Aerial Parts of Jologbo

  J. Boima Kiazolu, Lingyi Zhang, Azeem Intisar, Yun Wang, Runsheng Zhang, Zhongping Wu, Weibing Zhang
  Journal of Liquid Chromatography &amp Related Technologies 01/2013;
• Article: NEW GENERATION HALO COLUMN FOR FAST ANALYSES OF ASPIRIN AND ATORVASTATIN IN PHARMACEUTICAL PREPARATION.

  Imran Ali, Kishwar Saleem, Ashanul Haque, Waseem A. Wani, and Vinay D. Gaitode
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  ABSTRACT: A super-fast (within 4 min only) HPLC method is described for the analyses of aspirin and atorvastatin simultaneously in single dosage formulation. The mobile phase used was water (pH 2.0, adjusted by o-phosphoric acid)-acetonitrile (50:50, v=v) at 1.0mL=min flow rate with 210 nm detection. The column used was new generation Halo C18(100�46 mm; shell particles; 2.7 lm). The capacity factors of aspirin and atorvastatin were 1.20 and 2.01, while the separation and resolution factors were 1.68 and 5.63, respectively. The values of LOD and LOQ for aspirin were 0.10 and 0.50 lg=mL, while these values for atorvastatin were 0.50 and 2.5 lg=mL, respectively. The linearity was observed in the ranges of 0.1 to 5.0 mg=mL for both drugs. The reported method can be used for the quality control of aspirin and atorvastatin in pharmaceutical preparations with good economy. Additionally, this method can also be used for the analyses of aspirin and atorvastatin drugs in biological and environmental samples.
  Journal of Liquid Chromatography &amp Related Technologies 01/2013; 36:261–273.
• Article: DETERMINATION OF LAMOTRIGINE IN TABLETS USING HPTLC, HPLC, AND DERIVATIVE SPECTROPHOTOMETRY METHODS

  Marcin Koba, Michał Piotr Marszałł, Wiktor Sroka, Monika Tłuchowska, Tomasz Ba˛ czek
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  ABSTRACT: The determination of lamotrigine in tablets using high-performance thin-layer chromatography (HPTLC), high-performance liquid chromatography (HPLC), as well as direct, first, second, and third derivative ultraviolet spectrophotometry methods are described. HPTLC method was performed using silica plates, a mobile phase composed of toluene:acetone:ammonia (3:7:0.5, v=v=v), and a densitometric detection at 312 nm. Moreover, quantification was achieved in the concentration range of 0.25–10.0 lg=spot and with good precision (RSD¼2.19%) and recovery (97.92%), using a nonlinear calibration curve by fitting to y¼aþblnx. HPLC method was performed using a Luna C18 column and isocratic elution mode with a mobile phase composed of methanol: phosphate buffer (25:75, v=v) and delivered at a flow rate 1.2mL=min. Proposed HPLC method provided good results of precision (RSD¼1.86%) and recovery (101.51%) in the concentration range of 0.25–7.5 lg=mL using linear y¼aþbx regression analysis. For the UV-derivative spectrophotometry method, all derivatives and wavelengths studied proved accurate linearity, precision (RSD¼0.96–1.87%), and recovery (96.74–101.90%). Moreover, no interference was found from tablet excipients at the selected wavelength and assay procedures. The developed methods were found to be validated and showed good precision and reproducibility.
  Journal of Liquid Chromatography &amp Related Technologies 01/2013; 36:537-548.
• Article: Optimization of enantioseparation of 2,6-diketopiperazine derivatives with beta-cyclodextrin and hydroxy acids as components of mobile phase in liquid chromatography

  Kamila Szwed, Monika Asztemborska, Maciej Dawidowski
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  ABSTRACT: A novel method for a direct separation of the enantiomers of 2,6-diketopiperazine derivatives was devised. The enantiomers were separated by means of chromatography on reversed-phase (RP-HPLC) column with (-cyclodextrin as a chiral mobile phase additive and hydroxy acids as solubility enhancers. The effect of β-cyclodextrin concentration, hydroxy acids type on retention and enantioseparation were investigated. It was found that the systems with high concentrations of β-cyclodextrin in the presence of hydroxy acids, especially DL-tartaric acid, improve enantioselectivity, while the presence of citric acid aggravates it.
  Journal of Liquid Chromatography &amp Related Technologies 01/2013;
• Article: High-performance liquid chromatography with ultraviolet detection and protein precipitation as a way of quantitative determination of nilotinib with and without internal standard

  Marek Dziadosz, Marie-Christine Wagner, Daniel B. Lipka, Thomas Fischer, Heidemarie Bartels
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  ABSTRACT: A simple, fast, and effective HPLC-DAD method for the quantification of nilotinib in blood serum with and without dasatinib as the internal standard was developed and presented in this work. A simple protein precipitation extraction method leads to satisfactory recoveries, accuracies, and coefficients of variation as 83.9–96.8%, 95.8–105.1%, and 2.1–6.1%, respectively. A Marcherey-Nagel Lichrospher 100-5 RP8 250 × 4 mm column held at 40°C, a mobile phase of 0.05 M H3PO4/KH2PO4-acetonitrile (7:3, v/v) at a flow rate of 1 mL/min, and a diode array detector operated at a wavelength of 265 nm were used for the analysis of 50 µL prepared sample injected into the HPLC. A single run was completed in 20 min. The presented method has a limit of quantification of 0.20 µM and is linear between 0.20 and 10 µM. The possibility of its use for the nilotinib analysis without an internal standard is also discussed.
  Journal of Liquid Chromatography &amp Related Technologies 10/2012; 35(17):2503-2510.
• Article: Simultaneous analysis of vitamin C and aspirin in aspirin C effervescent tablets by high performance liquid chromatography-photodiode array detector

  Mohammad Rizwan Khan, Zeid Abdullah Alothman, Mu. Naushad, Ayman Abdul Ghfar & Saikh Mohammad Wabaidur
  Journal of Liquid Chromatography &amp Related Technologies 10/2012; 35(17):2012.
• Article: SEPARATION AND ESTIMATION OF PROCESS RELATED IMPURITIES AND DEGRADATION PRODUCTS OF LEVETIRACETAM IN SOLID PHARMACEUTICAL FORMULATION USING ION-PAIR CHROMATOGRAPHY

  Navneet Kumar, D. Sangeetha
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  ABSTRACT: A stability-indicating ion-pair chromatographic method has been developed and validated for the simultaneous estimation of impurities and forced degradation products of levetiracetam in tablet formulation. The chromatographic separation was achieved on ACE C8 (150 mm x 4.6 mm I.D., 5 µm) column at 25°C with UV detection at 200 nm using isocratic mobile phase at a flow rate of 0.9 mL/min. Mobile phase contains a mixture of buffer (50 mM sodium di-hydrogen orthophosphate and 1.25 mM sodium 1-octanesulfonate monohydrate, pH adjusted to 2.6 with ortho-phosphoric acid) and acetonitrile in the ratio of 95:5 (v/v), respectively. The drug product was exposed to the stress conditions of oxidative, hydrolysis (acid and base), hydrolytic, thermal and photolytic degradation. Significant degradation was observed during acid, base hydrolysis and oxidative stress conditions. The degradation products were well resolved from main peak and its impurities; and peak purity for the levetiracetam peak was passed in all stress samples. The mass balance was found to be in the range of 98.1-101.7% in all the stressed conditions, thus proved the stability-indicating power of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision and robustness.
  Journal of Liquid Chromatography &amp Related Technologies 09/2012;
• Article: Simultaneous Determination of Paracetamol, Caffeine, Domperidone, Ergotamine tartrate, Propyphenazone and Drotaverine HCl by HPLC

  Yousry M. Issa, Mohamed E.M. Hassoun, AShraf G. Zayed
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  ABSTRACT: A high performance liquid chromatographic (HPLC) method was developed for the simultaneous determination of paracetamol, (acetaminophen), caffeine, domperidone, ergotamine tartrate, ropyphenazone, and drotaverine HCl. The chromatography was performed in the isocratic mode on a Hypersil C18 BDS column using a mobile phase consisting of 0.02 mole L �1 tetrabutylammonium bisulphate and methanol (100:45, v=v) at 50�C using UV detection at 210nm. The method was validated by specificity, linearity, limit of detection, and limit of quantification, accuracy, and precision for the aforementioned drugs. The time required for a single analysis amounts to 14 min. The response was linear for the drug concentration ranges of 6.20–420.00, 0.80–80.00, 0.80–64.00, 2–40.00, 1.20–240.00, and 3.20–64.00, lgmL �1 for PA, CA, DO, ET, PP, and DH, respectively. Accuracy values for the method ranged from 99.40–101.94, 98.48–101.13, 98.97–100.54, 96.47–102.43, 98.92–101.82, and 97.63–100.45% for PA, CA, DO, ET, PP, and DH, respectively.
  Journal of Liquid Chromatography &amp Related Technologies 09/2012; 35(15-1082-6076):2148-2161.
• Article: A LIQUID CHROMATOGRAPHY MASS SPECTROMETRY METHODFOR THE DETERMINATION OF SOME PHARMACOLOGICALLYACTIVE SUBSTANCES VALIDATED USING MILK AS A MATRIX

  Rose Kibechu, Kwenga Sichilongo
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  ABSTRACT: Two QuEChERS kits originally designed for the extraction of pesticides in foods and foods of plant origin have been compared for the extraction efficiency of different analytes other than pesticides. Six veterinary drugs that have been prohibited for use in foods of animal origin were studied using milk as a matrix and LC-MS as a separation and detection mode. The Association of Official Analytical Chemists (AOAC) and the European Standard EN QuEChERS kits were compared after optimization of key parameters for extraction of chloramphenicol, metronidazole, chlorpromazine, dimetridazole, ronidazole, and dapsone. The EN QuEChERS kit was superior over the AOAC kit in terms of recoveries:(in brackets are% recoveries) chloramphenicol (79), metronidazole (55), chlorpromazine (93), dimetridazole (97), ronidazole (65), and dapsone (69). Using the AOAC kit gave the following values: (in brackets are% recoveries) chloramphenicol (71), metronidazole (66), chlorpromazine (60), dimetridazole (49), ronidazole (37), and dapsone (33). Additionally, three mass spectrometry scan modes, that is, full scan, SIM, and MS=MS were compared. Results showed that SIM was superior over full scan and MS=MS as in the case of chloramphenicol whose method detection limit (MDL) value was 16.3lg=kg in the SIM mode and 28.2lg=kg in the full scan mode.
  Journal of Liquid Chromatography &amp Related Technologies 07/2012; 35(12):1697-1711.
• Article: SEPARATION DIFFERENCES AMONG PHENYL HYDRIDE, UDC CHOLESTEROL AND BIDENTATE C8 STATIONARY PHASES FOR STABILITY INDICATING METHODS OF TETRACYCLINES

  Joshua E. Young, Maria T. Matyska, Anil K. Azad, Sergio E. Yoc, Joseph J. Pesek
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  ABSTRACT: Formulation extracts of tetracycline hydrochloride (HCl), minocycline hydrochloride (HCl), and doxycycline hyclate were degraded by strong acidic conditions and heating. Subsequently, components of the extracts were separated by Bidentate C8, Phenyl Hydride and Cholesterol (UDC) HPLC columns operating in the reverse phase mode. The Phenyl Hydride column was able to baseline separate minocycline from the observed degradant, while partial or total co-elution was observed with the other two columns using otherwise identical method conditions. For both the degraded tetracycline HCl and doxycycline hyclate extracts, the UDC column gave the best resolution for the critical pair. The findings suggest that the postulated secondary retention mechanisms of π–π interactions from the Phenyl Hydride and shape selectivity from the UDC can provide superior resolution for structurally similar analytes compared to hydrophobic interactions alone.
  Journal of Liquid Chromatography &amp Related Technologies 06/2012;
• Article: FAST ANALYSIS AND VALIDATION OF RUTIN IN ANTI-PSORIATIC AYURVEDIC FORMULATION BY HPLC

  S. Mohamed Musthaba, M. T. Athar, Kamal YT, Sanjula Baboota, Javed Ali, Sayeed Ahmad
  Journal of Liquid Chromatography &amp Related Technologies 04/2012;
• Article: DEVELOPMENT AND VALIDATION OF A STABILITY INDICATING RPLC METHOD FOR THE ESTIMATION OF PROCESS RELATED IMPURITIES AND DEGRADATION PRODUCTS OF DULOXETINE HYDROCHLORIDE AND PHTHALIC ACID IN DULOXETINE HYDROCHLORIDE DELAYED RELEASE CAPSULES

  Navneet Kumar, D. Sangeetha, Bhupendrasinh Vaghela, P. Sunil Reddy, Anuj Raghav
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  ABSTRACT: A stability-indicating gradient reverse phase liquid chromatographic method was developed for the quantitative determination of process related impurities and forced degradation products of duloxetine hydrochloride, duloxetine phthalamide impurity, and phthalic acid in duloxetine hydrochloride delayed release capsules. The method was developed by using Inertsil ODS-4 (150mm� 4.6 mm) 3 lm column with mobile phase containing a gradient mixture of solvent A (0.02M ammonium dihydrogen phosphate and 0.01M 1-octane sulfonate sodium salt, pH adjusted to 2.5 with orthophosphoric acid) and B (750:300mL mixture of acetonitrile and methanol). The flow rate of the mobile phase was 1.8mL=min with column temperature of 50�C and detection wavelength at 230 nm. Duloxetine hydrochloride was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal, and photolytic degradation. Duloxetine hydrochloride was found to degrade significantly in acid, base and oxidative stress conditions. The degradation products were well resolved from phthalic acid, duloxetine and its impurities. The mass balance was found to be in the range of 95–105% in all the stressed conditions, thus proved the stability-indicating power of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision and robustness.
  Journal of Liquid Chromatography &amp Related Technologies 04/2012; 35(7):867-881.
• Article: Effect of Mobile Phase Composition and pH on HPLC Separation of Rhizome of Polygonum bistorta

  Azeem Intisar, J. Boima Kiazolu, Yun Wang, Lingyi Zhang, Weibing Zhang
  Journal of Liquid Chromatography &amp Related Technologies 04/2012; 35(7):977-987.