Sample records for stability indicating rp-hplc

  1. Rapid Analysis of Glibenclamide Using an Environmentally Benign Stability-Indicating RP-HPLC Method

    PubMed Central

    Haq, Nazrul; Alanazi, Fars Kaed; Alsarra, Ibrahim Abdullah; Shakeel, Faiyaz

    2014-01-01

    An environmentally benign RP-HPLC approach for rapid analysis of glibenclamide in pure form, developed nanoemulsion and commercial tablets was developed and validated in present investigation. The green chromatographic identification was performed on Lichrosphere 250 X 4.0 mm RP C8 column having a 5 ?m packing as a stationary phase using a combination of ethanol: methanol (50:50 % v/v) as a mobile phase, at a flow rate of 1.0 mL/min with UV detection at 245 nm. The proposed method was validated for linearity, selectivity, accuracy, precision, robustness, sensitivity and specificity as per international conference on harmonization (ICH) guidelines. The utility of proposed method was verified by assay of glibenclamide in developed nanoemulsion and commercial tablets. The proposed method was found to be satisfactory in terms of selectivity, precision, accuracy, robustness, sensitivity and specificity. The content of glibenclamide in developed nanoemulsion and commercial tablets was found to be 100.50 % and 99.15 % respectively. The proposed method successfully resoled glibenclamide peak in the presence of its all type of degradation products which indicated stability-indicating property of the proposed method. These results indicated that the green chromatographic method could be successfully employed for routine analysis of glibenclamide in pure drug and various commercial formulations. PMID:25276186

  2. Rapid Analysis of Glibenclamide Using an Environmentally Benign Stability-Indicating RP-HPLC Method.

    PubMed

    Haq, Nazrul; Alanazi, Fars Kaed; Alsarra, Ibrahim Abdullah; Shakeel, Faiyaz

    2014-01-01

    An environmentally benign RP-HPLC approach for rapid analysis of glibenclamide in pure form, developed nanoemulsion and commercial tablets was developed and validated in present investigation. The green chromatographic identification was performed on Lichrosphere 250 X 4.0 mm RP C8 column having a 5 ?m packing as a stationary phase using a combination of ethanol: methanol (50:50 % v/v) as a mobile phase, at a flow rate of 1.0 mL/min with UV detection at 245 nm. The proposed method was validated for linearity, selectivity, accuracy, precision, robustness, sensitivity and specificity as per international conference on harmonization (ICH) guidelines. The utility of proposed method was verified by assay of glibenclamide in developed nanoemulsion and commercial tablets. The proposed method was found to be satisfactory in terms of selectivity, precision, accuracy, robustness, sensitivity and specificity. The content of glibenclamide in developed nanoemulsion and commercial tablets was found to be 100.50 % and 99.15 % respectively. The proposed method successfully resoled glibenclamide peak in the presence of its all type of degradation products which indicated stability-indicating property of the proposed method. These results indicated that the green chromatographic method could be successfully employed for routine analysis of glibenclamide in pure drug and various commercial formulations. PMID:25276186

  3. Stability-Indicating RP-HPLC Method for Simultaneous Estimation of Enrofloxacin and Its Degradation Products in Tablet Dosage Forms

    PubMed Central

    Chakravarthy, V. Ashok; Sailaja, B. B. V.; Kumar, Avvaru Praveen

    2015-01-01

    The present work was the development of a simple, efficient, and reproducible stability-indicating reverse-phase high performance liquid chromatographic (RP-HPLC) method for simultaneous determination enrofloxacin (EFX) and its degradation products including ethylenediamine impurity, desfluoro impurity, ciprofloxacin impurity, chloro impurity, fluoroquinolonic acid impurity, and decarboxylated impurity in tablet dosage forms. The separation of EFX and its degradation products in tablets was carried out on Kromasil C-18 (250 × 4.6?mm, 5??m) column using 0.1% (v/v) TEA in 10?mM KH2PO4 (pH 2.5) buffer and methanol by linear gradient program. Flow rate was 1.0?mL?min?1 with a column temperature of 35°C and detection wavelength was carried out at 278?nm and 254?nm. The forced degradation studies were performed on EFX tablets under acidic, basic, oxidation, thermal, humidity, and photolytic conditions. The degraded products were well resolved from the main active drug and also from known impurities within 65 minutes. The method was validated in terms of specificity, linearity, LOD, LOQ, accuracy, precision, and robustness as per ICH guidelines. The results obtained from the validation experiments prove that the developed method is a stability-indicating method and suitable for routine analysis. PMID:25705547

  4. Stability-indicating RP-HPLC method for the simultaneous determination of escitalopram oxalate and clonazepam.

    PubMed

    Kakde, Rajendra B; Satone, Dinesh D; Gadapayale, Kamalesh K; Kakde, Megha G

    2013-07-01

    The objective of the current study was to develop a validated, specific stability-indicating reversed-phase liquid chromatographic (LC) method for the quantitative determination of escitalopram oxalate and clonazepam and their related substances in bulk drugs and pharmaceutical dosage forms in the presence of degradation products. Forced degradation studies were performed on the pure drugs of escitalopram oxalate and clonazepam, as per the stress conditions prescribed by the International Conference on Harmonization (ICH) using acid, base, oxidation, thermal stress and photolytic degradation to show the stability-indicating power of the method. Significant degradation was observed during acid and alkaline hydrolysis and no degradation was observed in other stress conditions. The chromatographic method was optimized using the samples generated from forced degradation studies. Good resolution between the peaks corresponded to the active pharmaceutical ingredients, escitalopram oxalate and clonazepam, and degradation products from the analyte were achieved on an ODS Hypersil C18 column (250 × 4.6 mm) using a mobile phase consisting of a mixture of acetonitrile-50 mM phosphate buffer + 10 mM triethylamine (70:30, v/v). The detection was conducted at 268 nm. The limit of detection and the limit of quantitation for escitalopram oxalate and clonazepam were established. The stress test solutions were assayed against the qualified working standards of escitalopram oxalate and clonazepam, which indicated that the developed LC method was stability-indicating. Validation of the developed LC method was conducted as per ICH requirements. The developed LC method was found to be suitable to check the quality of bulk samples of escitalopram oxalate and clonazepam. PMID:23135233

  5. Stability Indicating RP-HPLC Estimation of Nebivolol Hydrochloride in Pharmaceutical Formulations.

    PubMed

    Shah, D A; Bhatt, K K; Mehta, R S; Baldania, S L; Gandhi, T R

    2008-09-01

    A simple, specific, accurate and stability indicating reversed phase liquid chromatographic method was developed for the determination of nebivolol hydrochloride in tablet dosage forms. A phenomenex Gemini C-18, 5 ?m column having 250×4.6 mm i.d., with mobile phase containing methanol: acetonitrile: 0.02 M potassium dihydrogen phosphate (60:30:10, v/v/v; pH 4.0) was used. The retention time of nebivolol hydrochloride was 2.6 min. The linearity for nebivolol hydrochloride was in the range of 0.2-10 ?g/ml. The recovery was found to be in the range of 98.68-100.86%. The detection limit and quantification limit were found to be 0.06 ?g/ml and 0.2 ?g/ml, respectively. Nebivolol stock solutions were subjected to acid, alkali and neutral hydrolysis, chemical oxidation and dry heat degradation. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time values. The proposed method was validated and successfully applied to the estimation of nebivolol hydrochloride in tablet formulations. PMID:21394254

  6. Stability Indicating RP-HPLC Estimation of Nebivolol Hydrochloride in Pharmaceutical Formulations

    PubMed Central

    Shah, D. A.; Bhatt, K. K.; Mehta, R. S.; Baldania, S. L.; Gandhi, T. R.

    2008-01-01

    A simple, specific, accurate and stability indicating reversed phase liquid chromatographic method was developed for the determination of nebivolol hydrochloride in tablet dosage forms. A phenomenex Gemini C-18, 5 ?m column having 250×4.6 mm i.d., with mobile phase containing methanol: acetonitrile: 0.02 M potassium dihydrogen phosphate (60:30:10, v/v/v; pH 4.0) was used. The retention time of nebivolol hydrochloride was 2.6 min. The linearity for nebivolol hydrochloride was in the range of 0.2-10 ?g/ml. The recovery was found to be in the range of 98.68-100.86%. The detection limit and quantification limit were found to be 0.06 ?g/ml and 0.2 ?g/ml, respectively. Nebivolol stock solutions were subjected to acid, alkali and neutral hydrolysis, chemical oxidation and dry heat degradation. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time values. The proposed method was validated and successfully applied to the estimation of nebivolol hydrochloride in tablet formulations. PMID:21394254

  7. Development and Validation of a Novel Stability-Indicating RP-HPLC Method for the Simultaneous Determination of Halometasone, Fusidic Acid, Methylparaben, and Propylparaben in Topical Pharmaceutical Formulation

    PubMed Central

    Goswami, Nishant; Gupta, V. Rama Mohan; Jogia, Hitesh A.

    2013-01-01

    A stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for the simultaneous determination of halometasone, fusidic acid, methylparaben, and propylparaben in topical pharmaceutical formulation. The desired chromatographic separation was achieved on an Agilent Zorbax CN (Cyano), 5 ?m (250 × 4.6 mm) column using gradient elution at 240 nm detector wavelength. The optimized mobile phase consisted of a mixture of 0.01 M phosphate buffer and 0.1% orthophosphoric acid, pH-adjusted to 2.5 with an ammonia solution as solvent-A and acetonitrile as solvent-B. The developed method separated halometasone, fusidic acid, methylparaben, and propylparaben in the presence of known impurities/degradation products. The stability-indicating capability was established by forced degradation experiments and separation of known and unknown degradation products. The developed RP-HPLC method was validated according to the International Conference on Harmonization (ICH) guidelines. This validated method was applied for the simultaneous estimation of HM, FA, MP, and PP in commercially available cream samples. Further, the method can be extended for the estimation of HM, FA, MP, and PP in various commercially available dosage forms. PMID:23833716

  8. Development of a Stability-Indicating RP-HPLC Method for the Determination of Rupatadine and its Degradation Products in Solid Oral Dosage Form

    PubMed Central

    Trivedi, Harshal Kanubhai; Patel, Mukesh C.

    2012-01-01

    A simple, sensitive, and reproducible reversed-phase high-performance liquid chromatography (RP-HPLC) method, coupled with a photodiode array detector, was developed for the determination of rupatadine (RUPA) and its related substances in pharmaceutical dosage forms. Chromatographic separation was achieved on the Hypersil BDS (150 x 4.6 mm, 5 ?m) column with a mobile phase containing a gradient mixture of a buffer (acetate buffer pH-6.0) and solvent (methanol). The eluted compounds were monitored at 264 nm for the related substances and assay, the flow rate was 1.0 mL/min, and the column oven temperature was maintained at 50°C. The developed method separated RUPA from its four known and three unknown impurities within 15.0 min. Rupatadine was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal, and photolytic degradation. Rupatadine was found to degrade significantly under oxidative stress conditions, and degrade slightly under acid, base, hydrolytic, thermal, and photolytic stress conditions. All impurities were well-resolved from each other and from the main peak, showing the stability-indicating power of the method. The developed method was validated as per the International Conference on Harmonization (ICH) guidelines. The developed and validated RP-HPLC method is LC-MS compatible and can be explored for the identification of eluted unknown impurities of RUPA. PMID:23264938

  9. A validated specific stability-indicating RP-HPLC assay method for Ambrisentan and its related substances.

    PubMed

    Narayana, M B V; Chandrasekhar, K B; Rao, B M

    2014-09-01

    A validated specific stability-indicating reverse-phase liquid chromatographic method was developed for the quantitative determination of Ambrisentan as well as its related substances in bulk samples, pharmaceutical dosage forms in the presence of degradation products and its related impurities. Forced degradation studies were performed on bulk samples of Ambrisentan as per the ICH-prescribed stress conditions using acid, base, oxidative, thermal stress and photolytic degradation to show the stability-indicating power of the LC method. Significant degradation in acidic, basic stress conditions was observed and no degradation was observed in other stress conditions. The chromatographic method was optimized using the samples generated from the forced degradation studies and the impurity-spiked solution. Good resolution between the peaks corresponds to Ambrisentan-related impurities and degradation products from the analyte were achieved on a SunFire C18 column using a mobile phase consisting of a mixture of potassium dihydrogen orthophosphate at a pH adjusted to 2.5 with ortho-phosphoric acid in water and a mixture of acetonitrile:methanol using a simple linear gradient. The detection was carried out at 225 nm. The limit of detection and the limit of quantification for the Ambrisentan and its related impurities were established. The stressed test solutions were assayed against the qualified working standard of Ambrisentan and the mass balance in each case was between 98.9 and 100.3%, indicating that the developed LC method was stability indicating. Validation of the developed LC method was carried out as per the ICH requirements. The developed method was found to be suitable to check the quality of bulk samples of Ambrisentan at the time of batch release and also during its storage (long-term and accelerated stability). PMID:23926121

  10. Development and validation of a stability-indicating RP-HPLC method for assay of betamethasone and estimation of its related compounds.

    PubMed

    Fu, Qiang; Shou, Minshan; Chien, Dwight; Markovich, Robert; Rustum, Abu M

    2010-02-01

    Betamethasone (9alpha-fluoro-16beta-methylprednisolone) is one of the members of the corticosteriod family of active pharmaceutical ingredient (API), which is widely used as an anti-inflammatory agent and also as a starting material to manufacture various esters of betamethasone. A stability-indicating reverse-phase high performance liquid chromatography (RP-HPLC) method has been developed and validated which can separate and accurately quantitate low levels of 26 betamethasone related compounds. The stability-indicating capability of the method was demonstrated through adequate separation of all potential betamethasone related compounds from betamethasone and also from each other that are present in aged and stress degraded betamethasone stability samples. Chromatographic separation of betamethasone and its related compounds was achieved by using a gradient elution at a flow rate of 1.0mL/min on a ACE 3 C18 column (150mmx4.6mm, 3microm particle size, 100A pore size) at 40 degrees C. Mobile phase A of the gradient was 0.1% methanesulfonic acid in aqueous solution and mobile phase B was a mixture of tert-butanol and 1,4-dioxane (7:93, v/v). UV detection at 254nm was employed to monitor the analytes. For betamethasone 21-aldehyde, the QL and DL were 0.02% and 0.01% respectively. For betamethasone and the rest of the betamethasone related compounds, the QL and DL were 0.05% and 0.02%. The precision of betamethasone assay is 0.6% and the accuracy of betamethasone assay ranged from 98.1% to 99.9%. PMID:19846264

  11. Development and Validation of a Stability-Indicating RP-HPLC Method for the Estimation of Drotaverine Impurities in API and Pharmaceutical Formulation.

    PubMed

    Thummala, Veera Raghava Raju; Tharlapu, Satya Sankarsana Jagan Mohan; Rekulapalli, Vijay Kumar; Ivaturi, Mrutyunjaya Rao; Nittala, Someswara Rao

    2014-03-01

    A sensitive, stability-indicating gradient RP-HPLC method with PDA detection has been developed for the simultaneous analysis of drotaverine impurities in active pharmaceutical ingredient (API) and pharmaceutical formulations. Efficient chromatographic separation was achieved on an XTerra RP18, 150 × 4.6 mm, 5 ?m column using gradient elution at 230 nm detection wavelength. The optimized mobile phase consisted of a 0.02 M potassium dihydrogen orthophosphate buffer of pH 3.0 as solvent A and acetonitrile as solvent B. The flow rate of the mobile phase was 1.0 mL min(-1) with a column temperature of 25°C. The method showed linearity over the range of 0.251-10.033 ?g/mL, 0.231-9.995 ?g/mL, 0.230-10.089 ?g/mL, 0.334-10.011 ?g/mL, and 0.324-10.050 ?g/mL for impurities 1, 2, 3, 4, and drotaverine, respectively, with a correlation coefficient greater than 0.999. The relative retention times and relative response factors of impurities 1, 2, 3, 4 were 0.36, 0.90, 1.42, 1.55 and 1.04, 0.84, 1.10, 1.30, respectively. The drotaverine formulation sample was subjected to the stress conditions of acid, base, oxidative, thermal, humidity, and photolytic degradation. Drotaverine was found to degrade significantly in peroxide, base, and heat stress conditions. The degradation products were well-resolved from drotaverine and its impurities. The peak purity test results confirmed that the drotaverine peak was homogenous and pure in all stress samples and the mass balance was found to be more than 98%, thus proving the stability-indicating power of the method. The developed method was validated according to ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, and robustness. PMID:24634845

  12. Development and validation of a stability indicating RP-HPLC method for the simultaneous determination of related substances of albuterol sulfate and ipratropium bromide in nasal solution.

    PubMed

    Kasawar, Gajanan B; Farooqui, Mazahar

    2010-05-01

    A simple, sensitive and specific RP-HPLC method was developed for the quantification of related impurities of albuterol sulfate (AS) and ipratropium bromide (IB) in liquid pharmaceutical dosage form. The chromatographic separation employs gradient elution using an inertsil C8-3, 250mmx4.6mm, 5mum columns. Mobile phase consisting of solvent A (solution containing 2.5g of potassium dihydrogen phosphate and 2.87g of heptane-1-sulfonic acid sodium salt per liter of water, adjusted to pH 4 with orthophosphoric acid) and solvent B (acetonitrile) delivered at a flow rate of 1.0mlmin(-1). The analytes were detected and quantified at 210nm using photodiode array (PDA) detector. The method was validated as per ICH guidelines, demonstrating to be accurate and precise (repeatability and intermediate precision level) within the corresponding linear range of known impurities of AS and IB. The specificity of the method was investigated under different stress conditions including hydrolytic, oxidative, photolytic and thermal as recommended by ICH guidelines. Relevant degradation was found to take place under hydrolytic and oxidative conditions. Robustness against small modification in pH, column oven temperature, flow rate and percentage of the mobile phase composition was ascertained. Lower limit of quantification and detection were also determined. The peak purity indices (purity anglestability indicating capability of the method. PMID:20045275

  13. Development and Validation of a Stability-Indicating RP-HPLC Method for the Simultaneous Determination of Phenoxyethanol, Methylparaben, Propylparaben, Mometasone Furoate, and Tazarotene in Topical Pharmaceutical Dosage Formulation.

    PubMed

    Roy, Chinmoy; Chakrabarty, Jitamanyu

    2013-12-01

    A stability-indicating RP-HPLC method has been developed and validated for the simultaneous determination of phenoxyethanol (PE), methylparaben (MP), propylparaben (PP), mometasone furoate (MF), and tazarotene (TA) in topical pharmaceutical dosage formulation. The desired chromatographic separation was achieved on the Waters X-Bridge™ C18 (50×4.6mm, 3.5?) column using gradient elution at 256 nm detection wavelength. The optimized mobile phase consisted of 0.1%v/v orthophosphoric acid in water as solvent-A and acetonitrile as solvent-B. The method showed linearity over the range of 5.88-61.76 ?g/mL, 0.18-62.36 ?g/mL, 0.17-6.26 ?g/mL, 0.47-31.22 ?g/mL, and 0.44-30.45 ?g/mL for PE, MP, PP, MF, and TA, respectively. The recovery for all of the components was in the range of 98-102%. The stability-indicating capability of the developed method was established by analysing the forced degradation samples, in which the spectral purity of PE, MP, PP, MF, and TA along with the separation of degradation products from the analyte peaks was achieved. The proposed method was successfully applied for the quantitative determination of PE, MP, PP, MF, and TA in a cream sample. PMID:24482766

  14. Development and validation of a RP-HPLC method for stability-indicating assay of gemifloxacin mesylate including identification of related substances by LC-ESI-MS/MS, 1H and 13C NMR spectroscopy.

    PubMed

    Rao, R Nageswara; Naidu, Ch Gangu; Prasad, K Guru; Narasimha, R

    2011-11-01

    A validated stability indicating RP-HPLC assay of gemifloxacin mesylate was developed by separating its related substances on an Inertsil-ODS3V-C18 (4.6 × 250 mm; 5 ?m) column using 0.1% trifluoroaceticacid (pH 2.5) and methanol as a mobile phase in a gradient elution mode at a flow rate of 1.0 mL/min at 27°C. The column effluents were monitored by a photodiode array detector set at 287 nm. The method was validated in terms of accuracy, precision and linearity as per ICH guidelines. Forced degradation of gemifloxacin (GFX) was carried out under acidic, basic, thermal, photolysis and peroxide conditions and the degradation products were separated and characterized by ESI-MS/MS, (1) H and (13) C NMR spectroscopy. The method was successfully applied to the analysis of bulk drugs and the recoveries of gemifloxacin and impurities were in the range of 97.60-102.90 and 96.99-102.10%, respectively. No previous reports were found in the literature on identification of degradation products of gemifloxacin. PMID:21370250

  15. Development and Validation of Rapid Stability-Indicating RP-HPLC-DAD Method for the Quantification of Lapatinib and Mass Spectrometry Analysis of Degraded Products.

    PubMed

    Saadat, Ebrahim; Dehghan Kelishady, Pooya; Ravar, Fatemeh; Kobarfard, Farzad; Dorkoosh, Farid A

    2015-07-01

    A rapid, simple and stability-indicating high-performance liquid chromatography assay method was developed and validated for quantitative analysis of lapatinib (LPT) in bulk pharmaceuticals. The newly developed method was assessed using a C18 MZ-Analytical column (5 µm, 150 × 4.6 mm, OSD-3), which was protected by a (5 µm, 4.0 × 4.6 mm, OSD-3) pre-column with mobile phase that was composed of acetonitrile and water (70/30, v/v) and a detection wave length of 227 nm. The method was validated according to the ICH guidelines with respect to precision, accuracy, linearity, robustness, specificity and system suitability. Forced degradation studies were also performed for LPT to determine the stability-indicating aspect of developed method. The method was found to be specific for LPT in the presence of degradation products. The retention time of LPT was ?4 min. Accuracy of the method was found to be 2.20% bias for all tested samples. The inter- and intra-day precision of the novel method were found to be 2.84 and 2.78%, respectively. The calibration curve was linear over the concentration range of 5-80 µg/mL with a regression coefficient of 0.9990. The limits of detection and quantification were also found to be 1 and 5 µg/mL, respectively. Mass spectrometry analysis was performed in order to better characterize degraded products. PMID:25491314

  16. Validated stability indicating RP-HPLC for quantitation of nitazoxanide in presence of its alkaline degradation products and their characterization by HPLC-tandem mass spectrometry.

    PubMed

    Hegazy, Maha; Kessiba, Amira; El Gindy, Ahmed Emad; Abdelkawy, Mohamed

    2014-10-01

    A simple and sensitive stability indicating HPLC method was developed and validated for quantitative determination of Nitazoxanide (NTZ), a new antiprotozoal drug, in presence of degradation products generated under forced alkaline hydrolysis. Chromatographic separation was achieved on Inertsil C8-3 column (150 × 4.6 mm i.d.) using a mobile phase composed of acetonitrile: 50 mM ammonium acetate buffer (50:50, v/v, pH 5.0 adjusted with acetic acid) at a flow rate of 1 mL/min. Quantification was achieved with UV detection at 298 nm based on relative peak area. The method was linear over the concentration range of 0.8-50 µg/mL (r = 0.9999) with a limit of detection and quantification 0.0410 and 0.1242 µg/mL, respectively. The developed method has the requisite accuracy, selectivity, sensitivity and precision to assay NTZ in presence of its degradation products either in bulk powder or in pharmaceutical formulations. The degradation products were then identified by HPLC-MS/MS analysis using an electrospray ionization source and an ion trap analyzer. PMID:24248557

  17. Quality by Design-Based Development of a Stability-Indicating RP-HPLC Method for the Simultaneous Determination of Methylparaben, Propylparaben, Diethylamino Hydroxybenzoyl Hexyl Benzoate, and Octinoxate in Topical Pharmaceutical Formulation

    PubMed Central

    Roy, Chinmoy; Chakrabarty, Jitamanyu

    2014-01-01

    Abstract A stability-indicating RP-HPLC method has been developed and validated for the simultaneous determination of methylparaben (MP), propylparaben (PP), diethylamino hydroxybenzoyl hexyl benzoate (DAHHB), and octinoxate (OCT) in topical pharmaceutical formulation. The desired chromatographic separation was achieved on the KinetexTM C18 (250 × 4.6 mm, 5 ?m) column using gradient elution at 257 nm detection wavelength. The optimized mobile phase consisted of a buffer : acetonitrile : tetrahydrofuran (60 : 30 : 10, v/v/v) as solvent A and acetonitrile : tetrahydrofuran (70 : 30, v/v) as solvent B. The method showed linearity over the range of 0.19–148.4 ?g/mL, 0.23–15.3 ?g/mL, 1.97–600.5 ?g/mL, and 1.85–451.5 ?g/mL for MP, PP, DAHHB, and OCT, respectively. Recovery for all the components was found to be in the range of 98–102%. The stability-indicating capability of the developed method was established by analysing the forced degradation samples in which the spectral purity of MP, PP, DAHHB, and OCT, along with the separation of the degradation products from the analyte peaks, was achieved. The proposed method was successfully applied for the quantitative determination of MP, PP, DAHHB, and OCT in the lotion sample. The design expert with ANOVA software with the linear model was applied and a 24 full factorial design was employed to estimate the model coefficients and also to check the robustness of the method. Results of the two-level full factorial design, 24 with 20 runs including four centrepoint analysis based on the variance analysis (ANOVA), demonstrated that all four factors, as well as the interactions of resolution between DAHHB and OCT are statistically significant. PMID:25853065

  18. Highly efficient, selective, sensitive and stability indicating RP-HPLC-UV method for the quantitative determination of potential impurities and characterization of four novel impurities in eslicarbazepine acetate active pharmaceutical ingredient by LC/ESI-IT/MS/MS.

    PubMed

    Thomas, Saji; Bharti, Amber; Maddhesia, Pawan Kumar; Shandilya, Sanjeev; Agarwal, Ashutosh; Dharamvir; Biswas, Sujay; Bhansal, Vikas; Gupta, Ashish Kumar; Tewari, Praveen Kumar; Mathela, Chandra S

    2012-03-01

    A novel, sensitive, selective and stability indicating LC-UV method was developed for the determination of potential impurities of eslicarbazepine acetate. High performance liquid chromatographic investigation of eslicarbazepine acetate laboratory sample revealed the presence of several impurities. Three impurities were characterized rapidly and four impurities were found to be unknown. The unknown impurities were identified by liquid chromatography coupled with electrospray ionization, ion trap mass spectrometry (LC/ESI-IT/MS/MS). Structural confirmation of these impurities was unambiguously carried out by synthesis followed by characterization using nuclear magnetic resonance spectroscopy (NMR), infrared spectroscopy (FT-IR) and mass spectrometry (MS). Based on the spectroscopic, spectrometric and elemental analysis data unknown impurities were characterized as 5-acetyl-5,11-dihydro-10H-dibenzo [b,f]azepin-10-one, N-acetyl-5H-dibenzo[b,f]azepine-5-carboxamide, 5-acetyl-10,11-dihydro-5H-dibenzo[b,f]azepin-10-yl acetate and 5-acetyl-5H-dibenzo[b,f]azepin-10-yl acetate. The newly developed LC-UV method was validated according to ICH guidelines considering eleven potential impurities and four new impurities to demonstrate specificity, precision, linearity, accuracy and stability indicating nature of the method. The newly developed method was found to be highly efficient, selective, sensitive and stability indicating. A plausible pathway for the formation of four new impurities is proposed. PMID:22178334

  19. Stability indicating methods for the determination of some anti-fungal agents using densitometric and RP-HPLC methods.

    PubMed

    Mousa, Bahia Abbas; El-Kousy, Naglaa Mahmoud; El-Bagary, Ramzia Ismail; Mohamed, Nashwah Gadalla

    2008-02-01

    Two chromatographic methods were developed for the determination of some anti-fungal drugs in the presence of either their degradation products or cortisone derivatives. The densitometric method determined mixtures of each of ketoconazole (KT), clotrimazole (CL), miconazole nitrate (MN) and econazole nitrate (EN) with the degradation products of each one. Mixtures of MN with hydrocortisone (HC) and of EN with triamcinolone acetonide (TA) were also successfully separated and determined by this technique. For KT and CL, a mixture of methanol:water:triethylamine (70:28:2 v/v) was used as a developing system and the spots were scanned at 243 nm and 220 nm for KT and CL, respectively. For MN and EN, a mixture of hexane:isopropyl alcohol:triethylamine (80:17:3 v/v) was used as a developing system and the spots were scanned at 225 nm for both drugs. The HPLC method determined mixtures of CL or EN with their degradation products which were separated and quantified on a Zorbax C8 column. Elution was carried out using methanol:phosphate buffer pH 2.5 (65:35 v/v) as a mobile phase at a flow rate of 1.5 ml/min and UV detection at 220 nm for CL. For EN, a mixture of methanol:water containing 0.06 ml triethylamine pH 10 (75:25 v/v) was used as a mobile phase at a flow rate of 1.5 ml/min and UV detection at 225 nm. The methods were also used to separate mixtures of CL with betamethasone dipropionate (BD) and EN with TA in a laboratory prepared mixture and in pharmaceutical preparations. The methods were sensitive, precise and applicable for determination of the drugs in pharmaceutical dosage forms. PMID:18239297

  20. Identification of Rhodiola species by using RP-HPLC*

    PubMed Central

    Wang, Qiang; Ruan, Xiao; Jin, Zhi-hua; Yan, Qi-chuan; Tu, Shan-jun

    2005-01-01

    An approach was established using RP-HPLC (reversed-phase high-performance liquid chromatography) to identify ten species of Rhodiola, R. coccinea A. Bor, R. junggarica C.Y. Yang et N.R. Cui spn., R. heterodonta A. Bor, R. linearifolia A. Bor, R. pamiro alaiucm A. Bor, R. kaschgarica A. Bor, R. litwinowii A. Bor, R. gelida schrenk, R. rosea L. and R. quadrifide Fisch et Mey collected from the Tianshan Mountains areas of China. Chromatograms of alcohol-soluble proteins, generated from these ten Rhodiola spp. were compared. Each chromatogram of alcohol-soluble proteins came from a single seed of one wild species only. The results showed that when using a Waters Delta Pak. C18, 5 ?m particle size reversed phase column (150 mm×3.9 mm), a linear gradient of 22%–55% solvent B with a flow rate of 1 ml/min and a run time of 67 min, the chromatography gave optimum separation of Rhodiola alcohol-soluble proteins. Chromatogram of each species was different and could be used to identify those species. Cluster analysis of genetic similarity coefficients of 37% to 60% showed a medium degree of genetic diversity among the species in these eco-areas. Cluster analysis showed that the ten species of Rhodiola can be divided into four clusters and yielded the general and unique biochemical markers of these species. RP-HPLC was shown to be a rapid, repeatable and reliable method for Rhodiola species identification and analysis of genetic diversity. PMID:15909330

  1. In vitro interaction studies of diltiazem with NSAID's using UV spectrophotometry and RP-HPLC techniques.

    PubMed

    Sultana, Najma; Arayne, M Saeed; Shafi, Nighat

    2007-07-01

    Diltiazem (DTZ) is a well-known cardiovascular drug used clinically in the treatment of angina pectoris and hypertension. Present paper deals with the in vitro availability studies of DTZ in presence of commonly used nonsteroidal anti-inflammatory drugs (NSAID's) like diclofenac sodium, flurbiprofen, mefenamic acid and meloxicam. Simultaneous administration of both types of drugs may alter the antihypertensive effect of DTZ. These studies were carried out using BP 2005 dissolution test apparatus in simulated human body environments at body temperature and at elevated temperature in order to study the kinetics and energitics of these interactions. Both the drug in each case were analyzed either by measuring the absorbance of aliquots on a UV/VIS spectrophotometer, or by RP-HPLC method. Present study clearly indicated that most of the NSAID's studied bind to DTZ forming charge transfer complexes, evident from the high availability of DTZ. Hence, concurrent administration of NSAID's with DTZ is not recommended. PMID:17545105

  2. STABILITY INDICATING HPLC METHOD FOR THE DETERMINATION OF ESLICARBAZEPINE ACETATE AND ITS IMPURITIES IN BULK DRUGS AND PHARMACEUTICAL DOSAGE FORMS

    Microsoft Academic Search

    Mudigonda Srinivas; Narasimha Rao Avupati; Shakil Sait; K. Mukkanti

    2012-01-01

    A new stability-indicating gradient reverse phase high-performance liquid chromatographic (RP-HPLC) method was developed for the quantitative determination of Eslicarbazepine acetate (antiepileptic drug) in bulk drugs and pharmaceutical dosage forms along with its impurities and degradation products. The method was developed using Zorbax SB C-18 (150 mm × 4.6 mm, 3.5 µm) column with mobile phase containing a gradient mixture of solvents A and B. The

  3. Stability indicating RP-LC determination of sildenafil citrate (Viagra) in pure form and in pharmaceutical samples

    Microsoft Academic Search

    N. D Dinesh; B. K Vishukumar; P Nagaraja; N. M Made Gowda; K. S Rangappa

    2002-01-01

    A simple, precise, sensitive and stability-indicating reverse-phase high performance liquid chromatographic (RP-HPLC) method has been developed for the quantitation of sildenafil citrate (SC) in pure form and its pharmaceutical formulations. Method employs water and acetonitrile (48:52 v\\/v) as mobile phase with flow rate of 1 ml min?1, LiChrospher C18-5 ?m (25×0.46 cm) column and UV detection set at 245 nm.

  4. A STABILITY INDICATING HPLC METHOD FOR THE DETERMINATION OF ESLICARBAZEPINE ACETATE AND ITS IMPURITIES IN BULK DRUGS AND PHARMACEUTICAL DOSAGE FORMS

    Microsoft Academic Search

    M. Srinivas; Narasimha Rao Avupati; Shakil Sait; K. Mukkanti

    2012-01-01

    A new stability-indicating gradient reverse phase high-performance liquid chromatographic (RP-HPLC) method was developed for the quantitative determination of Eslicarbazepine acetate (antiepileptic drug) in bulk drugs and pharmaceutical dosage forms along with its impurities and degradation products. The method was developed using Zorbax SB C-18 (150 mm × 4.6 mm, 3.5 µm) column with mobile phase containing a gradient mixture of solvents A and B. The

  5. A validated stability-indicating HPLC with photodiode array detector (PDA) method for the stress tests of Monascus purpureus-fermented rice, red yeast rice

    Microsoft Academic Search

    Yong-Guo Li; Hong Liu; Zheng-Tao Wang

    2005-01-01

    A stability-indicating reversed phase high-performance liquid chromatography (RP-HPLC) with photodiode array (PDA) detection method was developed and validated for the assay of monacolin series compounds including monacolin K, L, J and their hydroxyl acid forms as well as dehydroxymonacolin K simultaneously in Monascus purpureus-fermented rice, red yeast rice. Well-resolved peaks of seven main compounds of monacolin family were profiled on

  6. Cerebral nuclei distribution study of dehydrodiisoeugenol as an anxiogenic agent determined by RP-HPLC.

    PubMed

    Zhang, You-Bo; Zhu, Li-Qiao; Yang, Xiu-Wei

    2013-01-01

    A sensitive RP-HPLC-DAD method was established to quantify dehydrodiisoeugenol (DDIE) in rat cerebral nuclei. The assay procedure involved one-step extraction of DDIE and daidzein, as an internal standard, from rat plasma and various cerebral nuclei with ethyl acetate. Chromatographic separation was performed on a Diamonsil™ ODS C(18) column with methanol-water (81:19, v/v) as a mobile phase. The UV absorbance of the samples was measured at the wavelength of 270nm. The analysis method was proved to be precise and accurate at linearity ranges in plasma and each cerebral nucleus with correlation coefficients of ?0.9971. The results indicated that the method established was successfully applied to cerebral nuclei distribution study of DDIE after intravenous administration at a single dose of 40mg/kg to rat. DDIE showed high concentration in all of cerebral nuclei at 8min, which indicated that DDIE could cross the blood-brain barrier rapidly and might be one of the main bioactive substances of nutmeg. The results provide fundamental data for evaluating the effects of DDIE on the central nervous system and to be developed into an effective anxiogenic agent. PMID:23059843

  7. RP-HPLC LIPOPHILICITY STUDIES FOR SOME (HETERO)ARYLAMIDES DERIVED FROM 2AMINO 4,6DIMETHYL PYRIDINE: INTRODUCTION OF AN HYDROGEN-BOND DESCRIPTOR

    Microsoft Academic Search

    Khalid Fikri; Jean Debord; Jean-Claude Bollinger; Dominique Cledat; Bernard Penicaut; Jean-Michel H. Robert

    2011-01-01

    RP-HPLC measurements (in water + 60% v\\/v acetonitrile, on a porous polystyrene column) lead to a linear calibration between the retention factor logk and the lipophilicity logP for a series of 9 OECD standards. Introduction of a variable indicator D for hydrogen-bond donors enhances the goodness of fit. From experimental retention factors, estimated values of logP are given for 23 substituted (hetero)arylcarboxamides

  8. Determination of methylparaben, propylparaben, triamcinolone acetonide and its degradation product in a topical cream by RP-HPLC.

    PubMed

    Matysová, L; Hájková, R; Sícha, J; Solich, P

    2003-06-01

    A novel reversed-phase high-performance liquid chromatographic (RP-HPLC) method was developed and validated for the determination of active component triamcinolone acetonide, its degradation product triamcinolone (occurring in formulation after long-term stability tests) and two preservatives presented in the cream-methylparaben and propylparaben, using hydrocortisone as an internal standard. The chromatographic separation was performed on a Supelco Discovery C18 column; the mobile phase for separation of all compounds consists of a mixture of acetonitrile and water (40:60 v/v). The analysis time was less than 9 min, at a flow rate of 0.6 mL min(-1) and detection at 240 nm. The method was found to be applicable for routine analysis (stability tests, homogeneity) in the pharmaceutical product topical cream Triamcinolon cream 0.1%. PMID:12819846

  9. Quantitative analysis of quercetin in Euphorbia helioscopia L by RP-HPLC.

    PubMed

    Liu, Hai Peng; Shi, Xiao Feng; Zhang, You Cheng; Li, Zhong Xin; Zhang, Lin; Wang, Zhe Yuan

    2011-09-01

    Euphorbia helioscopia L is widespread in China and has a large number of flavonoids. Quercetin glycosides, having useful biological activities, are abundant in this plant, and no validated analytical method has so far been developed for their determination. We, therefore, standardized a reversed-phase high-performance liquid chromatography (RP-HPLC) assay for quercetin detection. For this, the plant was locally procured and identification was confirmed based on its morpho-histological characteristics. Ethyl acetate extracts of leaves, stems, and roots were analyzed by RP-HPLC using Agilent 1120 HPLC TC-C(18) column (250 × 4.6 mm; 5 ?m) with UV-detector system. The mobile phase of methanol-0.2% phosphoric acid (65:35) solution was used with the flow rate of 1.0 ml min(-1) at 30°C, and the detection was performed at 360 nm wavelength. Our data show that the linear range of quercetin was 0.025-0.150 mg.ml(-1) (r = 0.9995; n = 6) with the recovery rate of 97.50-103.30% (average 100.40%; RSD = 2.28%). The target component was baseline separated during only the period of 9 min. The repeatability of RP-HPLC analysis was demonstrated with an RSD of 1.77% (n = 6), and the highest quercetin content (average 1.42 mg g(-1)dry-weight) was present in leaves. It was, therefore, concluded that RP-HPLC is a simple, rapid, accurate, and sensitive method for the detection of quercetin from Euphorbia helioscopia L. PMID:21327945

  10. Quantitative Analysis of Quercetin in Euphorbia helioscopia L by RP-HPLC

    Microsoft Academic Search

    Hai Peng Liu; Xiao Feng Shi; You Cheng Zhang; Zhong Xin Li; Lin Zhang; Zhe Yuan Wang

    Euphorbia helioscopia L is widespread in China and has a large number of flavonoids. Quercetin glycosides, having useful biological activities,\\u000a are abundant in this plant, and no validated analytical method has so far been developed for their determination. We, therefore,\\u000a standardized a reversed-phase high-performance liquid chromatography (RP-HPLC) assay for quercetin detection. For this, the\\u000a plant was locally procured and identification

  11. Simultaneous estimation of phenolic acids in sea buckthorn ( Hippophaë rhamnoides) using RP-HPLC with DAD

    Microsoft Academic Search

    Ranjith Arimboor; K. Sarin Kumar; C. Arumughan

    2008-01-01

    A RP-HPLC-DAD method was developed and validated for the simultaneous analysis of nine phenolic acids including gallic acid, protocatechuic acid, p-hydroxybenzoic acid, vanillic acid, salicylic acid, p-coumaric acid, cinnamic acid, caffiec acid and ferulic acid in sea buckthorn (SB) (Hippophaë rhamnoides) berries and leaves. The method was validated in terms of linearity, LOD, precision, accuracy and recovery and found to

  12. RP-HPLC and NMR study of antioxidant flavonoids in extract from Gentiana piasezkii

    Microsoft Academic Search

    Quan-Xiang Wu; Juan Chen; Yan-Ping Shi

    2010-01-01

    A reversed-phase high performance liquid chromatography (RP-HPLC) separation with photodiode array detection (PDA) was developed for the simultaneous determination of five flavonoids, lutonarin (LO), saponarin (SA), isoorient (IO), 7-O-feruloylorientin (FO) and luteolin (LE) in the extract of Gentiana piasezkii, a popular forage grass, pharmaceutical and ornamental plant in China. The optimized method was achieved for the separation\\u000a and detection of

  13. Development and Validation of a Specific Stability Indicating High Performance Liquid Chromatographic Method for Valsartan

    PubMed Central

    Rao, KS; Jena, N; Rao, MEB

    2010-01-01

    A stability-indicating HPLC assay method has been developed and validated for valsartan in bulk drug and pharmaceutical dosage forms. An isocratic RP-HPLC was achieved on Waters 2695 using Symmetry C18 (250mm × 4.6mm × 5?) column with the mobile phase consisting of 0.02 mM sodium dihydrogen ortho-phosphate, pH adjusted to 2.5 using ortho-phosphoric acid (solvent A), and acetonitrile (solvent B) in the ratio of 58:42 %v/v. The stress testing of valsartan was carried out under acidic, alkaline, oxidative, thermal, and photolytic conditions. Valsartan was well resolved from its degradation products. The proposed method was validated as per ICH guidelines. The method was found to be suitable for the quality control of valsartan in bulk and pharmaceutical dosage forms as well as the stability-indicating studies. PMID:21264123

  14. RP-HPLC method development and validation for simultaneous estimation of atorvastatin calcium and pioglitazone hydrochloride in pharmaceutical dosage form.

    PubMed

    Peraman, Ramalingam; Mallikarjuna, Sasikala; Ammineni, Pravalika; Kondreddy, Vinod kumar

    2014-10-01

    A simple, selective, rapid, precise and economical reversed-phase high-performance liquid chromatographic (RP-HPLC) method has been developed for simultaneous estimation of atorvastatin calcium (ATV) and pioglitazone hydrochloride (PIO) from pharmaceutical formulation. The method is carried out on a C8 (25 cm × 4.6 mm i.d., 5 ?m) column with a mobile phase consisting of acetonitrile (ACN):water (pH adjusted to 6.2 using o-phosphoric acid) in the ratio of 45:55 (v/v). The retention time of ATV and PIO is 4.1 and 8.1 min, respectively, with the flow rate of 1 mL/min with diode array detector detection at 232 nm. The linear regression analysis data from the linearity plot showed good linear relationship with a correlation coefficient (R(2)) value for ATV and PIO of 0.9998 and 0.9997 in the concentration range of 10-80 µg mL(-1), respectively. The relative standard deviation for intraday precision has been found to be <2.0%. The method is validated according to the ICH guidelines. The developed method is validated in terms of specificity, selectivity, accuracy, precision, linearity, limit of detection, limit of quantitation and solution stability. The proposed method can be used for simultaneous estimation of these drugs in marketed dosage forms. PMID:24152592

  15. RP-HPLC prefractionation and its application in expressional proteomics analysis of an in vitro viral infection model.

    PubMed

    Vaziri, Behrouz; Rahimpour, Mehdi; Eslami, Naser; Fayaz, Ahmad; Rahimian, Heshmat

    2006-10-01

    Prefractionation of complex protein mixtures is an efficient method for increasing the separation power of 2-DE. RP-HPLC has been successfully utilized as a prefractionation method prior to 2-DE. Here we describe the optimization of an efficient RP-HPLC method for prefractionation of baby hamster kidney cell solubilized proteins. A step gradient elution of acetonitrile was optimized and collected fractions were further examined by SDS-PAGE and 2-DE. By utilizing this method an effective increase in separation power of 2-DE is accomplished. Moreover, we describe the application of this method to expressional proteome analysis of a virally infected cell model. PMID:17120811

  16. Stability-indicating HPLC method for the determination of cefquinome sulfate.

    PubMed

    Do?ha?, Agnieszka; Jelil?ska, Anna; Manuszewska, Monika

    2014-01-01

    A novel and sensitive stability-indicating RP-HPLC method for the quantitative determination of cefquinome sulfate has been developed. Chromatographic separation and quantitative determination were performed using a high-performance liquid chromatograph with UV detection. As the stationary phase a LiChroCART RP-18 column (5 microm particle size, 125 mm x 4 mm, Merck, Darmstadt, Germany) was used. The mobile phase consisted of 10 volumes of acetonitrile and 90 volumes of an 0.02 M phosphate buffer (pH = 7.0). The flow rate of the mobile phase was 1.0 mL/min. The eluents were monitored by a UV-VIS detector at 268 nm. The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. Significant degradation was found under basic, oxidizing stress and UV light. The developed method was validated with respect to linearity, accuracy, precision and robustness. PMID:25272644

  17. Dissemination of the highly expressed Bx7 glutenin subunit (Glu-B1al allele) in wheat as revealed by novel PCR markers and RP-HPLC.

    PubMed

    Butow, B J; Gale, K R; Ikea, J; Juhász, A; Bedö, Z; Tamás, L; Gianibelli, M C

    2004-11-01

    Increased expression of the high molecular weight glutenin subunit (HMW-GS) Bx7 is associated with improved dough strength of wheat (Triticum aestivum L.) flour. Several cultivars and landraces of widely different genetic backgrounds from around the world have now been found to contain this so-called 'over-expressing' allelic form of the Bx7 subunit encoded by Glu-B1al. Using three methods of identification, SDS-PAGE, RP-HPLC and PCR marker analysis, as well as pedigree information, we have traced the distribution and source of this allele from a Uruguayan landrace, Americano 44D, in the mid-nineteenth century. Results are supported by knowledge of the movement of wheat lines with migrants. All cultivars possessing the Glu-B1al allele can be identified by the following attributes: (1) the elution of the By sub-unit peak before the Dx sub-unit peak by RP-HPLC, (2) high expression levels of Bx7 (>39% Mol% Bx), (3) a 43 bp insertion in the matrix-attachment region (MAR) upstream of the gene promoter relative to Bx7 and an 18 bp nucleotide duplication in the coding region of the gene. Evidence is presented indicating that these 18 and 43 bp sequence insertions are not causal for the high expression levels of Bx7 as they were also found to be present in a small number of hexaploid species, including Chinese Spring, and species expressing Glu-B1ak and Glu-B1a alleles. In addition, these sequence inserts were found in different isolates of the tetraploid wheat, T. turgidum, indicating that these insertion/deletion events occurred prior to hexaploidization. PMID:15340686

  18. The RP-HPLC method for simultaneous estimation of esomeprazole and naproxen in binary combination

    PubMed Central

    Jain, Deepak Kumar; Jain, Nitesh; Charde, Rita; Jain, Nilesh

    2011-01-01

    Objective: A simple, precise, reliable, rapid, sensitive and validated RP-HPLC method has been developed to determine esomeprazole magnesium trihydrate (ESO) and naproxen (NAP) in synthetic mixture form. Materials and Methods: Chromatographic separation achieved isocratically on Phenomenex, Luna C18 column (5 ?m, 150mm × 4.60mm) and acetonitrile: phosphate buffer (pH 7.0) in the ratio of 50:50 (v/v) as the mobile phase, at a flow rate of 0.5 ml/min. Detection was carried out at 300 nm. The retention times for NAP and ESO was found to be 2.67 ±0.014 and 5.65 ±0.09 min respectively. Parameters such as linearity, precision, accuracy, recovery, specificity and ruggedness are studied as reported in the ICH guidelines. Results: The method was linear in the concentration range of 50-250 ?g/ml for NAP and 2-10 ?g/ml for ESO with correlation coefficient of 0.999 and 0.998 respectively. The mean recoveries obtained for NAP and ESO were 100.01% and 97.76 % respectively and RSD was less than 2. The correlation coefficients for all components are close to 1. Conclusions: Developed method was found to be accurate, precise, selective and rapid for simultaneous estimation of NAP and ESO. PMID:23781450

  19. Occurrence and behavior of system peaks in RP HPLC with solely aqueous mobile phases.

    PubMed

    Kalíková, Kveta; Hruska, Vlastimil; Svobodová, Jana; Chudoba, Richard; Gas, Bohuslav; Tesarová, Eva

    2009-09-01

    System peaks are important but often also disturbing phenomena occurring in separation systems. Behavior of system peaks was studied in reversed phase high performance liquid chromatography (RP HPLC) systems consisting of an RP Amide C16 column and aqueous solutions of organic acids with alkaline metal hydroxides as mobile phases. Binary mobile phases, composed of benzoic acid and lithium hydroxide (LiOH) or cesium hydroxide (CsOH), yielded two system peaks. The first peak was stationary and the second one moved with dilution of the mobile phase or with changes of the alkaline metal hydroxide concentration. The latter changes affected dissociation of the benzoic acid present in the mobile phase and thereby its retention. The presumption that the first system peak is not influenced by the type of alkaline metal cation and that it is related to the non-adsorbed component of the mobile phase was confirmed by a cyclic procedure. Three-component mobile phases composed of benzoic acid, tropic acid, and a hydroxide gave rise to three system peaks as expected. The first peak was again stationary and the two others shifted depending on the concentration variation of both acids. Resonance causing a zigzag peak, well described in capillary zone electrophoresis (CZE), was observed if 1-pentanol was injected into a chromatographic system with one-component mobile phase. PMID:19639550

  20. RP-HPLC determination of water-soluble vitamins in honey.

    PubMed

    Ciulu, Marco; Solinas, Silvia; Floris, Ignazio; Panzanelli, Angelo; Pilo, Maria I; Piu, Paola C; Spano, Nadia; Sanna, Gavino

    2011-01-15

    The assessment and validation of reliable analytical methods for the determination of vitamins in sugar-based matrices (e.g. honey) are still scarcely explored fields of research. This study proposes and fully validates a simple and fast RP-HPLC method for the simultaneous determination of five water-soluble vitamins (vitamin B(2), riboflavin; vitamin B(3), nicotinic acid; vitamin B(5), pantothenic acid; vitamin B(9), folic acid; and vitamin C, ascorbic acid) in honey. The method provides low detection and quantification limits, very good linearity in a large concentration interval, very good precision, and the absence of any bias. It has been successfully applied to 28 honey samples (mainly from Sardinia, Italy) of 12 different botanical origins. While the overall amount of the analytes in the samples is quite low (always below 40 mg kg(-1)), we have observed a marked dependence of some of their concentrations (i.e. vitamin B(3) and vitamin B(5)) and the botanical origin of the honey. This insight might lead to important characterization features for this food item. PMID:21147338

  1. Simultaneous determination of paracetamol and lornoxicam by RP-HPLC in bulk and tablet formulation

    PubMed Central

    Attimarad, Mahesh

    2011-01-01

    Aim: The objective of the study was to develop simple RP-HPLC method for the simultaneous determination of paracetamol and lornoxicam without prior separation. Materials and Methods: In this method, Kromasil C8 (250 mm, 4.6 mm, 5 ?m) column was used. The mobile phase used was methanol:phosphate buffer (60:40, v/v, pH 6.4), at flow rate of 1 ml min-1. UV detection was monitored at 302 nm. Results: Calibration graphs were established in the range of 1-150 ?g ml-1 and 0.5-100 ?g ml-1 for paracetamol and lornoxicam, respectively. The average retention time for paracetamol and lornoxicam was found to be 3.15 ± 0.03 min and 5.25 ± 0.06 min, respectively. The detection limit and quantitation limit for paracetamol are 0.19 ?g ml-1 and 0.59 ?g ml-1 and for lornoxicam 0.10 ?g ml-1 and 0.31 ?g mL-1, respectively. The intraday and interday precision expressed as percent relative standard deviation were below 2%. The mean recovery of paracetamol and lornoxicam was found to be in the range of 99.03-101.2%. Conclusion: The validated HPLC method was found to be rapid, precise and accurate and can be readily utilized for analysis of paracetamol and lornoxicam in bulk and in pharmaceutical formulations. PMID:23781432

  2. RP-HPLC Determination of vitamins B1 ,B 3 ,B 6, folic acid and B12 in multivitamin tablets

    Microsoft Academic Search

    JASMINA BRBORIC; SOTE VLADIMIROV

    2005-01-01

    A simple and sensitive reversed-phase, ion-pair HPLC method was developed and validated for the simultaneous determination of B-group vitamins, thiamine chloride hydro- chloride (B1), nicotinamide (B3), pyridoxine hydrochloride (B6) and folic acid in Pentovit ® coated tablets. The cyanocobalamine (B12) was determined separately, because of its low concentration in the investigated multivitamin preparation. RP-HPLC analysis was per- formed with a

  3. Estimating temperature dependence of solubility and octanol–water partition coefficient for organic compounds using RP-HPLC

    Microsoft Academic Search

    Antonio Finizio; Antonio Di Guardo

    2001-01-01

    Temperature dependence data for physical–chemical properties is increasingly required for modelling the fate of chemicals in the environment. Solubility and octanol–water partition coefficient (Kow) are among the most important parameters. A simple and fast method is presented to determine solubility and Kow of organic chemicals at different temperatures (5°C, 15°C, 25°C, 35°C) utilising a variable temperature RP-HPLC column. Correlations between

  4. Stability indicating RP-LC determination of sildenafil citrate (Viagra) in pure form and in pharmaceutical samples.

    PubMed

    Dinesh, N D; Vishukumar, B K; Nagaraja, P; Made Gowda, N M; Rangappa, K S

    2002-07-20

    A simple, precise, sensitive and stability-indicating reverse-phase high performance liquid chromatographic (RP-HPLC) method has been developed for the quantitation of sildenafil citrate (SC) in pure form and its pharmaceutical formulations. Method employs water and acetonitrile (48:52 v/v) as mobile phase with flow rate of 1 ml min(-1), LiChrospher C18-5 microm (25 x 0.46 cm) column and UV detection set at 245 nm. The internal standard method using piroxicam (PX) as the internal standard is used. The linear dynamic range of SC was found to be 0.05-7.5 microg ml(-1). The proposed method is successfully employed for the determination of SC in the tablets. The excipients present in the formulations do not interfere with the assay procedure. Analytical parameters were calculated and full statistical evaluation is included. PMID:12093504

  5. Structural modifications and adsorption capability of C18-silica\\/binary solvent interphases studied by EPR and RP-HPLC

    Microsoft Academic Search

    M. Francesca Ottaviani; Irene Leonardis; Achille Cappiello; Michela Cangiotti; Roberto Mazzeo; Helga Trufelli; Pierangela Palma

    2010-01-01

    The structure of the octadecyl (C18) chain layer attached to a silica surface in the presence of binary solvents (acetonitrile\\/water; methanol\\/water) was investigated by electron paramagnetic resonance (EPR) and reverse-phase high-performance liquid chromatography (RP-HPLC), using 4-hydroxy-2,2,6,6 tetramethylpiperidine-N-oxyl (Tempol) to mimic the behavior of pollutants with medium–low polarity. The computer-aided analysis of the EPR spectra provided structural and dynamical information of

  6. Simultaneous Determination of Tetrahydropalmatine, Magnolol, Emodin and Chrysophanol in Chinese Herbal Preparation by RP-HPLC-PDA

    Microsoft Academic Search

    Yan-Bin Shi; Yan-Ping Shi; Yan-Biao Yang; Guang Feng

    2007-01-01

    A reversed phase high performance liquid chromatography coupled with photo-diode array (RP-HPLC-PDA) detection method was\\u000a proposed for simultaneous determination of tetrahydropalmatine, magnolol, emodin and chrysophanol in a Chinese herbal preparation\\u000a (Dan’an mixture). The separation was performed on a Diamonsil™ C18 column (250 × 4.6 mm, 5 ?m) with methanol and 0.1% phosphoric acid (88:12, v\\/v) as the mobile phase at the flow-rate of 0.8 mL min?1.

  7. Development and Validation of an RP-HPLC Method for Quantitative Estimation of Eslicarbazepine Acetate in Bulk Drug and Tablets

    PubMed Central

    Singh, M.; Kumar, L.; Arora, P.; Mathur, S. C.; Saini, P. K.; Singh, R. M.; Singh, G. N.

    2013-01-01

    A convenient, simple, accurate, precise and reproducible RP-HPLC method was developed and validated for the estimation of eslicarbazepine acetate in bulk drug and tablet dosage form. Objective was achieved under optimised chromatographic conditions on Dionex RP-HPLC system with Dionex C18 column (250×4.6 mm, 5 ?m particle size) using mobile phase composed of methanol and ammonium acetate (0.005 M) in the ratio of 70:30 v/v. The separation was achieved using an isocratic elution method with a flow rate of 1.0 ml/ min at room temperature. The effluent was monitored at 230 nm using diode array detector. The retention time of eslicarbazepine acetate is found to be 4.9 min and the standard calibration plot was linear over a concentration range of 10-90 ?g/ml with r2=0.9995. The limit of detection and quantification were found to be 3.144 and 9.52 ?g/ml, respectively. The amount of eslicarbazepine acetate in bulk and tablet dosage form was found to be 99.19 and 97.88%, respectively. The method was validated statistically using the percent relative standard deviation and the values are found to be within the limits. The recovery studies were performed and the percentage recoveries were found to be 98.33± 0.5%. PMID:24591752

  8. Development and Validation of an RP-HPLC Method for Quantitative Estimation of Eslicarbazepine Acetate in Bulk Drug and Tablets.

    PubMed

    Singh, M; Kumar, L; Arora, P; Mathur, S C; Saini, P K; Singh, R M; Singh, G N

    2013-11-01

    A convenient, simple, accurate, precise and reproducible RP-HPLC method was developed and validated for the estimation of eslicarbazepine acetate in bulk drug and tablet dosage form. Objective was achieved under optimised chromatographic conditions on Dionex RP-HPLC system with Dionex C18 column (250×4.6 mm, 5 ?m particle size) using mobile phase composed of methanol and ammonium acetate (0.005 M) in the ratio of 70:30 v/v. The separation was achieved using an isocratic elution method with a flow rate of 1.0 ml/ min at room temperature. The effluent was monitored at 230 nm using diode array detector. The retention time of eslicarbazepine acetate is found to be 4.9 min and the standard calibration plot was linear over a concentration range of 10-90 ?g/ml with r(2)=0.9995. The limit of detection and quantification were found to be 3.144 and 9.52 ?g/ml, respectively. The amount of eslicarbazepine acetate in bulk and tablet dosage form was found to be 99.19 and 97.88%, respectively. The method was validated statistically using the percent relative standard deviation and the values are found to be within the limits. The recovery studies were performed and the percentage recoveries were found to be 98.33± 0.5%. PMID:24591752

  9. RP-HPLC-fluorescence analysis of aliphatic aldehydes: application to aldehyde-generating enzymes HACL1 and SGPL1

    PubMed Central

    Mezzar, Serena; de Schryver, Evelyn; Van Veldhoven, Paul P.

    2014-01-01

    Long-chain aldehydes are commonly produced in various processes, such as peroxisomal ?-oxidation of long-chain 3-methyl-branched and 2-hydroxy fatty acids and microsomal breakdown of phosphorylated sphingoid bases. The enzymes involved in the aldehyde-generating steps of these processes are 2-hydroxyacyl-CoA lyase (HACL1) and sphingosine-1-phosphate lyase (SGPL1), respectively. In the present work, nonradioactive assays for these enzymes were developed employing the Hantzsch reaction. Tridecanal (C13-al) and heptadecanal (C17-al) were selected as model compounds and cyclohexane-1,3-dione as 1,3-diketone, and the fluorescent derivatives were analyzed by reversed phase (RP)-HPLC. Assay mixture composition, as well as pH and heating, were optimized for C13-al and C17-al. Under optimized conditions, these aldehydes could be quantified in picomolar range and different long-chain aldehyde derivatives were well resolved with a linear gradient elution by RP-HPLC. Aldehydes generated by recombinant enzymes could easily be detected via this method. Moreover, the assay allowed to document activity or deficiency in tissue homogenates and fibroblast lysates without an extraction step. In conclusion, a simple, quick, and cheap assay for the study of HACL1 and SGPL1 activities was developed, without relying on expensive mass spectrometric detectors or radioactive substrates. PMID:24323699

  10. RP-HPLC-fluorescence analysis of aliphatic aldehydes: application to aldehyde-generating enzymes HACL1 and SGPL1.

    PubMed

    Mezzar, Serena; de Schryver, Evelyn; Van Veldhoven, Paul P

    2014-03-01

    Long-chain aldehydes are commonly produced in various processes, such as peroxisomal ?-oxidation of long-chain 3-methyl-branched and 2-hydroxy fatty acids and microsomal breakdown of phosphorylated sphingoid bases. The enzymes involved in the aldehyde-generating steps of these processes are 2-hydroxyacyl-CoA lyase (HACL1) and sphingosine-1-phosphate lyase (SGPL1), respectively. In the present work, nonradioactive assays for these enzymes were developed employing the Hantzsch reaction. Tridecanal (C13-al) and heptadecanal (C17-al) were selected as model compounds and cyclohexane-1,3-dione as 1,3-diketone, and the fluorescent derivatives were analyzed by reversed phase (RP)-HPLC. Assay mixture composition, as well as pH and heating, were optimized for C13-al and C17-al. Under optimized conditions, these aldehydes could be quantified in picomolar range and different long-chain aldehyde derivatives were well resolved with a linear gradient elution by RP-HPLC. Aldehydes generated by recombinant enzymes could easily be detected via this method. Moreover, the assay allowed to document activity or deficiency in tissue homogenates and fibroblast lysates without an extraction step. In conclusion, a simple, quick, and cheap assay for the study of HACL1 and SGPL1 activities was developed, without relying on expensive mass spectrometric detectors or radioactive substrates. PMID:24323699

  11. Quantization of Dextromethorphan and Levocetirizine in Combined Dosage form Using a Novel Validated RP-HPLC Method

    PubMed Central

    Joshi, Shalini; Bhatia, C.; Bal, C. S.; Rawat, M. S. M.

    2012-01-01

    The present study reveals a simple isocratic RP-HPLC method for the simultaneous determination of dextromethorphan hydrobromide and levocetirizine dihydrochloride in a cough syrup. The separation of these compounds was achieved within 10 min on a Phenomenex (USA) C18 analytical column, 250×4.0 mm i.d., using an isocratic mobile phase consisting of potassium dihydrogen phosphate buffer (pH 2.5) - acetonitrile- tetrahydrofuran (70:25:5, v/v/v). The analysis was performed at a flow rate of 1.2 ml/min and at a detection wavelength of 232 nm. Percentage recovery and RSD were 100.36% and 0.05% for levocetirizine dihydrochloride, 100.35% and 0.27% for dextromethorphan hydrobromide respectively. Quantification of the components in syrup formulation was calculated against the peak areas of freshly prepared standard solutions. The method was validated as per ICH guidelines. PMID:23204629

  12. A validated RP-HPLC-UV method for quantitative determination of puerarin in Pueraria tuberosa DC tuber extract

    PubMed Central

    Maji, Amal K.; Maity, Niladri; Banerji, Pratim; Banerjee, Debdulal

    2012-01-01

    Background: Pueraria tuberosa (Fabaceae) is a well-known medicinal herbs used in Indian traditional medicines. The puerarin is one of the most important bioactive constituent found in the tubers of this plant. Quantitative estimation of bioactive molecules is essential for the purpose of quality control and dose determination of herbal medicines. The study was designed to develop a validated reversed phase high-performance liquid chromatography (RP-HPLC) method for the quantification of puerarin in the tuber extract of P. tuberosa. Materials and Methods: The RP-HPLC system with Luna C18 (2) 100 Å, 250 × 4.6 mm column was used in this study. The analysis was performed using the mobile phase: 0.1% acetic acid in acetonitrile and 0.1% acetic acid in water (90:10, v/v) under column temperature 25°C. The detection wavelength was set at 254 nm with a flow rate of 1 ml/min. The method validation was performed according to the guidelines of International Conference on Harmonization. Results: The puerarin content of P. tuberosa extract was found to be 9.28 ±0.09%. The calibration curve showed good linearity relationship in the range of 200-1000?g/ml (r2>0.99). The LOD and LOQ were 57.12 and 181.26?g/ml, respectively and the average recovery of puerarin was 99.73% ±1.02%. The evaluation of system suitability, precision, robustness and ruggedness parameters were also found to produce satisfactory results. Conclusions: The developed method is very simple and rapid with excellent specificity, accuracy and precision which can be useful for the routine analysis and quantitative estimation of puerarin in plant extracts and formulations. PMID:23781483

  13. Bioactive compounds, RP-HPLC analysis of phenolics, and antioxidant activity of some Portuguese shrub species extracts.

    PubMed

    Luís, Angelo; Domingues, Fernanda; Duarte, Ana Paula

    2011-12-01

    In the ecosystem of Serra Da Estrela, some plant species have the potential to be used as raw material for extraction of bioactive products. The goal of this work was to determine the phenolic, flavonoid, tannin and alkaloid contents of the methanolic extracts of some shrubs (Echinospartum ibericum, Pterospartum tridentatum, Juniperus communis, Ruscus aculeatus, Rubus ulmifolius, Hakea sericea, Cytisus multiflorus, Crataegus monogyna, Erica arborea and Ipomoea acuminata), and then to correlate the phenolic compounds and flavonoids with the antioxidant activity of each extract. The Folin-Ciocalteu's method was used for the determination of total phenols, and tannins were then precipitated with polyvinylpolypyrrolidone (PVPP); a colorimetric method with aluminum chloride was used for the determination of flavonoids, and a Dragendorff's reagent method was used for total alkaloid estimation. The 2,2-diphenyl-1-picrylhydrazyl (DPPH) and beta-carotene bleaching tests were used to assess the antioxidant activity of extracts. The identification of phenolic compounds present in extracts was performed using RP-HPLC. A positive linear correlation between antioxidant activity index and total phenolic content of methanolic extracts was observed. The RP-HPLC procedure showed that the most common compounds were ferulic and ellagic acids and quercetin. Most of the studied shrubs have significant antioxidant properties that are probably due to the existence of phenolic compounds in the extracts. It is noteworthy to emphasize that for Echinospartum ibericum, Hakea sericea and Ipomoea acuminata, to the best of our knowledge, no phytochemical studies have been undertaken nor their use in traditional medicine been described. PMID:22312726

  14. Simultaneous determination of catechin, rutin, quercetin kaempferol and isorhamnetin in the extract of sea buckthorn ( Hippophae rhamnoides L.) leaves by RP-HPLC with DAD

    Microsoft Academic Search

    Yuangang Zu; Chunying Li; Yujie Fu; Chunjian Zhao

    2006-01-01

    A rapid and specific reversed-phase high performance liquid chromatography (RP-HPLC) method with diode array detection (DAD) at room temperature was used and validated for the simultaneous determination of five flavonoids (catechin, CA; rutin, RU; quercetin, QU; kaempferol, KA; isorhamnetin, IS) in the extract of sea buckthorn (Hippophae rhamnoides L.) leaves. The sample pretreatment process involved ultrasonic extraction with 85% ethanol

  15. Stability-Indicating HPLC Method for the Determination of Cefcapene Pivoxil.

    PubMed

    Zalewski, Przemys?aw; Cielecka-Piontek, Judyta; Garbacki, Piotr; Jeli?ska, Anna; Kara?niewicz-?ada, Marta

    2013-04-01

    The stability-indicating LC assay method was developed and validated for quantitative determination of cefcapene pivoxil in the presence of degradation products formed during forced degradation studies. An isocratic RP-HPLC method was developed with a Lichrospher RP-18 (250 mm × 4.6 mm, 5 ?m) column and the mobile phase composed of 45 volumes of acetonitrile and 55 volumes of mixture composed of citric acid 10 mmol L(-1) and potassium chloride 18 mmol L(-1). The flow rate of the mobile phase was 1 mL min(-1). Detection wavelength was 270 nm and temperature was 30 °C. Cefcapene pivoxil, similar to other cephalosporins, was subjected to stress conditions of degradation in aqueous solutions including hydrolysis, oxidation, and thermal degradation. The method was validated with regard to linearity, accuracy, precision, selectivity, and robustness. The method was applied successfully for the determination of cefcapene pivoxil during kinetic studies in aqueous solutions (pH and thermal degradation) and in solid state (oxidative, thermal, and radiolytic degradation). PMID:23555152

  16. Determination of seven phenolic compounds in Rhizoma Sparganii by RP-HPLC.

    PubMed

    Wang, Xinsheng; Wu, Qi-nan; Wu, Yanfang; Wu, Chengying; Yue, Wei; Liang, Qiaoli

    2013-04-01

    A reversed-phase high-performance liquid chromatographic method was developed for the simultaneous quantification of seven phenolic compounds from Rhizoma Sparganii. The samples were separated on a Waters SunFire C18 column with a temperature of 30°C. Gradient elution was applied, using 0.8% acetic acid (solvent A) and methanol (solvent B) with a flow rate of 1.0 mL/min, and detection wavelength was 280 nm. The validation of the method included linearity, precision, repeatability, stability and recovery. The calibration curves showed good linear regression (R(2) > 0.9996) within the test range. The developed method indicated good precision and accuracy, with the overall intra-day and inter-day variation at less than 3%. The range of recoveries for the seven analytes was 95.34-100.06% with relative standard deviation < 3.08 %. The established method was successfully applied for the determination of seven phenolic compounds in 12 batches of Rhizoma Sparganii. The study may be useful in the quality evaluation of Rhizoma Sparganii, and can provide technical support for pharmacological and clinical research of related drugs. PMID:23013896

  17. Simultaneous determination of piracetam and its four impurities by RP-HPLC with UV detection.

    PubMed

    Arayne, M Saeed; Sultana, Najma; Siddiqui, Farhan Ahmed; Mirza, Agha Zeeshan; Qureshi, Faiza; Zuberi, M Hashim

    2010-08-01

    A simple and rapid high-performance liquid chromatographic method for the separation and determination of piracetam and its four impurities, 2-oxopyrrolidin-1-yl)acetic acid, pyrrolidin-2-one, methyl (2-oxopyrrolidin-1-yl)acetate, and ethyl (2-oxopyrrolidin-1-yl)acetate, was developed. The separation was achieved on a reversed-phase C(18) Nucleosil column (25 cm x 0.46 cm, 10 microm). The mobile phase is composed of an aqueous solution containing 0.2 g/L of triethyl amine-acetonitrile (85:15, v/v). The pH of the mobile phase was adjusted to 6.5 with phosphoric acid at a flow rate of 1 mL/min at ambient temperature and UV detection at 205 nm. The developed method was found to give good separation between the pure drug and its four related substance. The polynomial regression data for the calibration plots showed good linear relationship in the concentration range of 50-10,000 ng/mL, 25-10,000 ng/mL, 45-10,000 ng/mL, 34-10,000 ng/mL, and 55-10,000 ng/mL, respectively, with r(2) = 0.9999. The method was validated for precision, accuracy, ruggedness, and recovery. The minimum quantifiable amounts were found to be 50 ng/mL of piracetam, 25 ng/mL of 2-oxopyrrolidin-1-yl)acetic acid, 45 ng/mL of pyrrolidin-2-one, 34 ng/mL of methyl (2-oxopyrrolidin-1-yl)acetate, and 55 ng/mL of ethyl (2-oxopyrrolidin-1-yl)acetate. Statistical analysis proves that the method is reproducible and selective for the estimation of piracetam as well as its related substance. As the method could effectively separate the drug from the related substances, it can be employed as a stability-indicating one. The proposed method shows high efficiency, allowing the separation of the main component piracetam from other impurities. PMID:20819285

  18. A Validated RP HPLC-PAD Method for the Determination of Hederacoside C in Ivy-Thyme Cough Syrup

    PubMed Central

    Khdair, Ayman; Mohammad, Mohammad K.; Tawaha, Khaled; Al-Hamarsheh, Eman; AlKhatib, Hatim S.; Al-khalidi, Bashar; Bustanji, Yasser; Najjar, Samer; Hudaib, Mohammad

    2010-01-01

    A simple reversed phase high-performance liquid chromatographic (RP-HPLC) method coupled with a photodiode array detector (PAD) has been developed and validated for the analysis of hederacoside C, the marker of ivy plant, in Ivy-Thyme cough syrup. Separation of hederacoside C was achieved using a Phenomenex-Gemini C18 column isothermally at 40°C. A mobile phase system constituted of solvent A (water: acetonitrile: orthophosphoric acid (85%), 860?:?140?:?2?v/v) and solvent B (acetonitrile: orthophosphoric acid (85%), 998?:?2?v/v) was used, at gradient conditions, at a flow rate of 1.5?mL/min. Analysis was performed using UV-detection (205?nm). The method was linear over the range (0.03–0.15)?mg/mL of hederacoside C (r = 0.9992). Repeatability and intermediate precision were acceptable (RSD <2%). Limits of detection (LOD) and quantitation (LOQ) were 0.011 and 0.032?mg/mL, respectively. Percentage recovery was found to lie between 99.69% and 100.90% (RSD <2%). The method was also proved to be specific (peak-purity coefficient = 0.996). PMID:20862201

  19. Application of RP-HPLC-diode array detector after SPE to the determination of pesticides in pepper samples.

    PubMed

    Tuzimski, Tomasz

    2012-01-01

    The application of HPLC-diode array detector (DAD) after SPE for identification and quantitative analysis of pesticides in red and green pepper samples is demonstrated. An HPLC procedure on an RP column (C18) was developed for analysis of selected pesticides from different chemical groups: metamitron, metalaxyl, linuron, and prometryn. Average recoveries for C18 Polar Plus cartridges and solvents by the proposed RP-HPLC-DAD method after SPE are presented. Average recoveries from the spiked samples and the SDs were 22.5 +/- 2.2, 138.0 +/- 4.1, 78.6 +/- 2.8, and 109.2 +/- 2.3% for metamitron, metalaxyl, linuron, and prometryn, respectively, at concentrations of 7 microg/g in the plant material. The efficiency of the SPE procedure was evaluated using real food samples. The quantities of prometryn, linuron, metalaxyl, and metamitron determined were in the ranges of 0.02-2.24 microg/g (n = 24), 0.08-1.01 microg/g (n = 9), 1.61-2.28 microg/g (n=4), and 0.05-1.07 microg/g (n = 3), respectively, in plant material sampled in 2011. The method was validated for precision, repeatability, and accuracy. PMID:23175966

  20. Comparison of RP-HPLC modes to analyse the N-glycome of the free-living nematode Pristionchus pacificus.

    PubMed

    Yan, Shi; Wilson, Iain B H; Paschinger, Katharina

    2015-06-01

    Pristionchus pacificus is a free-living nematode increasingly used as an organism for comparison to the more familiar model Caenorhabditis elegans. In this study, we examined the N-glycans of this organism isolated after serial release with peptide:N-glycosidases F and A; after fluorescent labelling with 2-aminopyridine, chromatographic fractionation by three types of RP-HPLC (with either classical C18, fused core C18 or alkylamide-bonded phases) followed by mass spectrometric analyses revealed key features of its N-glycome. In addition to paucimannosidic and oligomannosidic glycans typical of invertebrates, N-glycans with two core fucose residues were detected. Furthermore, a range of glycans carrying up to three phosphorylcholine residues was observed whereas, unlike C. elegans, no tetrafucosylated N-glycans were detected. Structures with three fucose residues, unusual methylation of core ?1,3-fucose or with galactosylated fucose motifs were found in low amounts; these features may correlate with a different ensemble or expression of glycosyltransferase genes as compared to C. elegans. From an analytical perspective, both the alkylamide RP-amide and fused core C18 columns, as compared to a classical C18 material, offer advantages in terms of resolution and of elution properties, as some minor pyridylamino-labelled glycans (e.g. those carrying phosphorylcholine) appear in earlier fractions and so potential losses of such structures due to insufficient gradient length can be avoided. PMID:25639343

  1. Isolation and determination of alpha-dicarbonyl compounds by RP-HPLC-DAD in green and roasted coffee.

    PubMed

    Daglia, Maria; Papetti, Adele; Aceti, Camilla; Sordelli, Barbara; Spini, Valentina; Gazzani, Gabriella

    2007-10-31

    Glyoxal, methylglyoxal, and diacetyl formed as Maillard reaction products in heat-treated food were determined in coffee extracts (coffee brews) obtained from green beans and beans with different degrees of roast. The compounds have been reported to be mutagenic in vitro and genotoxic in experimental animals in a number of papers. More recently, alpha-dicarbonyl compounds have been implicated in the glycation process. Our data show that small amounts of glyoxal and methylglyoxal occur naturally in green coffee beans. Their concentrations increase in the early phases of the roasting process and then decline. Conversely, diacetyl is not found in green beans and forms later in the roasting process. Therefore, light and medium roasted coffees had the highest glyoxal and methylglyoxal content, whereas dark roasted coffee contained smaller amounts of glyoxal, methylglyoxal, and diacetyl. For the determination of coffee alpha-dicarbonyl compounds, a reversed-phase high performance liquid chromatography with a diode array detector (RP-HPLC-DAD) method was devised that involved the elimination of interfering compounds, such as chlorogenic acids, by solid phase extraction (SPE) and their derivatization with 1,2-diaminobenzene to give quinoxaline derivatives. Checks of SPE and derivatization conditions to verify recovery and yield, respectively, resulted in rates of 100%. The results of the validation procedure showed that the proposed method is selective, precise, accurate, and sensitive. PMID:17927199

  2. [Simultaneous determination of 4 alkaloids and a flavonoid in Picrasmae Ramulus et Folium by RP-HPLC].

    PubMed

    Wu, Chong; Deng, Gui-Hua; Lin, Chao-Zhan; Zhu, Chen-Chen

    2014-05-01

    A RP-HPLC method was developed to evaluate the quality of Picrasmae Ramulus et Folium by simultaneous determination of five constituents including 1-hydroxymethyl-beta-carboline (1), 1-methoxicabony-beta-carboline (2), 4-methoxy-5-hydroxy-canthin-6-one (3), 4, 5-dimethoxy-canthin-6-one (4) and maackiain (5) in Picrasmae Ramulus et Folium. The samples were separated on a Kromasil RP-C18 (4.6 mm x 250 mm, 5 microm) column eluted with acetonitrile and 0.1% phosphoric acid as mobile phases in gradient mode. The detection wavelength was set at 254 nm. The calibration curves and linearity of the above five standards were determined as (1) Y = 6 525.6X + 37.25 (0.009-1.780 microg, r = 0.996 8), (2) Y = 3 662.3X + 41.55 (0.005-0.920 microg, r = 0.999 5), (3) Y = 3763.1X + 146.87 (0.015-3.060 microg, r = 0.999 0), (4) Y = 2 174.1X + 21.52 (0.003-0.620 microg, r = 0.999 5), and (5) Y = 276.25X + 7.65 (0.010-1.960 microg, r = 0.998 9), respectively. The method is simple and repeatable, and can be used for the quality assessment of Picrasmae Ramulus et Folium. PMID:25095379

  3. Simultaneous determination of chloramphenicol, dexamethasone and naphazoline in ternary and quaternary mixtures by RP-HPLC, derivative and wavelet transforms of UV ratio spectra.

    PubMed

    Hoang, Vu Dang; Hue, Nguyen Thu; Tho, Nguyen Huu; Nguyen, Hue Minh Thi

    2015-03-15

    The application of chemometrics-assisted UV spectrophotometry and RP-HPLC to the simultaneous determination of chloramphenicol, dexamethasone and naphazoline in ternary and quaternary mixtures is presented. The spectrophotometric procedure is based on the first-order derivative and wavelet transforms of ratio spectra using single, double and successive divisors. The ratio spectra were differentiated and smoothed using Savitzky-Golay filter; whereas wavelet transform realized with wavelet functions (i.e. db6, gaus5 and coif3) to obtain highest spectral recoveries. For the RP-HPLC procedure, the separation was achieved on a ZORBAX SB-C18 (150×4.6 mm; 5 ?m) column at ambient temperature and the total run time was less than 7 min. A mixture of acetonitrile - 25 mM phosphate buffer pH 3 (27:73, v/v) was used as the mobile phase at a flow rate of 1.0 mL/min and the effluent monitored by measuring absorbance at 220 nm. Calibration graphs were established in the range 20-70 mg/L for chloramphenicol, 6-14 mg/L for dexamethasone and 3-8 mg/L for naphazoline (R(2)>0.990). The RP-HPLC and ratio spectra transformed by a combination of derivative-wavelet algorithms proved to be able to successfully determine all analytes in commercial eye drop formulations without sample matrix interference (mean percent recoveries, 97.4-104.3%). PMID:25546493

  4. A Validated RP-HPLC Method for Simultaneous Estimation of Nebivolol and Hydrochlorothiazide in Tablets

    PubMed Central

    Meyyanathan, S. N.; Rajan, S.; Muralidharan, S.; Birajdar, Arunadevi S.; Suresh, B.

    2008-01-01

    A simple, selective, rapid, precise and economical reverse phase high pressure liquid chromatographic method has been developed for the simultaneous estimation of nebivolol and hydrochlorthiazide from pharmaceutical formulation. Phenomenex Gemini C18 (25 cm×4.6 mm i.d., 5 ?) column with a mobile phase consisting of acetonitrile: 50mM ammonium acetate (adjusted to pH 3.5 using orthophosphoric acid) (70:30 v/v) at a flow rate of 1.0 ml/min was used. Detection was carried out at 254 nm. Probenecid was used as an internal standard. The retention times of probenecid, nebivolol and hydrochlorthiazide were 13.05, 3.32 and 4.25 min, respectively. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantitation and solution stability. The proposed method can be used for the estimation of these drugs in combined dosage forms. PMID:21394278

  5. A Validated RP-HPLC Method for Simultaneous Estimation of Nebivolol and Hydrochlorothiazide in Tablets.

    PubMed

    Meyyanathan, S N; Rajan, S; Muralidharan, S; Birajdar, Arunadevi S; Suresh, B

    2008-09-01

    A simple, selective, rapid, precise and economical reverse phase high pressure liquid chromatographic method has been developed for the simultaneous estimation of nebivolol and hydrochlorthiazide from pharmaceutical formulation. Phenomenex Gemini C(18) (25 cm×4.6 mm i.d., 5 ?) column with a mobile phase consisting of acetonitrile: 50mM ammonium acetate (adjusted to pH 3.5 using orthophosphoric acid) (70:30 v/v) at a flow rate of 1.0 ml/min was used. Detection was carried out at 254 nm. Probenecid was used as an internal standard. The retention times of probenecid, nebivolol and hydrochlorthiazide were 13.05, 3.32 and 4.25 min, respectively. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantitation and solution stability. The proposed method can be used for the estimation of these drugs in combined dosage forms. PMID:21394278

  6. Development and Validation of a RP-HPLC Method for Determination of Cyclosporine in Capsule

    PubMed Central

    Aziz, F.; Gupta, A.; Khan, M. F.

    2010-01-01

    A simple, specific and accurate reverse phase high performance liquid chromatographic method was developed for the determination of cyclosporine in capsule dosage form. XTerra C18 column was used as stationary phase with mobile phase acetonitrile in combination with 0.1% trifluoro acetic acid buffer and pH is adjusted to 1.4. Method was developed in an isocratic run of 20% trifluoro acetic acid with 80% acetonitrile for 10 min, at flow rate of 1 ml/min. Effluents were monitored at 210 nm. Retention time of cyclosporine was 3.855 min. The method was validated for specificity, linearity, accuracy, precision, limit of quantification, limit of detection, robustness and solution stability. Limit of quantification and limit of detection of cyclosporine was found to be 100 ng/ml and 200 ng/ml. Recovery was found to be in the range of 98.08-101.55%. The proposed method was successfully applied for the quantitative determination of cyclosporine in a capsule dosage form. PMID:20838535

  7. Validation and Uncertainty Estimation of an Ecofriendly and Stability-Indicating HPLC Method for Determination of Diltiazem in Pharmaceutical Preparations

    PubMed Central

    Sadeghi, Fahimeh; Navidpour, Latifeh; Bayat, Sima; Afshar, Minoo

    2013-01-01

    A green, simple, and stability-indicating RP-HPLC method was developed for the determination of diltiazem in topical preparations. The separation was based on a C18 analytical column using a mobile phase consisted of ethanol: phosphoric acid solution (pH = 2.5) (35?:?65, v/v). Column temperature was set at 50°C and quantitation was achieved with UV detection at 240?nm. In forced degradation studies, the drug was subjected to oxidation, hydrolysis, photolysis, and heat. The method was validated for specificity, selectivity, linearity, precision, accuracy, and robustness. The applied procedure was found to be linear in diltiazem concentration range of 0.5–50??g/mL (r2 = 0.9996). Precision was evaluated by replicate analysis in which % relative standard deviation (RSD) values for areas were found below 2.0. The recoveries obtained (99.25%–101.66%) ensured the accuracy of the developed method. The degradation products as well as the pharmaceutical excipients were well resolved from the pure drug. The expanded uncertainty (5.63%) of the method was also estimated from method validation data. Accordingly, the proposed validated and sustainable procedure was proved to be suitable for routine analyzing and stability studies of diltiazem in pharmaceutical preparations. PMID:24163778

  8. Simultaneous Estimation of Withaferin A and Z-Guggulsterone in Marketed Formulation by RP-HPLC.

    PubMed

    Agrawal, Poonam; Vegda, Rashmi; Laddha, Kirti

    2015-07-01

    A simple, rapid, precise and accurate high-performance liquid chromatography (HPLC) method was developed for simultaneous estimation of withaferin A and Z-guggulsterone in a polyherbal formulation containing Withania somnifera and Commiphora wightii. The chromatographic separation was achieved on a Purosphere RP-18 column (particle size 5 µm) with a mobile phase consisting of Solvent A (acetonitrile) and Solvent B (water) with the following gradients: 0-7 min, 50% A in B; 7-9 min, 50-80% A in B; 9-20 min, 80% A in B at a flow rate of 1 mL/min and detection at 235 nm. The marker compounds were well separated on the chromatogram within 20 min. The results obtained indicate accuracy and reliability of the developed simultaneous HPLC method for the quantification of withaferin A and Z-guggulsterone. The proposed method was found to be reproducible, specific, precise and accurate for simultaneous estimation of these marker compounds in a combined dosage form. The HPLC method was appropriate and the two markers are well resolved, enabling efficient quantitative analysis of withaferin A and Z-guggulsterone. The method can be successively used for quantitative analysis of these two marker constituents in combination of marketed polyherbal formulation. PMID:25572656

  9. Determination of n-octanol/water partition coefficient for DDT-related compounds by RP-HPLC with a novel dual-point retention time correction.

    PubMed

    Han, Shu-ying; Qiao, Jun-qin; Zhang, Yun-yang; Yang, Li-li; Lian, Hong-zhen; Ge, Xin; Chen, Hong-yuan

    2011-03-01

    n-Octanol/water partition coefficients (P) for DDTs and dicofol were determined by reversed-phase high performance liquid chromatography (RP-HPLC) on a C(18) column using methanol-water mixture as mobile phase. A dual-point retention time correction (DP-RTC) was proposed to rectify chromatographic retention time (t(R)) shift resulted from stationary phase aging. Based on this correction, the relationship between logP and logk(w), the logarithm of the retention factor extrapolated to pure water, was investigated for a set of 12 benzene homologues and DDT-related compounds with reliable experimental P as model compounds. A linear regression logP=(1.10±0.04) logk(w) - (0.60±0.17) was established with correlation coefficient R(2) of 0.988, cross-validated correlation coefficient R(cv)(2) of 0.983 and standard deviation (SD) of 0.156. This model was further validated using four verification compounds, naphthalene, biphenyl, 2,2-bis(4-chlorophenyl)-1,1-dichloroethane (p,p'-DDD) and 2,2-bis(4-chlorophenyl)-1,1-dichloroethene (p,p'-DDE) with similar structure to DDT. The RP-HPLC-determined P values showed good consistency with shake-flask (SFM) or slow-stirring (SSM) results, especially for highly hydrophobic compounds with logP in the range of 4-7. Then, the P values for five DDT-related compounds, 2-(2-chlorophenyl)-2-(4-chlorophenyl)-1,1,1-trichloroethane (o,p'-DDT), 2-(2-chlorophenyl)-2-(4-chlorophenyl)-1,1-dichloroethane (o,p'-DDD), 2-(2-chlorophenyl)-2-(4-chlorophenyl)-1,1-dichloroethene (o,p'-DDE), and 2,2,2-trichloro-1,1-bis(4-chlorophenyl)ethanol (dicofol) and its main degradation product 4,4'-dichlorobenzophenone (p,p'-DBP) were evaluated by the improved RP-HPLC method for the first time. The excellent precision with SD less than 0.03 proved that the novel DP-RTC protocol can significantly increases the determination accuracy and reliability of P by RP-HPLC. PMID:21300395

  10. Determination of copper, nickel, cobalt, silver, lead, cadmium, and mercury ions in water by solid-phase extraction and the RP-HPLC with UV-Vis detection

    Microsoft Academic Search

    Qiufen Hu; Guangyu Yang; Yiyun Zhao; Jiayuan Yin

    2003-01-01

    A new method for the simultaneous determination of seven heavy metal ions in water by solid-phase extraction and reversed-phase high-performance liquid chromatography (RP-HPLC) was developed. The copper, nickel, cobalt, silver, lead, cadmium, and mercury ions were pre-column derivatized with tetra(m-aminophenyl)porphyrin (Tm-APP) to form colored chelates. The metal-Tm-APP chelates in 100 mL of sample were preconcentrated to 1 mL by solid-phase

  11. Development and validation of a stability-indicating column high-performance liquid chromatographic assay method for determination of nebivolol in tablet formulation.

    PubMed

    Kachhadia, Pankaj K; Doshi, Ashish S; Joshi, Hitendra S

    2008-01-01

    A simple, precise, and accurate isocratic reversed-phase (RP) stability-indicating column high-performance liquid chromatographic (HPLC) assay method was developed and validated for determination of nebivolol in solid pharmaceutical dosage forms. Isocratic RP-HPLC separation was achieved on a Phenomenex Luna C8 (2) column (250 mm x 4.6 mm id, 5 microm particle size) using mobile phase composed of acetonitrile-pH 3.5 phosphate buffer (35 + 65, v/v) at a flow rate of 1.0 mL/min, and detection was performed at 280 nm using a photodiode array detector. The drug was subjected to oxidation, hydrolysis, photolysis, and heat to apply stress conditions. The method was validated for specificity, linearity, precision, accuracy, robustness, and solution stability. The method was linear in the drug concentration range of 40-160 microg/mL with a correlation coefficient of 0.9999. The repeatability relative standard deviation (RSD) for 6 samples was 0.69%, and the intermediate precision (RSD) for 6 samples was 1.39%. The accuracy (recovery) was between 98.57 and 99.55%. Degradation products produced as a result of stress studies did not interfere with detection of nebivolol, and the assay can thus be considered stability-indicating. PMID:18567301

  12. Isolation, Characterization, and RP-HPLC Estimation of P-Coumaric Acid from Methanolic Extract of Durva Grass (Cynodon dactylon Linn.) (Pers.)

    PubMed Central

    Karthikeyan, Ramadoss; Devadasu, Chapala; Srinivasa Babu, Puttagunta

    2015-01-01

    P-coumaric acid is a nonflavonoid phenolic acid and is a major constituent of the species Cynodon dactylon Linn. (Pers.). In this study isolation of P-coumaric acid was achieved by preparative TLC and the compound thus isolated was characterised by UV, mass, and H1 NMR spectral analysis. An isocratic RP-HPLC method was developed for the estimation of P-coumaric acid from methanolic extracts of durva grass. The chromatographic separations were achieved by RP-C18 column (250?mm?×?4.6?mm, 5??), Shimadzu LC-20AT Prominence liquid chromatograph, and a mobile phase composed of water?:?methanol?:?glacial acetic acid (65?:?34?:?1?v/v). The flow rate was 1.0?mL/min and the analyses of column effluents were performed using UV-visible detector at 310?nm. Retention time of P-coumaric acid was found to be 6.617?min. This method has obeyed linearity over the concentration range of 2–10??g/mL and the regression coefficient obtained from linearity plot for P-coumaric acid was found to be 0.999. RP-HPLC method was validated in pursuance of ICH guidelines. PMID:25788944

  13. A Novel Ion-Pair RP-HPLC Method for Simultaneous Quantification of Naproxen and Esomeprazole in Pharmaceutical Formulations.

    PubMed

    Kayesh, Ruhul; Sultan, Md Zakir

    2015-05-01

    A rapid, sensitive and stability indicating ion-pair reversed-phase high-performance liquid chromatographic method was developed for simultaneous estimation of naproxen (NPX) and esomeprazole (ESP) in pharmaceutical preparations. In our study, this new method was used to overcome the instability problem of ESP during high-performance liquid chromatographic analysis in the presence of acidic drugs such as NPX. The method was validated according to ICH, FDA and USP guidelines with respect to accuracy, precision, specificity, linearity, solution stability, robustness, sensitivity and system suitability. The method was developed by using an isocratic condition of mobile phase comprising buffer [tetrabutylammonium hydroxide (0.0077 M) and n-heptane sulfonic acid-Na salt (0.002 M), pH 7.6], acetonitrile and methanol in a 60 : 20 : 20 v/v/v ratio at a flow rate of 1.5 mL/min over a C-18 (Octadecyl-silica, 5 µm, 250 × 4.6 mm) column at ambient temperature. The recovery for both drugs was found to be >99% which demonstrated the accuracy of this method. Intra- and inter-day precision studies of the new method were less than the maximum allowable limit [% relative standard deviation (RSD) ?2.0 according to FDA]. The method showed linear response with a correlation coefficient (r(2)) value of 0.999 for both drugs. More importantly, ESP was quite stable in diluting solvent and mobile phase in the presence of NPX for >3 days. Therefore, it was found to be an accurate, reproducible, sensitive and highly stability-indicating method and can be successfully applied for routine analysis of simultaneous assay of NPX and ESP in pharmaceutical dosage forms. PMID:25182005

  14. Quantitative Determination of three Angiotensin-II-receptor Antagonists in Presence of Hydrochlorothiazide by RP-HPLC in their Tablet Preparations

    PubMed Central

    Hafez, Hany Mohammed; Elshanawane, Abdullah Ahmed; Abdelaziz, Lobna Mohammed; Kamal, Magda Mohammed

    2013-01-01

    Losartan potassium, Valsartan , Telmisartan and Irbesartan are angiotensin-II-receptor antagonists (ARA II) group which used in treatment of hypertension alone or in combination with other drugs mainly Hydrochlorothiazide. RP- HPLC method was developed for the assay of three angiotensin-II-receptor antagonists (ARA-IIs) in presence of Hydrochlorothiazide. The method was performed by reversed phase high performance liquid chromatography using a mobile phase which is consisted of 0.025 M potassium dihydrogen phosphate (pH 6.0): acetonitrile = 65:35% with detection at 220 nm on an ACE C18 column (250 mm × 4.6 mm, 5 ?m) at flow rate 1.5 mL/min in an isocratic manner. The proposed method was validated according to ICH guidline in terms of linearity, accuracy, precision , robustness, limit of detection and limit of quantitation. PMID:24523743

  15. Quantitative Determination of three Angiotensin-II-receptor Antagonists in Presence of Hydrochlorothiazide by RP-HPLC in their Tablet Preparations.

    PubMed

    Hafez, Hany Mohammed; Elshanawane, Abdullah Ahmed; Abdelaziz, Lobna Mohammed; Kamal, Magda Mohammed

    2013-01-01

    Losartan potassium, Valsartan , Telmisartan and Irbesartan are angiotensin-II-receptor antagonists (ARA II) group which used in treatment of hypertension alone or in combination with other drugs mainly Hydrochlorothiazide. RP- HPLC method was developed for the assay of three angiotensin-II-receptor antagonists (ARA-IIs) in presence of Hydrochlorothiazide. The method was performed by reversed phase high performance liquid chromatography using a mobile phase which is consisted of 0.025 M potassium dihydrogen phosphate (pH 6.0): acetonitrile = 65:35% with detection at 220 nm on an ACE C18 column (250 mm × 4.6 mm, 5 ?m) at flow rate 1.5 mL/min in an isocratic manner. The proposed method was validated according to ICH guidline in terms of linearity, accuracy, precision , robustness, limit of detection and limit of quantitation. PMID:24523743

  16. RP-HPLC method with fluorescence detection for amino acids D/L ratio determination in fossil bones as a marker of DNA preservation.

    PubMed

    Iuliani, Piera; Di Federico, Lucia; Fontecchio, Gabriella; Carlucci, Giuseppe

    2010-08-01

    Only a small proportion of old specimens contain DNA that can be amplified by PCR. Therefore, rapid screening methods are crucial to identify the large fraction of samples that are so badly preserved that there is no need to attempt DNA extraction. In particular, the extent of racemization of some amino acids has proved to be a very useful proxy for DNA preservation. In this study, a rigorous method for the determination of the D/L ratio for aspartic acid and alanine by RP-HPLC with fluorescence detection was developed with the aim to obtain a fast and cheap procedure for both sample preparation and amino acids analysis, without compromising precision and accuracy. PMID:20603838

  17. A novel approach for the quantitation of carbohydrates in mash, wort, and beer with RP-HPLC using 1-naphthylamine for precolumn derivatization.

    PubMed

    Rakete, Stefan; Glomb, Marcus A

    2013-04-24

    A novel universal method for the determination of reducing mono-, di-, and oligosaccharides in complex matrices on RP-HPLC using 1-naphthylamine for precolumn derivatization with sodium cyanoborhydride was established to study changes in the carbohydrate profile during beer brewing. Fluorescence and mass spectrometric detection enabled very sensitive analyses of beer-relevant carbohydrates. Mass spectrometry additionally allowed the identification of the molecular weight and thereby the degree of polymerization of unknown carbohydrates. Thus, carbohydrates with up to 16 glucose units were detected. Comparison demonstrated that the novel method was superior to fluorophore-assisted carbohydrate electrophoresis (FACE). The results proved the HPLC method clearly to be more powerful in regard to sensitivity and resolution. Analogous to FACE, this method was designated fluorophore-assisted carbohydrate HPLC (FAC-HPLC). PMID:23578308

  18. Tocochromanols composition in kernels recovered from different apricot varieties: RP-HPLC/FLD and RP-UPLC-ESI/MS(n) study.

    PubMed

    Górna?, Pawe?; Mišina, Inga; Gr?v?te, Ilze; Soliven, Arianne; Kaufmane, Ed?te; Segli?a, Dalija

    2015-07-01

    Composition of tocochromanols in kernels recovered from 16 different apricot varieties (Prunus armeniaca L.) was studied. Three tocopherol (T) homologues, namely ?, ? and ?, were quantified in all tested samples by an RP-HPLC/FLD method. The ?-T was the main tocopherol homologue identified in apricot kernels and constituted approximately 93% of total detected tocopherols. The RP-UPLC-ESI/MS(n) method detected trace amounts of two tocotrienol homologues ? and ? in the apricot kernels. The concentration of individual tocopherol homologues in kernels of different apricots varieties, expressed in mg/100 g dwb, was in the following range: 1.38-4.41 (?-T), 42.48-73.27 (?-T) and 0.77-2.09 (?-T). Moreover, the ratio between individual tocopherol homologues ?:?:? was nearly constant in all varieties and amounted to approximately 2:39:1. PMID:25567675

  19. Development and Validation of a Stability-Indicating LC-Method for the Simultaneous Estimation of Levodropropizine, Chloropheniramine, Methylparaben, Propylparaben, and Levodropropizine Impurities.

    PubMed

    Kumar, Palakurthi Ashok; Raju, Thummala Veera Raghava; Thirupathi, Dongala; Kumar, Ravindra; Shree, Jaya

    2013-03-01

    A simple, fast, and efficient RP-HPLC method has been developed and validated for the simultaneous estimation of Levodropropizine, Chloropheniramine, Methylparaben, Propylparaben, and the quantification of Levodropropizine impurities in the Reswas syrup dosage form. A gradient elution method was used for the separation of all the actives and Levodropropizine impurities by using the X-Bridge C18, 150 mm × 4.6 mm, 3.5 ?m column with a flow rate of 1.0 mL/min and detector wavelength at 223 nm. The mobile phase consisted of a potassium dihydrogen orthophosphate buffer and acetonitrile. All the peaks were symmetrical and well-resolved (resolution was greater than 2.5 for any pair of components) with a shorter run time. The limit of detection for Levodropropizine and its Impurity B was 0.07 ?g/ml & 0.05 ?g/ml, whereas the limit of quantification was 0.19 ?g/ml & 0.15 ?g/ml respectively. The method was validated in terms of precision, accuracy, linearity, robustness, and specificity. Degradation products resulting from the stress studies were well-resolved and did not interfere with the detection of Levodropropizine, Chloropheniramine, Methylparaben, Propylparaben, and Levodropropizine Impurity B, thus the test method is stability-indicating. Validation of the method was carried out as per International Conference on Harmonization (ICH) guidelines. PMID:23641334

  20. Simultaneous RP-HPLC-DAD quantification of bromocriptine, haloperidol and its diazepane structural analog in rat plasma with droperidol as internal standard for application to drug-interaction pharmacokinetics.

    PubMed

    Billups, Johnique; Jones, Cynthia; Jackson, Tanise L; Ablordeppey, Seth Y; Spencer, Shawn D

    2010-07-01

    A simple and rapid RP-HPLC-DAD method was developed and validated for simultaneous determination of the dopamine antagonists haloperidol, its diazepane analog, and the dopamine agonist bromocriptine in rat plasma, to perform pharmacokinetic drug-interaction studies. Samples were prepared for analysis by acetonitrile (22.0 microg/mL) plasma protein precipitation with droperidol as an internal standard, followed by a double-step liquid-liquid extraction with hexane : chloroform (70:30) prior to C-18 separation. Isocratic elution was achieved using a 0.1% (v/v) trifluoroacetic acid in deionized water, methanol and acetonitrile (45/27.5/27.5, v/v/v). Triple-wavelength diode-array detection at the lambda(max) of 245 nm for haloperidol, 254 nm for the diazepane analog and droperidol, and 240 nm for bromocriptine was carried out. The LLOQ of DAL, HAL, and BCT were 45.0, 56.1, and 150 ng/mL, respectively. In rats, the estimated pharmacokinetic parameters (i.e., t(1/2), CL, and V(ss)) of HAL when administered with DAL and BCT were t(1/2) = 16.4 min, V(ss) = 0.541 L/kg for HAL, t(1/2) = 28.0 min, V(ss) = 2.00 L/kg for DAL, and t(1/2) = 24.0 min, V(ss) = 0.106 L/kg for BCT. The PK parameters for HAL differed significantly from those previously reported, which may be an indication of a drug-drug interaction. PMID:19908205

  1. Stability-indicating determination of rebamipide in the presence of its acid degradation products.

    PubMed

    Abbas, Samah S; Zaazaa, Hala E; Essam, Hebat Allah M; El-Bardicy, Mohammed G

    2014-01-01

    Four sensitive and precise stability-indicating methods for the determination of rebamipide (REB) in the presence of its acid-degradation products and in a pharmaceutical formulation were developed and validated. Method A used the first derivative of the ratio spectra (1DD) spectrophotometric method by measuring the peak amplitude at 249.4 nm (maximum) and at 259 nm (minimum), and at the total peak amplitude (from 249.4 to 259 nm, 1DD(249.4 + 259 nm)) in the range of 2-14 microg/mL. This method yielded mean recoveries of 99.87 +/- 0.83, 100.04 +/- 0.75, and 100.28 +/- 1.11%, respectively. Method B is a dual wavelength method, which allows the determination of REB in presence of its acid-degradation products by measuring the absorbance difference between 254 and 269 nm within a linearity range of 5-65 microg/mL; it showed a mean recovery of 99.84 +/- 1.06. Method C is a TLC-densitometric procedure in which REB was separated from its degradation products using a developing solution of methanol-chloroform-ammonia (8.5 + 1.5 + 0.5, v/v/v). The quantitative evaluation of REB at 329 nm was linear over the concentration range of 0.50-4.5 microg/band, with a mean recovery of 99.49 +/- 0.99% even in the presence of up to 90% degradation products. Method D is an RP-HPLC procedure. It provided the complete separation of REB from its degradation products on an Xterra C18 column using phosphate buffer (pH 6, 0.01 M)-methanol (1 + 1, v/v) as the mobile phase (UV detection at 254 nm). Recovery was 99.28 +/- 0.78% within the range of 10-190 microg/mL. The selectivity of the proposed methods was checked using laboratory-prepared mixtures. The proposed methods have been successfully applied to the analysis of REB in pharmaceutical dosage forms without interference from other dosage form excipients. PMID:24672862

  2. The salivary proteome profile in patients affected by SAPHO syndrome characterized by a top-down RP-HPLC-ESI-MS platform.

    PubMed

    Sanna, Monica; Firinu, Davide; Manconi, Paolo Emilio; Pisanu, Maria; Murgia, Giuseppe; Piras, Valentina; Castagnola, Massimo; Messana, Irene; Del Giacco, Stefano Renato; Cabras, Tiziana

    2015-05-19

    SAPHO syndrome is a rare and often unrecognized disease with prominent inflammatory cutaneous and articular symptoms characterized by musculoskeletal manifestations (synovitis, hyperostosis, osteomyelitis) associated with dermatological conditions (severe acne and pustulosis). The acidic soluble fraction of whole saliva from 10 adult women affected by SAPHO syndrome and from a group of 28 healthy women was analysed by RP-HPLC-ESI-MS with the aim of discovering salivary biomarkers of the disorder. The levels of the oral proteins and peptides were correlated with clinical data. The following proteins showed a significant decreased concentration in saliva of SAPHO subjects with respect to controls: cystatin S1 and SN, histatins, the major acidic PRPs, P-C and P-B peptides. The cystatin SN abundance lowered according to the disease duration and histatins showed positive correlations with the C reactive protein. Statistical analysis performed excluding one patient with a different pattern of salivary proteins/peptides highlighted a positive relationship between cystatin S1, histatins 3, histatin 5, and the neutrophil count. Moreover, histatin 3 correlated positively with the total white cell count and negatively with the erythrocyte sedimentation rate. Levels and frequency of S100A12 protein showed a trend to increase in SAPHO patients. The high expression of this pro-inflammatory protein is probably related to the inflammatory response and to the altered neutrophil responses to functional stimuli that characterize SAPHO syndrome suggesting a possible application as a salivary biomarker. PMID:25671558

  3. Simultaneous determination of 15 phenolic compounds and caffeine in teas and mate using RP-HPLC/UV detection: method development and optimization of extraction process.

    PubMed

    Bae, In Kyung; Ham, Hyeon Mi; Jeong, Min Hee; Kim, Dong Ho; Kim, Ho Jin

    2015-04-01

    A reversed-phase high performance liquid chromatographic coupled to ultraviolet detection (RP-HPLC/UV) method was developed for simultaneous determination of 15 phenolic compounds and caffeine in TEAS (green tea, oolong tea, black tea and mate). Furthermore, the extraction process of total phenolic contents (TPC) from TEAS were optimized using response surface methodology (RSM) based on a central composite design (CCD) and then applied to extraction of TEAS. The best conditions obtained using the model were as follow: green tea--extraction time of 123 min, extraction temperature of 70 °C and ethanol concentration of 75%, oolong tea--extraction time of 98 min, extraction temperature of 70 °C and ethanol concentration of 69%, black tea--extraction time of 105 min, extraction temperature of 71 °C and ethanol concentration of 63%, and mate--extraction time of 103 min, extraction temperature of 71 °C and ethanol concentration of 61%. Among the extraction methods used in this study, heat-reflux extraction was found to result in the highest values of TPC. The chromatographic peaks of the 16 studied compounds were successfully identified by comparing their retention time and UV spectra with the reference standards. Method validation was performed by means of linearity, sensitivity, selectivity, accuracy and precision. The developed method was found to be simple, specific and reliable and is suited for routine analysis of phenolic compounds and caffeine in TEAS. PMID:25442580

  4. Evaluation of a Propolis Water Extract Using a Reliable RP-HPLC Methodology and In Vitro and In Vivo Efficacy and Safety Characterisation

    PubMed Central

    Rocha, Bruno Alves; Bueno, Paula Carolina Pires; Vaz, Mirela Mara de Oliveira Lima Leite; Nascimento, Andresa Piacezzi; Ferreira, Nathália Ursoli; Moreno, Gabriela de Padua; Rodrigues, Marina Rezende; Costa-Machado, Ana Rita de Mello; Barizon, Edna Aparecida; Campos, Jacqueline Costa Lima; de Oliveira, Pollyanna Francielli; Acésio, Nathália de Oliveira; Martins, Sabrina de Paula Lima; Tavares, Denise Crispim; Berretta, Andresa Aparecida

    2013-01-01

    Since the beginning of propolis research, several groups have studied its antibacterial, antifungal, and antiviral properties. However, most of these studies have only employed propolis ethanolic extract (PEE) leading to little knowledge about the biological activities of propolis water extract (PWE). Based on this, in a previous study, we demonstrated the anti-inflammatory and immunomodulatory activities of PWE. In order to better understand the equilibrium between effectiveness and toxicity, which is essential for a new medicine, the characteristics of PWE were analyzed. We developed and validated an RP-HPLC method to chemically characterize PWE and PEE and evaluated the in vitro antioxidant/antimicrobial activity for both extracts and the safety of PWE via determining genotoxic potential using in vitro and in vivo mammalian micronucleus assays. We have concluded that the proposed analytical methodology was reliable, and both extracts showed similar chemical composition. The extracts presented antioxidant and antimicrobial effects, while PWE demonstrated higher antioxidant activity and more efficacious for the most of the microorganisms tested than PEE. Finally, PWE was shown to be safe using micronucleus assays. PMID:23710228

  5. Simultaneous determination of fangchinoline and tetrandrine in Stephania tetrandra S. Moore by using 1-alkyl-3-methylimidazolium-based ionic liquids as the RP-HPLC mobile phase additives.

    PubMed

    Tang, Yan; Sun, Ailing; Liu, Renmin; Zhang, Yongqing

    2013-03-12

    A reversed phase high performance liquid chromatography (RP-HPLC) method for simultaneous determination of fangchinoline (FAN) and tetrandrine (TET) in Stephania tetrandra S. Moore was established by using 1-hexyl-3-methylimidazolium tetrafluoroborate as the mobile phase additives in this paper. Four types of 1-alkyl-3-methylimidazolium-based ionic liquids (ILs) were used as additives of the mobile phase to separate FAN and TET by RP-HPLC. The effects of the length of the alkyl group on the imidazolium ring and its counterion, the concentrations of IL and the pH of the mobile phase, which influenced the chromatographic behaviors of FAN and TET, were investigated in detail. The linearity, sensitivity, accuracy and repeatability of the proposed method were also investigated. The probable mechanism of the separation with ILs as the mobile phase additives was explored and discussed. PMID:23452799

  6. A validated stability-indicating HPLC with photodiode array detector (PDA) method for the stress tests of Monascus purpureus-fermented rice, red yeast rice.

    PubMed

    Li, Yong-Guo; Liu, Hong; Wang, Zheng-Tao

    2005-09-01

    A stability-indicating reversed phase high-performance liquid chromatography (RP-HPLC) with photodiode array (PDA) detection method was developed and validated for the assay of monacolin series compounds including monacolin K, L, J and their hydroxyl acid forms as well as dehydroxymonacolin K simultaneously in Monascus purpureus-fermented rice, red yeast rice. Well-resolved peaks of seven main compounds of monacolin family were profiled on a C(18) reverse-phase column using a linear gradient of 0.1% trifluoroacetic acid and acetonitrile as the mobile phase, and the detection wavelength was set at 237nm. The method was validated with respect to specificity, chromatographic parameters, linearity, precision, accuracy, limits of detection and quantitation. The stability stress testing for fermented red yeast rice powder was carried out to show the effects of high temperature (80 degrees C), high humidity at room temperature (92.5% RH, 25 degrees C), high humidity at high temperature (75% RH, 60 degrees C) and light (sunlight) in solid state. The results exhibited that monacolins decreased significantly under the conditions of high humidity at high temperature (75% RH, 60 degrees C) and sunlight. Monacolin K and its hydroxyl acid form would be dehydrolyzed and turned to dehydromonacolin K at high temperature (80 degrees C) while the monacolin K, J and L would be transformed into their corresponding hydroxyl acid forms under the condition of high humidity (92.5% RH, 25 degrees C). The indication is that monacolins in red yeast rice powder are light-sensitive and thermal-sensitive. Therefore, it has been suggested that the preparations containing monacolins be stored in the place of cool and lightproof. The proposed degradation pathways were discussed as well. The multi-components assay for stability of botanical products could provide much more information than the normal marker-orientation method. PMID:15876509

  7. Development and validation of a RP-HPLC method for the determination of gentamicin sulfate and its related substances in a pharmaceutical cream using a short pentafluorophenyl column and a Charged Aerosol Detector

    Microsoft Academic Search

    Arul Joseph; Abu Rustum

    2010-01-01

    Gentamicin sulfate is a potent broad spectrum aminoglycoside antibiotic which is used as an active pharmaceutical ingredient (API) against both Gram-positive and Gram-negative bacteria. A reversed-phase high performance liquid chromatographic (RP-HPLC) method has been developed and validated to determine the composition of gentamicin sulfate and to estimate its related substances (without any pre- or post-column derivatization) in a pharmaceutical cream.

  8. RP-HPLC method and its validation for the determination of naloxone from a novel transdermal formulation.

    PubMed

    Panchagnula, Ramesh; Sharma, Puneet; Khandavilli, Sateesh; Varma, Manthena V S

    2004-10-01

    The aim of the present work was to develop a simple and reliable liquid chromatographic method for the quantitative determination of naloxone (NLX) in a novel transdermal formulation. Chromatography was carried out by reversed-phase technique on a C-18 column with a mobile phase composed of methanol, acetonitrile and 50 mM phosphate buffer (pH 7) in the proportion of 40:20:40 v/v/v, at a flow rate of 1 ml/min. The UV spectrophotometric determination was performed at 220 nm. This method was found to be specific and accurate with the mean recovery of 98.72% in the range of 2-50 microg/ml, and a run time of 15 min (retention time of NLX 11.3 min). Method was applied for stability testing of novel transdermal formulation developed in our laboratory. Assay content of NLX in the formulation was determined in stability samples and compared with the control samples. Statistical analysis by Student's t-test showed no significant difference between the assay content of NLX in control and test samples at 95% confidence interval. Overall, the proposed method is highly sensitive, precise and accurate and can be used for the reliable quantitation of NLX in developed transdermal formulation with the added advantage of simple procedure. PMID:15474062

  9. Chemometrics-Assisted UV Spectrophotometric and RP-HPLC Methods for the Simultaneous Determination of Tolperisone Hydrochloride and Diclofenac Sodium in their Combined Pharmaceutical Formulation.

    PubMed

    Gohel, Nikunj Rameshbhai; Patel, Bhavin Kiritbhai; Parmar, Vijaykumar Kunvarji

    2013-12-01

    Chemometrics-assisted UV spectrophotometric and RP-HPLC methods are presented for the simultaneous determination of tolperisone hydrochloride (TOL) and diclofenac sodium (DIC) from their combined pharmaceutical dosage form. Chemometric methods are based on principal component regression and partial least-square regression models. Two sets of standard mixtures, calibration sets, and validation sets were prepared. Both models were optimized to quantify each drug in the mixture using the information included in the UV absorption spectra of the appropriate solution in the range 241-290 nm with the intervals ? = 1 nm at 50 wavelengths. The optimized models were successfully applied to the simultaneous determination of these drugs in synthetic mixture and pharmaceutical formulation. In addition, an HPLC method was developed using a reversed-phase C18 column at ambient temperature with a mobile phase consisting of methanol:acetonitrile:water (60:30:10 v/v/v), pH-adjusted to 3.0, with UV detection at 275 nm. The methods were validated in terms of linearity, accuracy, precision, sensitivity, specificity, and robustness in the range of 3-30 ?g/mL for TOL and 1-10 ?g/mL for DIC. The robustness of the HPLC method was tested using an experimental design approach. The developed HPLC method, and the PCR and PLS models were used to determine the amount of TOL and DIC in tablets. The data obtained from the PCR and PLS models were not significantly different from those obtained from the HPLC method at 95% confidence limit. PMID:24482768

  10. Chemometrics-Assisted UV Spectrophotometric and RP-HPLC Methods for the Simultaneous Determination of Tolperisone Hydrochloride and Diclofenac Sodium in their Combined Pharmaceutical Formulation

    PubMed Central

    Gohel, Nikunj Rameshbhai; Patel, Bhavin Kiritbhai; Parmar, Vijaykumar Kunvarji

    2013-01-01

    Chemometrics-assisted UV spectrophotometric and RP-HPLC methods are presented for the simultaneous determination of tolperisone hydrochloride (TOL) and diclofenac sodium (DIC) from their combined pharmaceutical dosage form. Chemometric methods are based on principal component regression and partial least-square regression models. Two sets of standard mixtures, calibration sets, and validation sets were prepared. Both models were optimized to quantify each drug in the mixture using the information included in the UV absorption spectra of the appropriate solution in the range 241–290 nm with the intervals ? = 1 nm at 50 wavelengths. The optimized models were successfully applied to the simultaneous determination of these drugs in synthetic mixture and pharmaceutical formulation. In addition, an HPLC method was developed using a reversed-phase C18 column at ambient temperature with a mobile phase consisting of methanol:acetonitrile:water (60:30:10 v/v/v), pH-adjusted to 3.0, with UV detection at 275 nm. The methods were validated in terms of linearity, accuracy, precision, sensitivity, specificity, and robustness in the range of 3–30 ?g/mL for TOL and 1–10 ?g/mL for DIC. The robustness of the HPLC method was tested using an experimental design approach. The developed HPLC method, and the PCR and PLS models were used to determine the amount of TOL and DIC in tablets. The data obtained from the PCR and PLS models were not significantly different from those obtained from the HPLC method at 95% confidence limit. PMID:24482768

  11. A developed and validated stability-indicating reverse-phase high performance liquid chromatographic method for determination of cefdinir in the presence of its degradation products as per International Conference on Harmonization guidelines

    PubMed Central

    Hamrapurkar, Purnima; Patil, Priti; Phale, Mitesh; Gandhi, Mital; Pawar, Sandeep

    2011-01-01

    The present article deals with the development and validation of a stability-indicating, reverse-phase high performance liquid chromatographic (RP-HPLC) method, for the determination of cefdinir on a Waters RP Spherisorb C-18 column (250 mm × 4.6 mm, 5 ?m). A mobile phase consisting of water (pH adjusted to 3.0 with orthophosphoric acid) : acetonitrile : methanol 13:5:2 (v/v/v) was used. The flow rate was 1 mL min-1. The separation was performed at room temperature. Detection was carried out at 286 nm, using a PDA detector. The developed method was statistically validated for the linearity, accuracy, specificity, Limit of Detection (LOD), and Limit of Quantitation (LOQ). The specificity of the method was ascertained by forced degradation studies, by acid and alkali degradation, oxidation, photolysis, and heat degradation. The degraded products were well-separated from the analyte, with significant differences in their retention time values. The Beer Law was obeyed over a concentration range of 0.05 – 15.00 ?g mL-1 and the correlation coefficient was 0.999. PMID:23781424

  12. Validated stability-indicating methods for the simultaneous determination of amiloride hydrochloride, atenolol, and chlorthalidone using HPTLC and HPLC with photodiode array detector.

    PubMed

    Youssef, Rasha M; Maher, Hadir M; El-Kimary, Eman I; Hassan, Ekram M; Barary, Magda H

    2013-01-01

    Two stability-indicating chromatographic methods are described for simultaneous determination of amiloride hydrochloride (AMI), atenolol (ATE), and chlorthalidone (CHL) in combined dosage forms. The first method was based on HPTLC separation of the three drugs followed by densitometric measurements of their bands at 274 nm. The separation was carried out on Merck HPTLC silica gel 60F254 aluminum sheets using chloroform-methanol-ammonia 27%, w/w (9 + 2 + 0.3, v/v/v) mobile phase. Analysis data was used for the linear regression graph in the range of 0.1-0.5, 0.8-5.0, and 0.3-1.5 microg/band for AMI, ATE, and CHL, respectively. The second method was based on an RP-HPLC separation of the cited drugs performed on an RP stainless steel C18 analytical column (250 x 4.6 mm id) with a gradient elution system of methanol and 0.05 M aqueous phosphate buffer adjusted to pH 4 as the mobile phase, at the flow rate of 1.0 mL/min. Quantitation was achieved with photodiode array detection at 275 nm for AMI and 225 nm for ATE and CHL. The calibration graphs for each drug were rectilinear in the range of 2-50, 25-150, and 2-100 microg/mL for AMI, ATE, and CHL, respectively. The proposed chromatographic methods were successfully applied for determination of the investigated drugs in pharmaceutical preparations. Both methods were validated in compliance with International Conference on Harmonization guidelines in terms of linearity, accuracy, precision, robustness, LOD, and LOQ. PMID:23767356

  13. Validation of a RP-HPLC method for the assay of formoterol and its related substances in formoterol fumarate dihydrate drug substance.

    PubMed

    Akapo, Samuel O; Asif, Muhammad

    2003-12-01

    A stability-indicating reversed-phase high performance liquid chromatographic (HPLC) method has been developed and validated for the assay of formoterol fumarate and the related substances, namely, formoterol fumarate desformyl and formoterol fumarate acetamide analogs, in the active pharmaceutical ingredient. The separation was achieved by isocratic elution using an Alltech Alltima C18 (150 x 4.6 mm) column, a mobile phase consisting of ammonium acetate (50 mM; pH 5.0)-ethanol (65:35, v/v), a flow rate of 1.0 ml/min and UV detection at 242 nm. The detection and quantitation limits were 0.03 and 08 microg/ml, respectively, while the linear range of detection was between 0.03 and 255 microg/ml. Comparative determinations of formoterol fumarate in three lots of bulk drugs using the proposed HPLC method and the standard potentiometric titration method of pharmacopoeia show that both methods are equivalent for pure drug substance assay. However, the HPLC method allowed the separation and quantitation of the impurities not achievable with the official methods in the bulk drugs. This study shows that the proposed method is accurate, linear, and sensitive as stability indicating assay method for formoterol fumarate in the bulk drug. PMID:14656584

  14. RP-HPLC method with fluorescence detection for determination of small quantities of triamcinolone in plasma in presence of endogenous steroids after derivatization with 9-anthroyl nitrile; pharmacokinetic studies.

    PubMed

    G?ówka, Franciszek K; Kara?niewicz, Marta; Lipnicka, Ewelina

    2006-07-24

    A new indirect RP-HPLC method was developed for determination of small, ng/ml, concentrations of triamcinolone (TMC) in human plasma, in presence of endogenous corticosteroids: cortisol (hydrocortisone, F), cortisone (E) and their metabolites, after administration of TMC in a free alcohol form. After solid phase extraction (SPE) in cartridges with octadecyl phase, TMC and prednisolone (I.S.) were derivatized by treatment with 9-anthroyl nitrile (9-AN) in a basic mixture, consisting of triethanolamine and quinuclidine, to receive fluorescent esters at 21-hydroxyl group of the steroid chain. Optimal conditions were also established to purify fluorescent TMC and I.S. derivatives before injection into HPLC column. The fluorescent esters were determined using an isocratic RP-HPLC technique in a C18 column. The mobile phase consisted of acetonitrile and 0.3 mM ortho-phoshoric acid. The method was validated before using to pharmacokinetic studies. Calibration curve of TMC was linear in the range of 2.5-100.0 ng/ml. Intra- and inter-day measurement precision and accuracy were equal to or lower than 15%. Percent recovery, and limits of detection (LOD) and quantification (LOQ) of TMC were also determined. The method was applied for in vivo conditions after administration of tablets containing TMC to healthy volunteers. Moreover, the method provided potential to determine TMC and, simultaneously, other glucocorticoids: E, F and their metabolites in one analytical run. Column interactions were observed between endogenous metabolites of E. Usefulness of the elaborated method was confirmed in pharmacokinetic studies following administration of a small (4 mg) dose of TMC to human volunteers. The method can provide an alternative to HPLC coupled with RIA in determination of small quantities of TMC. PMID:16551513

  15. Stability-indicating assay for vidarabine.

    PubMed

    Hong, W H; Szulczewski, D H

    1979-04-01

    A physicochemical procedure for the analysis of vidarabine in aqueous parenteral formulations was needed to assure potency and to define stability. Concurrent with the development of this method, its decomposition products and route in aqueous solution were determined. A quantitative procedure was developed to determine intact drug in the presence of decomposition products, and the results obtained were validated by microbial assay. Spectral (UV and polarimetric) and TLC evidence indicated that, in aqueous solution, hydrolysis without racemization occurs, yielding adenine and arabinose. The sensitivity of the method to decomposition is improved by ion-exchange separation of adenine and drug before UV measurement. Analysis of partially decomposed solutions of the drug by both ion-exchange and microbiological methods gave comparable results. PMID:438978

  16. Development and validation of a novel stability-indicating HPLC method for the quantitative determination of eleven related substances in ezetimibe drug substance and drug product.

    PubMed

    Luo, Zhiqiang; Deng, Zhongqing; Liu, Yang; Wang, Guopeng; Yang, Wenning; Hou, Chengbo; Tang, Minming; Yang, Ruirui; Zhou, Huaming

    2015-07-01

    Ezetimibe is a novel lipid-lowering agent that inhibits intestinal absorption of dietary and biliary cholesterol. In the present work, a simple, sensitive and reproducible gradient reverse phase high performance liquid chromatographic (RP-HPLC) method for separation and determination of the related substances of ezetimibe was developed and validated. Eleven potential process-related impurities (starting materials, (3S,4S,3'S)-isomer, degradants and byproducts) were identified in the crude samples. Tentative structures for all the impurities were assigned primarily based on comparison of their retention time and mass spectrometric data with that of available standards and references. This method can be applied to routine analysis in quality control of both bulk drugs and commercial tablets. Separation of all these compounds was performed on a Phenomenex Luna Phenyl-Hexyl (100mm×4.6mm, 5?m) analytical column. The mobile phase-A consists of acetonitrile-water (pH adjusted to 4.0 with phosphoric acid)-methanol at 15:75:10 (v/v/v), and mobile phase-B contains acetonitrile. The eluted compounds were monitored at 210nm. Ezetimibe was subjected to hydrolytic, acid, base, oxidative, photolytic and thermal stress conditions as per ICH serves to generate degradation products that can be used as a worst case to assess the analytical method performance. The drug showed extensive degradation in thermal, acid, oxidative, base and hydrolytic stress conditions, while it was stable to photolytic degradation conditions. The main degradation product formed under thermal, acid, oxidative, base and hydrolytic stress conditions corresponding to (2R,3R,6S)-N, 6-bis(4-fluorophenyl)-2-(4-hydroxyphenyl)-oxane-3-carboxamide (Ezetimibe tetrahydropyran impurity) was characterized by LC-MS/MS analysis. The degradation products were well resolved from the main peak and its impurities, thus proved the stability-indicating power of the method. The developed method was validated as per international conference on harmonization (ICH) guidelines with respect to specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision and robustness. PMID:25882410

  17. Unique variability of tocopherol composition in various seed oils recovered from by-products of apple industry: rapid and simple determination of all four homologues (?, ?, ? and ?) by RP-HPLC/FLD.

    PubMed

    Górna?, Pawe?

    2015-04-01

    The tocochromanol profile was studied in seed oils recovered from by-products of fruit industry, five dessert and seven crab apple varieties grown in Eastern Europe (Latvia). The seed oils obtained from dessert apples were characterized by higher contents of tocopherols (191.05-379.08 mg/100g oil) when compared to seed oils recovered from crab apples (130.55-202.54 mg/100g oil). The predominant homologues of tocopherol in all the studied samples were ? and ? over ? and ?. However, seed oils recovered from the apple cultivars 'Antej' and 'Beforest' had a unique profile of four tocopherol homologues (?:?:?:?) 91.41:80.55:72.46:79.03 and 114.55:112.84:78.69:73.00 mg/100g oil, respectively. A single dilution of seed oils in 2-propanol facilitated the direct use samples in the DPPH assay as well as injection into the RP-HPLC system containing a PFP (pentafluorophenyl) column, which resulted in a rapid separation of all four tocopherol homologues with excellent repeatability and reproducibility. PMID:25442533

  18. Simultaneous detection of tocopherols, carotenoids, and chlorophylls in vegetable oils by direct injection C 30 RP-HPLC with coulometric electrochemical array detection

    Microsoft Academic Search

    Ni Luh Puspitasari-Nienaber; Mario G. Ferruzzi; Steven J. Schwartz

    2002-01-01

    Detection and quantification of tocopherols, carotenoids, and chlorophylls in vegetable oil have been used to aid their authentication.\\u000a Their importance in influencing the oxidative stability of vegetable oils and their possible health benefits have been shown\\u000a in numerous studies. Therefore, the need for a rapid and reliable analysis method has become increasingly important. This\\u000a study demonstrates the application of C30

  19. Development and validation of a stability-indicating high-performance liquid chromatographic assay for ketoprofen topical penetrating gel.

    PubMed

    Bempong, Daniel K; Bhattacharyya, Lokesh

    2005-05-01

    An isocratic RP-HPLC procedure has been developed and validated for the quantitative determination of ketoprofen in a topical gel. The HPLC procedure consist of a YMC ODS-AQ, 5-microm particle size analytical column (150 mm x 4.6 mm); Alltech Econosphere C18, 5-microm particle size guard column; detection at 233 nm; 1 ml/min flow rate; 20-microl injection volume. The mobile phase consisted of pH 3.5 phosphate buffer-water-acetonitrile (8:43:49, v/v). Sample preparation was a simple extraction of ketoprofen with mobile phase. The above conditions resolved and eluted ketoprofen, excipients, and potential degradants within 35 min, with ketoprofen eluting at about 6.5 min. The procedure was validated with respect to specificity, accuracy, precision, and linearity. The accuracy of the procedure, determined by spike recovery measurements, was 100.1-100.5%. The intra- and inter-day precisions were demonstrated by the relative standard deviations (RSD) of 0.3-0.6% and 0.5%, respectively. The intermediate precision was determined by comparing the results obtained with four independently prepared samples by two chemists using two columns on different days. The results indicate no significant difference (P = 0.17). The procedure showed linearity over the concentration range 4 x 10(-5) to 1 x 10(-1) mg/ml. PMID:15909539

  20. Microwave-assisted extraction of herbacetin diglucoside from flax (Linum usitatissimum L.) seed cakes and its quantification using an RP-HPLC-UV system.

    PubMed

    Fliniaux, Ophélie; Corbin, Cyrielle; Ramsay, Aina; Renouard, Sullivan; Beejmohun, Vickram; Doussot, Joël; Falguières, Annie; Ferroud, Clotilde; Lamblin, Frédéric; Lainé, Eric; Roscher, Albrecht; Grand, Eric; Mesnard, François; Hano, Christophe

    2014-01-01

    Flax (Linum usitatissimum L.) seeds are widely used for oil extraction and the cold-pressed flaxseed (or linseed) cakes obtained during this process constitute a valuable by-product. The flavonol herbacetin diglucoside (HDG) has been previously reported as a constituent of the flaxseed lignan macromolecule linked through ester bonds to the linker molecule hydroxymethylglutaric acid. In this context, the development and validation of a new approach using microwave-assisted extraction (MAE) of HDG from flaxseed cakes followed by quantification with a reverse-phase HPLC system with UV detection was purposed. The experimental parameters affecting the HDG extraction yield, such as microwave power, extraction time and sodium hydroxide concentration, from the lignan macromolecule were optimized. A maximum HDG concentration of 5.76 mg/g DW in flaxseed cakes was measured following an irradiation time of 6 min, for a microwave power of 150 W using a direct extraction in 0.1 M NaOH in 70% (v/v) aqueous methanol. The optimized method was proven to be rapid and reliable in terms of precision, repeatability, stability and accuracy for the extraction of HDG. Comparison with a conventional extraction method demonstrated that MAE is more effective and less time-consuming. PMID:24619301

  1. Simultaneous determination of cefdinir and cefixime in human plasma by RP-HPLC/UV detection method: Method development, optimization, validation, and its application to a pharmacokinetic study.

    PubMed

    Khan, Abbas; Iqbal, Zafar; Khan, Muhammad Imran; Javed, Khalid; Khan, Abad; Ahmad, Lateef; Shah, Yasar; Nasir, Fazli

    2011-08-15

    A novel isocratic reversed-phase high performance liquid-chromatography/ultraviolet detection method for simultaneous determination of cefdinir and cefixime in human plasma was developed and validated after optimization of various chromatographic conditions and other experimental parameters. Sample preparation based on a simple extraction procedure consisting of deproteination and extraction with 3 parts of 6% trichloroacetic acid aqueous solution followed by volume make up with the aqueous component of the mobile phase obtained best recoveries of the two analytes. Samples were separated on a Supelco Discovery HS C(18) (150 mm × 4.6 mm, 5 ?m) analytical column protected by a Perkin Elmer C(18) (30 mm × 4.6 mm, 10 ?m) guard cartridge. The mobile phase, methanol/acetonitrile (50/50, v/v):0.05% trifluoroacetic acid (19:81, v/v), operated at 50°C column oven temperature was pumped at a flow rate of 2.0 mL min(-1) and the column eluents were monitored at a wavelength of 285 nm. When Sample was injected into the Perkin Elmer high performance liquid-chromatography system through Rheodyne manual (or auto-sampler) injector equipped with 20 ?L loop, separation was achieved within 4 min. The present method demonstrated acceptable values for selectivity, linearity within the expected concentration range (0.004-5.0 ?g mL(-1); r(2)>0.999 for both analytes), recovery (>95% for cefdinir and >96% for cefixime), precision (%RSD<2.0 for cefdinir and <2.2 for cefixime), sensitivity (limit of detection: 1 ng mL(-1) and lower limit of quantification: 4 ng mL(-1) for both analytes), stability of solutions, and robustness. The method was efficiently applied to a pharmacokinetic study in healthy volunteers. PMID:21782531

  2. Quantitative and Chemical Fingerprint Analysis for the Quality Evaluation of Receptaculum Nelumbinis by RP-HPLC Coupled with Hierarchical Clustering Analysis

    PubMed Central

    Wu, Yan-Bin; Zheng, Li-Jun; Yi, Jun; Wu, Jian-Guo; Chen, Ti-Qiang; Wu, Jin-Zhong

    2013-01-01

    A simple and reliable method of high-performance liquid chromatography with photodiode array detection (HPLC-DAD) was developed to evaluate the quality of Receptaculum Nelumbinis (dried receptacle of Nelumbo nucifera) through establishing chromatographic fingerprint and simultaneous determination of five flavonol glycosides, including hyperoside, isoquercitrin, quercetin-3-O-?-d-glucuronide, isorhamnetin-3-O-?-d-galactoside and syringetin-3-O-?-d-glucoside. In quantitative analysis, the five components showed good regression (R > 0.9998) within linear ranges, and their recoveries were in the range of 98.31%–100.32%. In the chromatographic fingerprint, twelve peaks were selected as the characteristic peaks to assess the similarities of different samples collected from different origins in China according to the State Food and Drug Administration (SFDA) requirements. Furthermore, hierarchical cluster analysis (HCA) was also applied to evaluate the variation of chemical components among different sources of Receptaculum Nelumbinis in China. This study indicated that the combination of quantitative and chromatographic fingerprint analysis can be readily utilized as a quality control method for Receptaculum Nelumbinis and its related traditional Chinese medicinal preparations. PMID:23337200

  3. Reversed phase-high performance liquid chromatographic (RP-HPLC) method to measure migration of semi-volatile compound, vanillin, in ipratropium bromide inhalation solution.

    PubMed

    Conkins, D; Economou, J E; Boersma, J A; Dedhiya, M G; Hansen, G

    1999-01-01

    Ipratropium bromide, a bronchodilator, is used as an inhalation solution. Commercial ipratropium bromide solution products are packaged in low-density polyethylene (LDPE) vials, through which semivolatile compounds are reported to migrate. In this article, a specific reversed phase-high performance liquid chromatographic method to assay vanillin, a semivolatile compound, in ipratropium bromide solution is described. The method was validated for a concentration range for vanillin from 30 ng/mL to 1,600 ng/mL. Migration of vanillin was assessed in two commercial preparations, ATROVENT (ipratropium bromide) Inhalation Solution packaged in a secondary foil pouch and a generic ipratropium bromide inhalation solution packaged in a carton. Levels of vanillin detected in ATROVENT after 6 months of storage at 40 degrees C and 75% RH were below the limit of detection (11 ng/mL). Significant migration of vanillin was observed after 1 month in the generic product and reached 165 ng/mL to 999 ng/mL in three months under the same storage conditions. It is concluded that this method can be readily used to measure vanillin in commercial preparations of ipratropium bromide inhalation solution. The results strongly indicate that a protective secondary packaging material is critical in preventing migration of semivolatile compounds. This study result is in agreement with the FDA's recommendation to consider even the secondary packaging components as potential sources of contamination and the use of an overwrap (typically aluminum foil) to decrease the overall permeability. PMID:11741211

  4. Determination of Rottlerin, a Natural Protein Kinases C Inhibitor, in Pancreatic Cancer Cells and Mouse Xenografts by RP-HPLC Method

    PubMed Central

    Lu, Qing-Yi; Zhang, Lifeng; Lugea, Aurelia; Moro, Aune; Edderkaoui, Mouad; Eibl, Guido; Pandol, Stephen J.; Go, Vay-Liang W

    2014-01-01

    Rottlerin is a natural polyphenolic ketone isolated from the pericarps of Mallotus phillippinensis. In previous studies we showed that parenteral administration of rottlerin reduced tumor growth in murine xenograft models of pancreatic cancer. The aim of this study was to develop a simple and validated method for the quantitative determination of rottlerin in plasma and tumor tissues of mice fed a rottlerin diet. A xenograft model of pancreatic cancer was prepared by injection of 2×106 HPAF-II cells subcutaneously into nude mice. One week before tumor implantation, mice were randomly allocated to standard diet (AIN76A) and standard diet supplement with 0.012% rottlerin (n=6 per group). Mice were sacrificed after 6 weeks on diets. Rottlerin was extracted from the plasma and tissues using protein precipitation-extraction and analyzed by reverse-phase HPLC-DAD method. The same HPLC method was also applied to determine rottlerin levels in conditioned culture media and in cell lysates from HPAF-II cells exposed to 25 µM concentration of rottlerin. A substantial amount of rottlerin was detected in tumor (2.11 ± 0.25 nmol/g tissue) and plasma (2.88 ± 0.41 µM) in mice fed rottlerin diet. In addition, significant levels of rottlerin (57.4 ± 5.4 nmol/mg protein) were detected in cell lysates from rottlerin-treated HPAF-II cells. These data indicate that rottlerin is efficiently absorbed in cells and tissues both in vivo and in vitro and suggest a strong potential for rottlerin as a preventive or adjuvant supplement for pancreatic cancer. PMID:24482742

  5. Determination of Rottlerin, a Natural Protein Kinases C Inhibitor, in Pancreatic Cancer Cells and Mouse Xenografts by RP-HPLC Method.

    PubMed

    Lu, Qing-Yi; Zhang, Lifeng; Lugea, Aurelia; Moro, Aune; Edderkaoui, Mouad; Eibl, Guido; Pandol, Stephen J; Go, Vay-Liang W

    2013-01-01

    Rottlerin is a natural polyphenolic ketone isolated from the pericarps of Mallotus phillippinensis. In previous studies we showed that parenteral administration of rottlerin reduced tumor growth in murine xenograft models of pancreatic cancer. The aim of this study was to develop a simple and validated method for the quantitative determination of rottlerin in plasma and tumor tissues of mice fed a rottlerin diet. A xenograft model of pancreatic cancer was prepared by injection of 2×10(6) HPAF-II cells subcutaneously into nude mice. One week before tumor implantation, mice were randomly allocated to standard diet (AIN76A) and standard diet supplement with 0.012% rottlerin (n=6 per group). Mice were sacrificed after 6 weeks on diets. Rottlerin was extracted from the plasma and tissues using protein precipitation-extraction and analyzed by reverse-phase HPLC-DAD method. The same HPLC method was also applied to determine rottlerin levels in conditioned culture media and in cell lysates from HPAF-II cells exposed to 25 µM concentration of rottlerin. A substantial amount of rottlerin was detected in tumor (2.11 ± 0.25 nmol/g tissue) and plasma (2.88 ± 0.41 µM) in mice fed rottlerin diet. In addition, significant levels of rottlerin (57.4 ± 5.4 nmol/mg protein) were detected in cell lysates from rottlerin-treated HPAF-II cells. These data indicate that rottlerin is efficiently absorbed in cells and tissues both in vivo and in vitro and suggest a strong potential for rottlerin as a preventive or adjuvant supplement for pancreatic cancer. PMID:24482742

  6. The value of analytical assays that are stability-indicating.

    PubMed

    Chan, E C; Wee, P Y; Ho, P C

    1999-10-01

    It is essential to validate an assay with regards to its precision, accuracy, reproducibility, selectivity and robustness. In pharmaceutical research, in addition to these requirements, an assay is often required to be proven beyond doubt to be stability-indicating. A stability-indicating assay is one that can accurately and selectively differentiate an intact drug from its potential decomposition products. An assay that fails to meet this requirement would produce stability data that are inaccurate and misleading. This concept could be applied to other fields of research, such as clinical laboratory chemistry where accurate and reliable clinical data are imperative in the diagnosis and following-up of diseases. In this study, we employed an amperometric HPLC assay developed for the measurements of urinary catecholamines and metanephrines to illustrate the validation process of this assay with regards to its stability-indicating capacity. The implications of this study are also discussed. PMID:10529457

  7. Development of an HPLC method for measurements of the stability of Irganox-type polymer antioxidants in fatty food simulants

    Microsoft Academic Search

    P. G. Demertzis; R. Franz

    1998-01-01

    A reversed-phase high-performance liquid chromatography (RP-HPLC) method has been developed to measure the stability of four\\u000a Irganox-type polymer antioxidants (Irganox 245, Irganox 1035, Irganox 1098 and Irganox 3114) in an olive oil food simulant\\u000a and isooctane, which has been proposed as an alternative fatty food simulant. The tests of stability in olive oil were carried\\u000a out under three different conditions,

  8. Degradation Study on Sulfasalazine and a Validated HPLC-UV Method for its Stability Testing

    PubMed Central

    Saini, Balraj; Bansal, Gulshan

    2014-01-01

    Sulfasalazine (SSZ) was subjected to degradation under the conditions of hydrolysis (acid, alkali, and water), oxidation (30% H2O2), dry heat, and photolysis (UV-VIS light) in accordance with the ICH guidelines. An RP-HPLC method was developed to study the degradation behavior. No degradation was noted under any condition except alkaline hydrolysis where SSZ was degraded to a single minor product. SSZ was optimally resolved from this product on an XTerra® RP18 column with a mobile phase composed of methanol and an ammonium acetate buffer (10 mM, pH 7.0) (48:52, v/v) delivered at a rate of 0.8 mL/min in an isocratic mode. The method was validated and found to be linear (r2=0.99945), precise (%RSD <2), robust, and accurate (94–102%) in the concentration range of 0.5–50 ?g/mL of SSZ. The PDA analysis of the degraded sample revealed the SSZ peak purity to be 998.99 and the drug peak eluted with a resolution factor of >2 from the nearest resolving peak, indicating the method to be selectively stability-indicating for the drug analysis. The method was applied successfully for the stability testing of the commercially available SSZ tablets that were under varied ICH-prescribed conditions. An explanation for the unusual stability of the drug when exposed to acidic hydrolysis, despite the presence of the sulfonamide linkage, is also discussed. PMID:24959403

  9. The IDV and IHV Indices: Derivation and Stability

    NASA Astrophysics Data System (ADS)

    Svalgaard, L.

    2008-05-01

    We review the recently introduced geomagnetic activity indices: IDV (InterDiurnal Variability) and IHV (InterHourly Variability). Their salient features are the use of night-time data only to cleanly avoid the effect of the daily 'quiet- time' variation and the use of only hourly values of the magnetic elements. Since the two indices have different dependencies on interplanetary magnetic field strength (B) and solar wind speed (V), they can be used to deduce B and V separately affording us a way of estimating solar wind properties in the past ~180 years. In addition, they provide a valuable check on the calibration of other long-term indices, e.g. the aa-index, which has been found in need of a recalibration. We discuss the physical meaning of the indices, e.g. show that IHV is directly proportional to the power input to the ionosphere [POES Hp-index]. We discuss the construction and stability with time of the indices and the several pitfalls to avoid.

  10. Development of stability-indicating methods for cefquinome sulphate.

    PubMed

    Shantier, Shaza W; Gadkariem, Elrasheed A; Adam, Mohamed O; Mohamed, Magdi A

    2013-09-01

    The degradation behavior of cefquinome sulphate in alkaline medium at different temperatures was investigated using both first derivative spectrophotometric and HPLC methods. The drug degradation was found to be pH and temperature dependant. The pH-rate profile indicated a first order dependence of Kobs on [OH(-)] at pHs ranging between 9 and 11. Arrhenius plot obtained at pH 10 was linear between 65° and 100°C. The estimated activation energy of the hydrolysis was found to be 21.1 kcal mol(-1). Stability-indicating thin-layer chromatographic method for the separation of the drug and its alkaline hydrolysis product has been developed. PMID:24170991

  11. Development of Stability-Indicating Methods for Cefquinome Sulphate

    PubMed Central

    Shantier, Shaza W.; Gadkariem, Elrasheed A.; Adam, Mohamed O.; Mohamed, Magdi A.

    2013-01-01

    The degradation behavior of cefquinome sulphate in alkaline medium at different temperatures was investigated using both first derivative spectrophotometric and HPLC methods. The drug degradation was found to be pH and temperature dependant. The pH-rate profile indicated a first order dependence of Kobs on [OH-] at pHs ranging between 9 and 11. Arrhenius plot obtained at pH 10 was linear between 65° and 100°C. The estimated activation energy of the hydrolysis was found to be 21.1 kcal mol-1. Stability-indicating thin-layer chromatographic method for the separation of the drug and its alkaline hydrolysis product has been developed. PMID:24170991

  12. Stability-Indicating HPLC Determination of Gemcitabine in Pharmaceutical Formulations

    PubMed Central

    Singh, Rahul; Shakya, Ashok K.; Naik, Rajashri; Shalan, Naeem

    2015-01-01

    A simple, sensitive, inexpensive, and rapid stability indicating high performance liquid chromatographic method has been developed for determination of gemcitabine in injectable dosage forms using theophylline as internal standard. Chromatographic separation was achieved on a Phenomenex Luna C-18 column (250?mm × 4.6?mm; 5?) with a mobile phase consisting of 90% water and 10% acetonitrile (pH 7.00 ± 0.05). The signals of gemcitabine and theophylline were recorded at 275?nm. Calibration curves were linear in the concentration range of 0.5–50??g/mL. The correlation coefficient was 0.999 or higher. The limit of detection and limit of quantitation were 0.1498 and 0.4541??g/mL, respectively. The inter- and intraday precision were less than 2%. Accuracy of the method ranged from 100.2% to 100.4%. Stability studies indicate that the drug was stable to sunlight and UV light. The drug gives 6 different hydrolytic products under alkaline stress and 3 in acidic condition. Aqueous and oxidative stress conditions also degrade the drug. Degradation was higher in the alkaline condition compared to other stress conditions. The robustness of the methods was evaluated using design of experiments. Validation reveals that the proposed method is specific, accurate, precise, reliable, robust, reproducible, and suitable for the quantitative analysis. PMID:25838825

  13. A stability-indicating HPLC assay for metronidazole benzoate.

    PubMed

    Bempong, Daniel K; Manning, Ronald G; Mirza, Tahseen; Bhattacharyya, Lokesh

    2005-07-15

    A simple and rapid stability-indicating HPLC assay procedure has been developed and validated for metronidazole benzoate. The HPLC conditions were as follows, column: Waters Symmetry C8, 5 microm packing, 4.6 mm x 250 mm; detection: UV at 271 nm; injection volume: 20 microl; mobile phase: acetonitrile-0.1% glacial acetic acid in monobasic potassium phosphate (0.01 M) (40:60, v/v); isocratic elution under ambient temperature at 2.0 ml min(-1). The procedure separated metronidazole benzoate and its potential degradation products, metronidazole and benzoic acid, in an overall analysis time of about 6 min with metronidazole benzoate eluting at about 5 min. The injection repeatability was 0.03%, and the intraday and interday repeatability were 0.4 and 0.7%, respectively. The procedure provided a linear response over the concentration range 0.2-800 microg ml(-1) (r=1.0000) with the limits of detection and quantitation 0.03 and 0.2 microg ml(-1), respectively. The solubilities of metronidazole benzoate in water, 0.01 M hydrochloric acid and 0.05 M phosphate buffer, pH 6.8, determined each in triplicate using the procedure, were 0.2 mg ml(-1) (R.S.D. 7%), 0.4 mg ml(-1) (R.S.D. 2%) and 0.2 mg ml(-1) (R.S.D. 8%), respectively. The results show no detectable hydrolysis of metronidazole benzoate in 0.01 M hydrochloric acid at 37 degrees C or in the mobile phase at ambient temperature in 10 h. PMID:15967308

  14. Development of new method for simultaneous analysis of piracetam and levetiracetam in pharmaceuticals and biological fluids: application in stability studies.

    PubMed

    Siddiqui, Farhan Ahmed; Sher, Nawab; Shafi, Nighat; Wafa Sial, Alisha; Ahmad, Mansoor; Mehjebeen; Naseem, Huma

    2014-01-01

    RP-HPLC ultraviolet detection simultaneous quantification of piracetam and levetiracetam has been developed and validated. The chromatography was obtained on a Nucleosil C18 column of 25?cm×0.46?cm, 10??m, dimension. The mobile phase was a (70:30?v/v) mixture of 0.1?g/L of triethylamine and acetonitrile. Smooth flow of mobile phase at 1?mL/min was set and 205?nm wavelength was selected. Results were evaluated through statistical parameters which qualify the method reproducibility and selectivity for the quantification of piracetam, levetiracetam, and their impurities hence proving stability-indicating properties. The proposed method is significantly important, permitting the separation of the main constituent piracetam from levetiracetam. Linear behavior was observed between 20?ng/mL and 10,000?ng/mL for both drugs. The proposed method was checked in bulk drugs, dosage formulations, physiological condition, and clinical investigations and excellent outcome was witnessed. PMID:25114921

  15. Herring gull eggs indicate stabilizing Great Lakes PCB concentrations

    SciTech Connect

    Stow, C. [Univ. of Wisconsin, Madison, WI (United States). Center for Limnology

    1995-12-31

    The author evaluated the fit of 3 alternative models to herring gull (Larus argentatus) egg PCB concentration data from 1978--1992 to examine whether PCB levels were decreasing or had ceased to decline. The best fit models indicate that, following initial declines, no discernible PCB decreases are occurring in 4 of the 5 lakes. Only Lake Erie indicates a continued PCB decline, though the Erie data may be too noisy to differentiate model fits. These results are consistent with previous analyses indicating stable PCB concentrations in Lake Michigan fishes and suggest that further improvements may be too slow to be of practical importance from a management perspective.

  16. The Stability of School Effectiveness Indices across Years.

    ERIC Educational Resources Information Center

    Mandeville, Garrett K.

    School effectiveness indices (SEIs) based on residuals from regressing test performance in reading and mathematics onto prior-year test performance and a socioeconomic status measure (percentage eligible for a subsidized lunch program) were obtained for two consecutive years for 431 South Carolina elementary schools. The analysis involved school…

  17. Environmental stability of PAH source indices in pyrogenic tars

    SciTech Connect

    Uhler, A.D.; Emsbo-Mattingly, S.D. [New Fields Environmental Forensics Practice, Rockland, MA (United States)

    2006-04-15

    Polycyclic aromatic hydrocarbons (PAHs) are widespread environmental contaminants found in soil, sediments, and airborne particulates. The majority of PAHs found in modern soils and sediments arise from myriad anthropogenic petrogenic and pyrogenic sources. Tars and tar products such as creosote produced from the industrial pyrolysis of coal or oil at former manufactured gas plants (MGPs) or in coking retorts are viscous, oily substances that contain significant concentrations of PAH, usually in excess of 30% w/w. Pyrogenic tars and tar products have unique PAH patterns (source signatures) that are a function of their industrial production. Among pyrogenic materials, certain diagnostic ratios of environmentally recalcitrant 4-, 5- and 6-ring PAHs have been identified as useful environmental markers for tracking the signature of tars and petroleum in the environment. The use of selected PAH source ratios is based on the concept that PAHs with similar properties (i.e., molecular weight, partial pressure, solubility, partition coefficients, and biotic/abiotic degradation) will weather at similar rates in the environment thereby yielding stable ratios. The stability of more than 30 high molecular weight PAH ratios is evaluated during controlled studies of tar evaporation and aerobic biodegradation. The starting materials in these experiments consisted of relatively unweathered tars derived from coal and petroleum, respectively. The PAH ratios from these laboratory studies are compared to those measured in PAH residues found in tar-contaminated soils at a former MGP that operated with a carburetted water gas process.

  18. RP-HPLC Estimation of Ramipril and Telmisartan in Tablets

    PubMed Central

    Kurade, V. P.; Pai, M. G.; Gude, R.

    2009-01-01

    A rapid high performance liquid chromatographic method has been developed and validated for the estimation of ramipril and telmisartan simultaneously in combined dosage form. A Genesis C18 column having dimensions of 4.6×250 mm and particle size of 5 ?m in isocratic mode, with mobile phase containing a mixture of 0.01 M potassium dihydrogen phosphate buffer (adjusted to pH 3.4 using orthophosphoric acid): methanol:acetonitrile (15:15:70 v/v/v) was used. The mobile phase was pumped at a flow rate of 1.0 ml/min and the eluents were monitored at 210 nm. The selected chromatographic conditions were found to effectively separate ramipril (Rt: 3.68 min) and telmisartan (Rt: 4.98 min) having a resolution of 3.84. The method was validated in terms of linearity, accuracy, precision, specificity, limit of detection and limit of quantitation. Linearity for ramipril and telmisartan were found in the range of 3.5-6.5 ?g/ml and 28.0-52.0 ?g/ml, respectively. The percentage recoveries for ramipril and telmisartan ranged from 99.09-101.64% and 99.45-100.99%, respectively. The limit of detection and the limit of quantitation for ramipril was found to be 0.5 ?g/ml and 1.5 ?g/ml respectively and for telmisartan was found to be 1.5 ?g/ml and 3.0 ?g/ml, respectively. The method was found to be robust and can be successfully used to determine the drug content of marketed formulations. PMID:20336215

  19. RP-HPLC Estimation of Ramipril and Telmisartan in Tablets.

    PubMed

    Kurade, V P; Pai, M G; Gude, R

    2009-03-01

    A rapid high performance liquid chromatographic method has been developed and validated for the estimation of ramipril and telmisartan simultaneously in combined dosage form. A Genesis C18 column having dimensions of 4.6x250 mm and particle size of 5 mum in isocratic mode, with mobile phase containing a mixture of 0.01 M potassium dihydrogen phosphate buffer (adjusted to pH 3.4 using orthophosphoric acid): methanol:acetonitrile (15:15:70 v/v/v) was used. The mobile phase was pumped at a flow rate of 1.0 ml/min and the eluents were monitored at 210 nm. The selected chromatographic conditions were found to effectively separate ramipril (R(t): 3.68 min) and telmisartan (R(t): 4.98 min) having a resolution of 3.84. The method was validated in terms of linearity, accuracy, precision, specificity, limit of detection and limit of quantitation. Linearity for ramipril and telmisartan were found in the range of 3.5-6.5 mug/ml and 28.0-52.0 mug/ml, respectively. The percentage recoveries for ramipril and telmisartan ranged from 99.09-101.64% and 99.45-100.99%, respectively. The limit of detection and the limit of quantitation for ramipril was found to be 0.5 mug/ml and 1.5 mug/ml respectively and for telmisartan was found to be 1.5 mug/ml and 3.0 mug/ml, respectively. The method was found to be robust and can be successfully used to determine the drug content of marketed formulations. PMID:20336215

  20. Simultaneous Estimation of Nebivolol Hydrochloride and Valsartan using RP HPLC.

    PubMed

    Kokil, S U; Bhatia, M S

    2009-03-01

    In this study, a rapid, precise, accurate, specific and sensitive ion-paired reverse phase liquid chromatographic method has been developed for the simultaneous estimation of nebivolol hydrochloride and valsartan in their capsule formulation. The chromatographic method was standardized using a HIQ sil C(18) column (250x4.6 mm i.d., 5 mum particle size) with UV detection at 289 nm and flow rate of 1 ml/min. The mobile phase consisting of methanol:water (80:20 v/v) with addition of 0.1 percent 1-hexanesulfonic acid monohydrate sodium salt as an ion-pairing reagent was selected. The method was validated and produced accurate and precise results for estimation of the two drugs. PMID:20336202

  1. Simultaneous Estimation of Nebivolol Hydrochloride and Valsartan using RP HPLC

    PubMed Central

    Kokil, S. U.; Bhatia, M. S.

    2009-01-01

    In this study, a rapid, precise, accurate, specific and sensitive ion-paired reverse phase liquid chromatographic method has been developed for the simultaneous estimation of nebivolol hydrochloride and valsartan in their capsule formulation. The chromatographic method was standardized using a HIQ sil C18 column (250×4.6 mm i.d., 5 ?m particle size) with UV detection at 289 nm and flow rate of 1 ml/min. The mobile phase consisting of methanol:water (80:20 v/v) with addition of 0.1 percent 1-hexanesulfonic acid monohydrate sodium salt as an ion-pairing reagent was selected. The method was validated and produced accurate and precise results for estimation of the two drugs. PMID:20336202

  2. Two Approaches to Examining the Stability of Myers-Briggs Type Indicator Scores

    ERIC Educational Resources Information Center

    Salter, Daniel W.; Forney, Deanna S.; Evans, Nancy J.

    2005-01-01

    In this study, two approaches are used to assess the stability of Myers-Briggs Type Indicator scores across 3 administrations (N = 231): longitudinal configural frequency analysis with categorical scores and generalizability theory with the Preference Clarity Indices and continuous scores. The results are generally positive. Evaluation of…

  3. Kinetics of ?-Globin Binding to ?-Hemoglobin Stabilizing Protein (AHSP) Indicate Preferential Stabilization of Hemichrome Folding Intermediate*

    PubMed Central

    Mollan, Todd L.; Khandros, Eugene; Weiss, Mitchell J.; Olson, John S.

    2012-01-01

    Human ?-hemoglobin stabilizing protein (AHSP) is a conserved mammalian erythroid protein that facilitates the production of Hemoglobin A by stabilizing free ?-globin. AHSP rapidly binds to ferrous ? with association (k?AHSP) and dissociation (kAHSP) rate constants of ?10 ?m?1 s?1 and 0.2 s?1, respectively, at pH 7.4 at 22 °C. A small slow phase was observed when AHSP binds to excess ferrous ?CO. This slow phase appears to be due to cis to trans prolyl isomerization of the Asp29-Pro30 peptide bond in wild-type AHSP because it was absent when ?CO was mixed with P30A and P30W AHSP, which are fixed in the trans conformation. This slow phase was also absent when met(Fe3+)-? reacted with wild-type AHSP, suggesting that met-? is capable of rapidly binding to either Pro30 conformer. Both wild-type and Pro30-substituted AHSPs drive the formation of a met-? hemichrome conformation following binding to either met- or oxy(Fe2+)-?. The dissociation rate of the met-?·AHSP complex (kAHSP ? 0.002 s?1) is ?100-fold slower than that for ferrous ?·AHSP complexes, resulting in a much higher affinity of AHSP for met-?. Thus, in vivo, AHSP acts as a molecular chaperone by rapidly binding and stabilizing met-? hemichrome folding intermediates. The low rate of met-? dissociation also allows AHSP to have a quality control function by kinetically trapping ferric ? and preventing its incorporation into less stable mixed valence Hemoglobin A tetramers. Reduction of AHSP-bound met-? allows more rapid release to ? subunits to form stable fully, reduced hemoglobin dimers and tetramers. PMID:22298770

  4. Respiration and enzymatic activities as indicators of stabilization of sewage sludge composting.

    PubMed

    Nikaeen, Mahnaz; Nafez, Amir Hossein; Bina, Bijan; Nabavi, BiBi Fatemeh; Hassanzadeh, Akbar

    2015-05-01

    The objective of this work was to study the evolution of physico-chemical and microbial parameters in the composting process of sewage sludge (SS) with pruning wastes (PW) in order to compare these parameters with respect to their applicability in the evaluation of organic matter (OM) stabilization. To evaluate the composting process and organic matter stability, different microbial activities were compared during composting of anaerobically digested SS with two volumetric ratios, 1:1 and 3:1 of PW:SS and two aeration techniques including aerated static piles (ASP) and turned windrows (TW). Dehydrogenase activity, fluorescein diacetate hydrolysis, and specific oxygen uptake rate (SOUR) were used as microbial activity indices. These indices were compared with traditional parameters, including temperature, pH, moisture content, organic matter, and C/N ratio. The results showed that the TW method and 3:1 (PW:SS) proportion was superior to the ASP method and 1:1 proportion, since the former accelerate the composting process by catalyzing the OM stabilization. Enzymatic activities and SOUR, which reflect microbial activity, correlated well with temperature fluctuations. Based on these results it appears that SOUR and the enzymatic activities are useful parameters to monitor the stabilization of SS compost. PMID:25728091

  5. A validated stability indicating HPTLC method for simultaneous estimation of irbesartan and hydrochlorothiazide

    PubMed Central

    Khodke, Amol S; Potale, Laxman V; Damle, Mrinalini C; Bothara, Kailash G

    2010-01-01

    Introduction: Irbesartan, a diazaspiro angiotensin II blocker, is marketed in combination with Hydrochlorothiazide, which is a diuretic acting on distal convoluted tubule; for synergistic anti-hypertensive action. The present study deals with development and validation of a stability indicating HPTLC method for simultaneous estimation of Irbesartan and Hydrochlorothiazide using TLC plates precoated with Silica gel 60F254 and the mobile phase comprising Acetonitrile: Chloroform in the ratio of 5:6 v/v. Irbesartan and Hydrochlorothiazide were well resolved with Rf 0.27 ± 0.03 and 0.45 ± 0.03, respectively. Wavelength selected for the quantization was 270 nm. Inherent stability of these drugs was studied by exposing both drugs to various stress conditions as per ICH guidelines viz. Dry heat, oxidative, photolysis (UV and cool white fluorescent light) and hydrolytic conditions under different pH values. Results: Both the drugs were not degraded under dry heat and photolytic conditions, but showed degradation under hydrolytic condition. The degraded products of Irbesartan and hydrochlorothiazide were well resolved from the individual bulk drug response. Conclusion: The developed method is found to be simple, specific, precise and stability indicating. The specificity of the method was confirmed by peak purity profile of the resolved peaks. PMID:23781414

  6. Stability-indicating LC method for the simultaneous determination of lisinopril and hydrochlorothiazide.

    PubMed

    de Diego, Marta; Soto, Jorge; Mennickent, Sigrid

    2014-01-01

    A simple and rapid stability-indicating liquid chromatographic method was developed and validated for the simultaneous determination of lisinopril and hydrochlorotiazide (HCTZ) in drug substances and dosage forms in the presence of degradation products. Forced degradation studies were conducted on the pure drugs under hydrolytic, oxidative, thermal and photolytic conditions. A chromatographic separation of the two drugs and its degradation products was achieved with an RP-18 column, using methanol, acetonitrile and phosphate buffer (pH 7.1; 0.05 M) (15:15:70, v/v/v) as mobile phase at a flow rate of 0.8 mL min(-1) and UV detection at 210 nm. Lisinopril and HCTZ were well resolved from its degradation products showing the stability-indicating capability of the method. The described method was linear over a range of 40-200 µg mL(-1) for lisinopril and 25-175 µg mL(-1) for HCTZ. The assay was also selective, accurate and precise for lisinopril and HCTZ determination. This method represents an alternative to the United States Pharmacopeia (USP) method showing shorter retention time. The method was successfully applied for determination of lisinopril and HCTZ in combined commercial tablets. The results showed that the proposed method was found to be suitable for quantitative determination and the stability study of lisinopril and HCTZ in pharmaceutical samples. PMID:24297524

  7. Soil aggregate stability as an indicator for eco-engineering effectiveness?

    NASA Astrophysics Data System (ADS)

    Graf, Frank

    2015-04-01

    Eco-engineering aims at stabilising soil and slopes by applying technical and biological measures. Engineering structures are commonly well defined, immediately usable and operative, and their stability effects quantifiable and verifiable. Differently, the use of plants requires more restrictive boundary conditions and the protection potential is rarely easily calculable and develop-ing as a function of growth rate. Although the use of vegetation is widely appreciated and their stabilising effect recognised, there is an increasing demand on sound facts on its efficiency, in particular, in relation to time. Conclusively, a certain necessity has been recognised to monitor, assess and quantify the effectiveness of ecological restora-tion measures in order to facilitate the transfer of technology and knowledge. Recent theoretical models emphasize the im-portance of taking an integrated monitoring approach that considers multiple variables. However, limited financial and time resources often prevent such comprehensive assessments. A solution to this problem may be to use integrated indicators that reflect multiple aspects and, therefore, allow extensive information on ecosystem status to be gathered in a relatively short time. Among various other indicators, such as fractal dimension of soil particle size distribution or microbiological parameters, soil aggregate stability seems the most appropriate indicator with regard to protecting slopes from superficial soil failure as it is critical to both plant growth and soil structure. Soil aggregation processes play a crucial role in re-establishing soil structure and function and, conclusively, for successful and sustainable re-colonisation. Whereas the key role of soil aggregate stability in ecosystem functioning is well known concerning water, gas, and nutrient fluxes, only limited information is available with regard to soil mechanical and geotechnical aspects. Correspondingly, in the last couple of years several studies have been performed in order to bridge this gap addressing partic-ularly the influence of root growth and mycorrhizal fungi on the resistance of soil aggregates against disintegration and linking it to slope stability. As superficial soil failure is often related to heavy rainstorms and, in this regard, mainly due to water satura-tion, recent investigations focused on the pore water pressure, too. Summarising main results of the different studies a positive relationship between soil aggregate stability and traditional soil mechanical shear strength parameters was found, e.g. given certain soil conditions, an increase in aggregate stability may be equated to an increase of the angle of internal friction ?' and/or cohesion c'. In addition, almost all investigations showed a strong positive correlation between root length per soil volume and soil aggregate stability. In respect of mycorrhizal fungi, results are not yet as clear. On the one hand it was found that the use of unspecific (commercial) inoculum had no or even a negative effect on root growth within the first vegetation period and, correspondingly, on soil aggregate stability. However, the use of specific plant fungi combinations almost ever resulted in an obvious acceleration of root growth immediately with con-comitant gain of soil stability. As far as pore water pressure is concerned we did not yet find an interpretation that is fairly straightforward and not overly prone to controversy. It looks like soil aggregated by mycorrhized plants does have a higher capacity for building up pressure than such permeated by non-mycorrhized roots. Within this scope results of several studies showing these (inter-) relationships and correlations are presented and differences as well as unexpected results discussed.

  8. Evaluation of the stability indices for the thunderstorm forecasting in the region of Belgrade, Serbia

    NASA Astrophysics Data System (ADS)

    Vujovi?, D.; Paskota, M.; Todorovi?, N.; Vu?kovi?, V.

    2015-07-01

    The pre-convective atmosphere over Serbia during the ten-year period (2001-2010) was investigated using the radiosonde data from one meteorological station and the thunderstorm observations from thirteen SYNOP meteorological stations. In order to verify their ability to forecast a thunderstorm, several stability indices were examined. Rank sum scores (RSSs) were used to segregate indices and parameters which can differentiate between a thunderstorm and no-thunderstorm event. The following indices had the best RSS values: Lifted index (LI), K index (KI), Showalter index (SI), Boyden index (BI), Total totals (TT), dew-point temperature and mixing ratio. The threshold value test was used in order to determine the appropriate threshold values for these variables. The threshold with the best skill scores was chosen as the optimal. The thresholds were validated in two ways: through the control data set, and comparing the calculated indices thresholds with the values of indices for a randomly chosen day with an observed thunderstorm. The index with the highest skill for thunderstorm forecasting was LI, and then SI, KI and TT. The BI had the poorest skill scores.

  9. PrimeSupplier Cross-Program Impact Analysis and Supplier Stability Indicator Simulation Model

    NASA Technical Reports Server (NTRS)

    Calluzzi, Michael

    2009-01-01

    PrimeSupplier, a supplier cross-program and element-impact simulation model, with supplier solvency indicator (SSI), has been developed so that the shuttle program can see early indicators of supplier and product line stability, while identifying the various elements and/or programs that have a particular supplier or product designed into the system. The model calculates two categories of benchmarks to determine the SSI, with one category focusing on agency programmatic data and the other focusing on a supplier's financial liquidity. PrimeSupplier was developed to help NASA smoothly transition design, manufacturing, and repair operations from the Shuttle program to the Constellation program, without disruption in the industrial supply base.

  10. Stability-Indicating HPLC Determination of Trandolapril in Bulk Drug and Pharmaceutical Dosage Forms

    PubMed Central

    Al-Hawash, Leena A.; Shakya, Ashok K.; Saleem, Maher L.

    2015-01-01

    A rapid, simple, accurate, precise, economical, robust, and stability indicating reverse phase HPLC-PDA procedure has been developed and validated for the determination of trandolapril. The trandolapril was separated isocratically on Hypersil-Gold C18 column (250?mm × 4.6?mm, 5??m) with a mobile phase consisting of 50% acetonitrile and 50% water (containing 0.025% triethylamine, pH 3.0 ± 0.1), at 25 ± 2°C. Retention time of the drug was ~4.6?min. The eluted compounds were monitored and identified at 210?nm. The linearity of the method was excellent (r2 > 0.9999) over the concentration range of 1–24??g/mL; the limit of detection (LOD) and limit of quantitation (LOQ) were 0.0566??g/mL and 0.1715??g/mL, respectively. The overall precision was less than 2%. Mean recovery of trandolapril was more than 99%; no interference was found from the component present in the preparation. Stability studies indicate that the drug was stable to sunlight and UV light. The drug gives 6 different oxidative products on exposure to hydrogen peroxide. Slight degradation was observed in acidic condition. Degradation was higher in the alkaline condition compared to other conditions. The robustness of the method was studied using factorial design experiment. PMID:25802524

  11. Indication.

    PubMed

    Pust, Ronald E

    2012-01-01

    Should the indications for therapies differ from one nation to the next? What are the reasons behind controversial therapeutic variations? What roles do cultural history and authoritarian conflict among clinicians play in the adoption of therapies? When I worked at a rural hospital in Kenya, a woman experiencing obstructed labor made me ponder many questions-but only after our emergency ended in the death of her newborn son. In recounting and learning from this episode, I listened to the disparate Kenyan voices of the patient, the hospital's director, the consultant obstetrician, and to the even more controversial voices of evidence-based medicine. In reflecting on this process, I have learned at least 3 lessons-about the transmissibility of arrogance, the role of guests in other countries, and the nature of science. PMID:22230834

  12. Indication

    PubMed Central

    Pust, Ronald E.

    2012-01-01

    Should the indications for therapies differ from one nation to the next? What are the reasons behind controversial therapeutic variations? What roles do cultural history and authoritarian conflict among clinicians play in the adoption of therapies? When I worked at a rural hospital in Kenya, a woman experiencing obstructed labor made me ponder many questions—but only after our emergency ended in the death of her newborn son. In recounting and learning from this episode, I listened to the disparate Kenyan voices of the patient, the hospital’s director, the consultant obstetrician, and to the even more controversial voices of evidence-based medicine. In reflecting on this process, I have learned at least 3 lessons—about the transmissibility of arrogance, the role of guests in other countries, and the nature of science. PMID:22230834

  13. Stability Indicating Liquid Chromatographic Method for the Simultaneous Determination of Rosuvastatin and Ezetimibe in Pharmaceutical Formulations

    PubMed Central

    Mukthinuthalapati, Mathrusri Annapurna; Bukkapatnam, Venkatesh; Bandaru, Sai Pavan Kumar

    2014-01-01

    Purpose: A simple stability indicating reverse phase liquid chromatographic method was developed for the simultaneous determination of rosuvastatin and ezetimibe in pharmaceutical formulations. Methods: Best chromatographic response was achieved with C18 column (250 X 4.6 mm, 5µm) with photo diode array (PDA) detector. The mobile phase was composed of a mixture of sodium acetate buffer (pH 4.0) and acetonitrile (30:70, %v/v) with a flow rate of 1.2 mL/min. (UV detection at 254 nm). Rosuvastatin and ezetimibe were subjected to stress conditions of degradation and the method was validated as per ICH guidelines. Results: The method shows linearity over a concentration range of 0.5-250 µg/ml for both rosuvastatin (r2 = 0.9993) and ezetimibe (r2 = 0.9996). Both the drugs are highly sensitive towards alkaline conditions in comparison to other stress conditions. Conclusion: The proposed method can be successfully applied to perform long-term and accelerated stability studies for the simultaneous determination of rosuvastatin and ezetimibe in pharmaceutical formulations. PMID:25436199

  14. Stability-indicating Simultaneous HPTLC Method for Olanzapine and Fluoxetine in Combined Tablet Dosage Form

    PubMed Central

    Shah, C. R.; Suhagia, B. N.; Shah, N. J.; Patel, D. R.; Patel, N. M.

    2008-01-01

    A rapid, selective and stability-indicating high performance thin layer chromatographic method was developed and validated for the simultaneous estimation of olanzapine and fluoxetine in combined tablet dosage form. Olanzapine and fluoxetine were chromatographed on silica gel 60 F254 TLC plate using methanol:toluene (4:2 v/v) as the mobile phase and spectrodensitometric scanning-integration was performed at a wavelength of 233 nm using a Camag TLC Scanner III. This system was found to give compact spots for both olanzapine (Rf value of 0.63±0.01) and fluoxetine (Rf value of 0.31±0.01). The polynomial regression data for the calibration plots showed good linear relationship with r2=0.9995 in the concentration range of 100-800 ng/spot for olanzapine and 1000-8000 ng/spot for fluoxetine with r2=0.9991. The method was validated in terms of linearity, accuracy, precision, recovery and specificity. The limit of detection and the limit of quantification for the olanzapine were found to be 30 and 100 ng/spot, respectively and for fluoxetine 300 and 1000 ng/spot, respectively. Olanzapine and fluoxetine were degraded under acidic, basic and oxidation degradation conditions which showed all the peaks of degraded product were well resolved from the active pharmaceutical ingredient. Both drugs were not further degraded after thermal and photochemical degradation. The method was found to be reproducible and selective for the simultaneous estimation of olanzapine and fluoxetine. As the method could effectively separate the drugs from their degradation products, it can be employed as a stability-indicating method. PMID:20046726

  15. Stability-indicating UPLC method for determining related substances and degradants in dronedarone.

    PubMed

    Pydimarry, Surya Prakash Rao; Cholleti, Vijay Kumar; Vangala, Ranga Reddy

    2014-08-01

    A simple, sensitive and reproducible method was developed on ultra-performance liquid chromatography coupled with photodiode array detection for the quantitative determination of dronedarone hydrochloride (DRO) in drug substance and pharmaceutical dosage forms. The method is applicable for the quantification of related substances and assays of drug substances. Chromatographic separation was achieved on Acquity UPLC BEH C8 100 mm, 2.1 mm and 1.7 µm columns, using gradient elution within a short run time of 10.0 min. The eluted compounds were monitored at 288 nm, the flow rate was 0.5 mL/min and the column oven temperature was maintained at 40°C. The resolution of DRO and 11 impurities (potentials and by-products) was greater than 2.0 for all pairs of components. The high correlation coefficient value (>0.9995) indicates the clear correlations between the concentrations of investigated compound and their peak areas within the test ranges. The repeatability and intermediate precision, expressed by the relative standard deviation, were less than 2.5%. The accuracy and validity of the method were further ascertained by performing recovery studies via a spike method. The accuracy of the method, expressed as relative error, was satisfactory. No interference was observed from concomitant substances normally added to the tablets. DRO was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. DRO was found to degrade significantly in acid and base stress conditions and to remain stable in thermal, photolytic degradation, oxidative and hydrolytic conditions. The degradation products were well resolved from primary peak and its impurities, proving that the method is stability indicating. The developed method was validated as per International Conference on Harmonization guidelines with respect to specificity, limit of detection, limit of quantification, linearity, accuracy, precision, solution stability and robustness. This method is also suitable for the determination of DRO drug substance and pharmaceutical dosage forms. PMID:23863770

  16. Application of stability-indicating HPTLC method for quantitative determination of metadoxine in pharmaceutical dosage form.

    PubMed

    Kaul, Neeraj; Agrawal, Himani; Patil, Bharat; Kakad, Abhijit; Dhaneshwar, S R

    2005-04-01

    A sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic method for analysis of metadoxine both as a bulk drug and in formulations was developed and validated. The method employed TLC aluminium plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of acetone-chloroform-methanol-ammonia (7.0:4.0:3.0:1.2, v/v/v/v). Densitometric analysis of metadoxine was carried out in the absorbance mode at 315 nm. This system was found to give compact spots for metadoxine (Rf value of 0.45+/-0.02, for six replicates). Metadoxine was subjected to acid, alkali and neutral hydrolysis, oxidation, dry and wet heat treatment and photo and UV degradation. The drug undergoes degradation under all stress conditions. Also, the degraded products were well resolved from the pure drug with significantly different Rf values. The method was validated for linearity, precision, robustness, LOD, LOQ, specificity and accuracy. Linearity was found to be in the range of 100-1500 ng/spot with significantly high value of correlation coefficient r2=0.9997+/-1.02. The linear regression analysis data for the calibration plots showed good linear relationship with r2=0.9999+/-0.58 in the working concentration range of 200-700 ng/spot. The mean value of slope and intercept were 0.11+/-0.04 and 18.73+/-1.89, respectively. The limits of detection and quantitation were 50 and 100 ng/spot, respectively. Statistical analysis proves that the method is repeatable and specific for the estimation of the said drug. As the method could effectively separate the drug from its degradation products, it can be employed as a stability-indicating one. Moreover, the proposed HPTLC method was utilized to investigate the kinetics of acid and base degradation process. Arrhenius plot was constructed and activation energy was calculated respectively for acid and base degradation process. PMID:15848212

  17. Bioremediation of Contaminated Lake Sediments and Evaluation of Maturity Indicies as Indicators of Compost Stability

    PubMed Central

    Rekha, P.; Suman Raj, D. S.; Aparna, C.; Bindu, V. Hima; Anjaneyulu, Y.

    2005-01-01

    Land contamination is one of the widely addressed problems, which is gaining importance in many developed and developing countries. International efforts are actively envisaged to remediate contaminated sites as a response to adverse health effects. Popular conventional methodologies only transfer the phase of the contaminant involving cost intensive liabilities besides handling risk of the hazardous waste. Physico-chemical methods are effective for specific wastes, but are technically complex and lack public acceptance for land remediation. “Bioremediation”, is one of the emerging low-cost technologies that offer the possibility to destroy various contaminants using natural biological activities. Resultant non -toxic end products due to the microbial activity and insitu applicability of this technology is gaining huge public acceptance. In the present study, composting is demonstrated as a bioremediation methodology for the stabilization of contaminated lake sediments of Hyderabad, A.P, India. Lake sediment contaminated with organics is collected from two stratums – upper (0.25 m) and lower (0.5m) to set up as Pile I (Upper) and Pile II (Lower) in the laboratory. Lime as a pretreatment to the lake sediments is carried out to ensure metal precipitation. The pretreated sediment is then mixed with organic and inorganic fertilizers like cow dung, poultry manure, urea and super phosphate as initial seeding amendments. Bulking agents like sawdust and other micronutrients are provided. Continuous monitoring of process control parameters like pH, moisture content, electrical conductivity, total volatile solids and various forms of nitrogen were carried out during the entire course of the study. The stability of the compost was evaluated by assessing maturity indices like C/N, Cw (water soluble carbon), CNw (Cw/Nw), nitrification index (NH4/NO?3), Cation Exchange Capacity (CEC), germination index, humification ratio, compost mineralization index (ash content/oxidizable carbon), sorption capacity index (CEC/oxidizable carbon). Enzyme activities of agricultural interest like urease, phosphatase, ?-glucosidase, dehydrogenase and BAA-hydrolyzing protease, which are involved in the nitrogen, phosphorus and carbon cycles, were also assessed. Total content of macro and micronutrients in the final compost was also determined to assess the fertilizer value. The studies revealed that composting could be applied as a remediation technology after removing the top sediment. The maturity indices that are evaluated from the present study can be used to validate the success of the remediation technology. PMID:16705825

  18. Stress Degradation Studies on Varenicline Tartrate and Development of a Validated Stability-Indicating HPLC Method

    PubMed Central

    Pujeri, Sudhakar S.; Khader, Addagadde M. A.; Seetharamappa, Jaldappagari

    2012-01-01

    A simple, rapid and stability-indicating reversed-phase liquid chromatographic method was developed for the assay of varenicline tartrate (VRT) in the presence of its degradation products generated from forced decomposition studies. The HPLC separation was achieved on a C18 Inertsil column (250 mm × 4.6 mm i.d. particle size is 5 ?m) employing a mobile phase consisting of ammonium acetate buffer containing trifluoroacetic acid (0.02M; pH 4) and acetonitrile in gradient program mode with a flow rate of 1.0 mL min?1. The UV detector was operated at 237 nm while column temperature was maintained at 40 °C. The developed method was validated as per ICH guidelines with respect to specificity, linearity, precision, accuracy, robustness and limit of quantification. The method was found to be simple, specific, precise and accurate. Selectivity of the proposed method was validated by subjecting the stock solution of VRT to acidic, basic, photolysis, oxidative and thermal degradation. The calibration curve was found to be linear in the concentration range of 0.1–192 ?g mL?1 (R2 = 0.9994). The peaks of degradation products did not interfere with that of pure VRT. The utility of the developed method was examined by analyzing the tablets containing VRT. The results of analysis were subjected to statistical analysis. PMID:22396908

  19. Stability-indicating HPLC Method for Simultaneous Determination of Montelukast and Fexofenadine Hydrochloride.

    PubMed

    Pankhaniya, Mona; Patel, Parula; Shah, J S

    2013-05-01

    A simple, specific, accurate, and stability-indicating reversed-phase high-performance liquid chromatographic method was developed for the simultaneous determination of montelukast and fexofenadine hydrochloride, using a Lichrospher(®) 100, RP-18e column and a mobile phase composed of methanol:0.1% o-phosphoric acid (90:10 v/v), pH 6.8. The retention times of montelukast and fexofenadine hydrochloride were found to be 10.16 and 12.03 min, respectively. Linearity was established for montelukast and fexofenadine hydrochloride in the range of 2-10 ?g/ml and 24-120 ?g/ml, respectively. The percentage recoveries of montelukast and fexofenadine hydrochloride were found to be in the range of 99.09 and 99.81%, respectively. Both the drugs were subjected to acid and base hydrolysis, oxidation, photolytic, and thermal degradation conditions. The degradation products of montelukast and fexofenadine hydrochloride were well resolved from the pure drug with significant differences in their retention time values. This method can be successfully employed for simultaneous quantitative analysis of montelukast and fexofenadine hydrochloride in bulk drugs and formulations. PMID:24082344

  20. Stability indicating LC-method for estimation of paracetamol and lornoxicam in combined dosage form.

    PubMed

    Shah, Dimal A; Patel, Neel J; Baldania, Sunil L; Chhalotiya, Usman K; Bhatt, Kashyap K

    2011-03-01

    A simple, specific and stability indicating reversed phase high performance liquid chromatographic method was developed for the simultaneous determination of paracetamol and lornoxicam in tablet dosage form. A Brownlee C-18, 5 ?m column having 250×4.6 mm i.d. in isocratic mode, with mobile phase containing 0.05 M potassium dihydrogen phosphate:methanol (40:60, v/v) was used. The flow rate was 1.0 ml/min and effluents were monitored at 266 nm. The retention times of paracetamol and lornoxicam were 2.7 min and 5.1 min, respectively. The linearity for paracetamol and lornoxicam were in the range of 5-200 ?g/ml and 0.08-20 ?g/ml, respectively. Paracetamol and lornoxicam stock solutions were subjected to acid and alkali hydrolysis, chemical oxidation and dry heat degradation. The proposed method was validated and successfully applied to the estimation of paracetamol and lornoxicam in combined tablet dosage form. PMID:21617776

  1. Stability-indicating spectrofluorometric method for the determination of some cephalosporin drugs via their degradation products.

    PubMed

    Mostafa, Nadia M; Abdel-Fattah, Laila; Weshahy, Soheir A; Hassan, Nagiba Y; Boltia, Shereen A

    2015-01-01

    A stability-indicating spectrofluorometric method was investigated for the determination of three cephalosporin drugs, namely, cefpodoxime proxetil (CPD), cefixime trihydrate (CFX), and cefepime hydrochloride (CPM), via their acid and alkali degradation products. The three drugs were determined via their acid degradation at 432, 422, and 435 nm using an excitation wavelength of 310, 330, and 307 nm for CPD, CFX, and CPM determination, respectively, and via their alkali degradation at 407, 411, and 405 nm using an excitation wavelength of 310, 305, and 297 nm for CPD, CFX, and CPM determination, respectively. Linearity was achieved in the ranges of 0.35-3.50, 0.4-4.0, and 0.3-3.0 ?g/mL for the acid degradation products of CPD, CFX, and CPM, respectively, and in ranges of 0.05-0.5, 0.1-1.0, and 0.08-0.80 ?g/mL for the alkali degradation products of CPD, CFX, and CPM, respectively. The method was validated for various parameters according to International Conference on Harmonization guidelines. The method was successfully applied for the determination of these cephalosporin drugs in pharmaceutical dosage forms with good accuracy and precision. The results obtained by the proposed spectrofluorometric method were compared with good agreement to the official HPLC method. PMID:25905742

  2. Stability indicating methods for determination of Donepezil Hydrochloride according to ICH guidelines.

    PubMed

    Abbas, Samah Sayed; Fayez, Yasmin Mohamed; Abdel Fattah, Laila El-Sayed

    2006-10-01

    Stability indicating assays for determination of Donepezil Hydrochloride in presence of its oxidative degradate were developed and validated. The first three are spectrophotometric methods depending on using zero order (D(0)), first order (D(1)) and second order (D(2)) spectra. The absorbance was measured at 315 nm for (D(0)) while the amplitude was measured at 332.1nm for (D(1)) and 340 nm for (D(2)) using deionized water as a solvent. Donepezil Hydrochloride (I) can be determined in the presence of up to 70% of its oxidative degradate (II) using (D(0)), 80% using (D(1)) and 90% using (D(2)). The linearity range was found to be 8-56 microg ml(-1) for (D(0)), (D(1)) and (D(2)). These methods were applied for the analysis of I in both powder and tablet form. Also, a spectrofluorimetric method depending on measuring the native fluorescence of I in deionized water using lambda excitation 226 nm and lambda emission 391 nm is suggested. The linearity range was found to be 0.32-3.20 microg ml(-1) using this method, I was determined in the presence of up to 90% of II. The proposed method was applied for the analysis of I in tablet form as well as in human plasma. The last method depends on using TLC separation of I from its oxidative degradate II and I was then determined spectrodensitometrically. The mobile phase was methanol : chloroform : 25% ammonia (16 : 64 : 0.1 by volume). The linearity range was found to be 2-15 microg/spot. This method was applied to the analysis of I in both powder and tablet form using acetonitrile as a solvent. PMID:17015988

  3. Stability-indicating methods for the determination of piretanide in presence of the alkaline induced degradates.

    PubMed

    Youssef, Nadia F

    2005-10-01

    Stability-indicating high performance liquid chromatography (HPLC), thin-layer chromatography (TLC) and first-derivative of ratio spectra (1DD) methods are developed for the determination of piretanide in presence of its alkaline induced degradates. HPLC method depends on separation of piretanide from its degradates on mu-Bondapak C18 column using methanol:water:acetic acid (70:30:1, v/v/v) as a mobile phase at flow rate 1.0 ml/min and UV detector at 275 nm. TLC densitometic method is based on the difference in Rf-values between the intact drug and its degradates on thin-layer silica gel. Iso-propanol:ammonia 33% (8:2, v/v) was used as a developing mobile phase and the chromatogram was scanned at 275 nm. The derivative of ratio spectra method (1DD) depends on the measurement of the absorbance at 288 nm in the first-derivative of ratio spectra for the determination of the cited drug in the presence of its degradates. Calibration graphs of the three suggested methods are linear in the concentration ranges 0.02-0.3 microg/20 microl, 0.5-10 microg/spot and 5-50 microg/ml, with mean percentage recovery 99.27+/-0.52, 99,17+/-1.01 and 99.65+/-1.01%, respectively. The three proposed methods were successfully applied for the determination of piretanide in bulk powder, laboratory-prepared mixtures and pharmaceutical dosage form with good accuracy and precision. The results were statistically analyzed and compared with those obtained by the official method. Validation of the method was determined with favourable specificity, linearity, precision, and accuracy was assessed by applying the standard addition technique. PMID:16223647

  4. Reduction of indicator and pathogenic microorganisms in pig manure through fly ash and lime addition during alkaline stabilization.

    PubMed

    Wong, Jonathan W C; Selvam, Ammaiyappan

    2009-09-30

    A pilot scale study was conducted to evaluate the effect of lime and alkaline coal fly ash (CFA) on the reduction of pathogens in pig manure during alkaline stabilization and suppression of re-growth during post-stabilization incubation. Pig manure was mixed with CFA at 25%, 33% and 50%, and a control without fly ash was maintained. To these manure-ash mixtures, lime was added at the rate of 2% or 4% and incubated for 8 days. During the incubation, the population of Salmonella, fecal coliforms, Escherichia coli, fecal Streptococcus and total bacteria were enumerated. After the alkaline stabilization process, the mixtures were incubated under green house condition to evaluate the re-growth of pathogens. During the 8-day alkaline stabilization, Salmonella, fecal coliforms, E. coli and fecal Streptococcus were completely devitalized in manure-ash-lime mixtures, whereas in the control, incubation reduced the pathogen and total bacterial population by 2-3 logs. Fecal streptococcus was destructed within 4 days of alkaline stabilization, whereas other pathogens needed 8 days for their destruction. During the incubation in green house, an increase in the population of the pathogens and total bacteria was observed. Results indicate that alkaline stabilization of pig manure with lime at 4% and CFA at 50% is effective in devitalizing the pathogens and reducing the post-stabilization re-growth. PMID:19442442

  5. Using thermal and spectroscopic (XANES) indices to understand the biological stability of soil organic matter.

    NASA Astrophysics Data System (ADS)

    Gillespie, A. W.; Sanei, H.; Diochon, A.; Tarnocai, C.; Janzen, H.; Regier, T. Z.; Gregorich, E.

    2014-12-01

    Soil organic matter (SOM) composition is a key property that underpins ecosystem productivity. Understanding its physical, chemical and biological properties is important for evaluating its role in carbon (C) and nutrient cycling in terrestrial ecosystems. In particular, the stability of SOM (i.e., resistance to microbial degradation) has important implications in ecosystem processes, including nutrient cycling, emission of greenhouse gases from soil, and C sequestration. Thus there is interest in developing new ways to measure and quantify the labile and stable forms of soil organic carbon. In this presentation, we describe the combined use of thermal decomposition methods based on pyrolysis, and chemical properties using X-ray absorption spectroscopy (XAS), to describe the stability of soil organic matter. Soils (n=81) for this study were obtained from a wide geographical range and management practices. Controlled respiration studies were conducted on the soils to determine the biodegradability of organic C after 98 days. In the thermal analysis, the sample is subjected to a temperature ramp and pyrolyzed/volatilized organic C was recorded as a function of temperature. Analysis by XAS provided information on the types of C functional groups present in a soil sample. We show that biological stability is well described using a two component model which included thermal stability and C composition chemistry.

  6. Identification and quantification of furanocoumarins in stem bark and wood of eight Algerian varieties of Ficus carica by RP-HPLC-DAD and RP-HPLC-DAD-MS.

    PubMed

    Rouaiguia-Bouakkaz, Samia; Amira-Guebailia, Habiba; Rivière, Céline; Delaunay, Jean-Claude; Waffo-Téguo, Pierre; Mérillon, Jean-Michel

    2013-04-01

    Furanocoumarins are the major phytoalexins of Ficus carica and are effective natural drug candidates for treatment of several types of cancer and skin disease. The objectives of this study were to analyze and quantify linear furanocoumarins, mainly psoralen and bergapten, in wood and bark of stems from eight Algerian varieties of fig and to establish the differences in the content of these metabolites in the eight local samples. Psoralen and bergapten contents in the stem bark and wood (in microg/g DW) varied respectively from 146.6 to 1110.3 and from 395.7 to 1671.8 for psoralen, and from 114.3 to 524.0 and from 144.2 to 718.6 for bergapten. This study fills a gap in our knowledge of furanocoumarin distribution in different parts of the fig tree. Psoralen and bergapten concentrations were higher in the wood than in the stem bark. Most of the dark fruited fig trees produce these two coumarins more than the green ones. PMID:23738460

  7. Survey of wastewater indicators and human pathogen genomes in biosolids produced by class a and class B stabilization treatments.

    PubMed

    Viau, Emily; Peccia, Jordan

    2009-01-01

    Accurate modeling of the infectious aerosol risk associated with the land application of biosolids requires an in-depth knowledge of the magnitudes and changes in pathogen concentrations for a variety of class A and class B stabilization methods. The following survey used quantitative PCR (qPCR) and culture assays to detect environmentally resistant bacterial and viral pathogens and biosolid indicator organisms for 36 biosolid grab samples. Biosolids were collected from 14 U.S. states and included 16 class B mesophilic anaerobic digestion (MAD) samples and 20 class A biosolid samples from temperature-phased anaerobic digestion (TPAD), MAD plus composting (COM), and MAD plus heat pelletization processes. The indicator concentrations of fecal coliforms and male-specific coliphages as well as pathogen genome concentrations for human adenovirus species, Legionella pneumophila, Staphylococcus aureus, and Clostridium difficile were significantly lower in the class A samples, and a multivariate analysis of variance ranked the stabilization processes from the lowest pathogen/indicator load to the highest as (i) class A COM, (ii) class A TPAD, and (iii) class B MAD. Human adenovirus genomes were found in 88% of the class B samples and 70 to 100% of the class A samples. L. pneumophila, S. aureus, and C. difficile genomes were detected at the qPCR assay detection limits in 19 to 50% of the class B and class A anaerobic digestion samples, while L. pneumophila was detected in 50% of the class A compost samples. When considering all the stabilization methods, both the fecal coliform and the male-specific coliphage concentrations show a significant linear correlation with the pathogen genome concentrations. This survey provides the necessary pathogen concentrations to add to biosolid aerosol risk and pathogen exposure analyses and clarifies the effectiveness of class A stabilization methods with the pathogen and indicator loads in biosolids. PMID:18997022

  8. Amphiphile-induced vesiculation in aged hereditary spherocytosis erythrocytes indicates normal membrane stability properties under

    E-print Network

    Iglic, Ales

    Amphiphile-induced vesiculation in aged hereditary spherocytosis erythrocytes indicates normal protein or ankyrin were incubated with amphiphiles (detergents) at sublytic concentrations (378C, 60 min erythrocytes (1%). Control and HS cells responded, however, similarly to amphiphile-treatment (non

  9. A performance indicator for reduction in vulnerability through stabilization of plutonium

    SciTech Connect

    Marchese, A.R. [Dept. of Energy, Germantown, MD (United States); Neogy, P.; Azarm, M.A. [Brookhaven National Lab., Upton, NY (United States). Dept. of Advanced Technology

    1997-02-01

    The US Department of Energy (DOE) is currently storing several metric tons of plutonium in various forms in a variety of facilities throughout the DOE complex. Since the cessation of weapons production in 1990, many of these facilities with plutonium in storage have not operated. Since the shutdown was regarded as temporary, little attempt was made at that time to empty the process lines of plutonium, or to place the plutonium in containers or packages that would provide safe storage for extended periods of time. As a result, the packages and containers providing interim storage are vulnerable to failure through leakage, rupture and other modes, and pose potential hazards to facility workers, the public and the environment. Here, an approach to measuring and tracking the reduction in vulnerabilities resulting from stabilizing and repackaging plutonium is developed and presented. The approach utilizes results obtained by the DOE Working Group on the vulnerabilities associated with plutonium storage.

  10. A validated stability-indicating LC method for estimation of etoposide in bulk and optimized self-nano emulsifying formulation: Kinetics and stability effects

    PubMed Central

    Akhtar, Naseem; Talegaonkar, Sushama; Khar, Roop Kishan; Jaggi, Manu

    2012-01-01

    The present investigation was aimed to establish a validated stability-indicating liquid chromatographic method for the estimation of etoposide (ETP) in bulk drug and self-nano emulsifying formulation. ETP was successfully separated from the degradation products formed under stress conditions on LiChrospher 100 C18 reverse-phase column (a 250 mm × 4.6 mm i.d., 5-?m particle size) using 55:45 (v/v) acetonitrile–phosphate buffer saline (pH 4.5) as the mobile phase, at a flow rate of 1.0 mL min?1 and detection at 283 nm. The response was a linear function of analyte concentration (R2 > 0.9997) over the concentration range of 0.05–50 ?g mL?1. The method was validated for precision, accuracy, robustness, sensitivity and specificity. The % recovery of ETP at three different levels (50%, 100% and 150%) ranged between 93.84% and 100.06% in optimized self-nano emulsifying formulation, Etosid® soft-gelatin capsule and Fytosid® injection. First-order degradation kinetics of ETP were observed under acidic and alkaline conditions. The method was also applied for the stability assessment of self-nano emulsifying formulation under accelerated conditions, the formulation was found to be stable at all storage conditions with the shelf-life of 2.37 years at 25 °C. The method holds promise for routine quality control of ETP in bulk, pharmaceutical formulations as well as in stability-indicating studies. PMID:23960824

  11. A size exclusion-reversed phase two dimensional-liquid chromatography methodology for stability and small molecule related species in antibody drug conjugates.

    PubMed

    Li, Yi; Gu, Christine; Gruenhagen, Jason; Zhang, Kelly; Yehl, Peter; Chetwyn, Nik P; Medley, Colin D

    2015-05-01

    Antibody drug conjugates (ADCs) are complex therapeutic agents combining the specific targeting properties of antibodies and highly potent cytotoxic small molecule drugs to selectively eliminate tumor cells while limiting the toxicity to normal healthy tissues. One unique critical quality attribute of ADCs is the content of unconjugated small molecule drug present from either incomplete conjugation or degradation of the ADC. In this work, size exclusion chromatography (SEC) was coupled with reversed-phase (RP) HPLC in an online 2-dimensional chromatography format for identification and quantitation of unconjugated small molecule drugs and related small molecule impurities in ADC samples directly without sample preparation. The SEC method in the 1st dimension not only separated the small molecule impurities from the intact ADC, but also provided information about the size variants (monomer, dimer, aggregates, etc.) of the ADC. The small molecule peak from the SEC was trapped and sent to a RP-HPLC in the 2nd dimension to further separate and quantify the different small molecule impurities present in the ADC sample. This SEC-RP 2D-LC method demonstrated excellent precision (%RSD<2.0), linearity (r(2)=0.9999), sensitivity (LOQ of 0.05?g/mL of free drug in ADC sample) and accuracy (95-105% recovery of spiked samples). The 2D-LC method was further utilized to study the stability of an ADC drug product at different temperatures and pHs. Both small molecule degradation products and aggregation of the conjugate were observed in the stability samples and the degradation pathways of the ADC were investigated. This 2D-LC method offers a powerful tool for ADC characterization and provides valuable information for conjugation and formulation development. PMID:25818558

  12. Stability-indicating spectrofluorimetric method for determination of itopride hydrochloride in raw material and pharmaceutical formulations.

    PubMed

    Walash, Mohamed I; Ibrahim, Fawzia; Eid, Manal I; El Abass, Samah Abo

    2013-11-01

    A simple, sensitive and rapid spectrofluorimetric method for determination of itopride hydrochloride in raw material and tablets has been developed. The proposed method is based on the measurement of the native fluorescence of the drug in water at 363 nm after excitation at 255 nm. The relative fluorescence intensity-concentration plot was rectilinear over the range of 0.1-2 ?g/mL (2.5?×?10(-7)-5.06?×?10(-6) mole/L), with good correlation (r?=?0.9999), limit of detection of 0.015 ?g/mL and a lower limit of quantification of 0.045 ?g/mL. The described method was successfully applied for the determination of itopride hydrochloride in its commercial tablets with average percentage recovery of 100.11?±?0.32 without interference from common excipients. Additionally, the proposed method can be applied for determination of itopride in combined tablets with rabeprazole or pantoprazole without prior separation. The method was extended to stability study of itopride. The drug was exposed to acidic, alkaline, oxidative and photolytic degradation according to ICH guidelines. Moreover, the method was utilized to investigate the kinetics of the alkaline, acidic and oxidative degradation of the drug. A proposal for the degradation pathways was postulated. PMID:23852162

  13. LC method for telithromycin in tablets: a stability-indicating assay.

    PubMed

    Vaucher, Lauren C; Paim, Clésio S; Lange, Alini D; Schapoval, Elfrides E S

    2009-01-21

    A liquid chromatographic (LC) method for the quantitative determination of telithromycin, the first member of the ketolides, which is a new class of macrolides, was developed. Analytical parameters were studied according to International Conference on Harmonization (ICH) guidelines. An Ace RP-18 octadecyl silane column (250 mm x 4.6 mm, 5 microm) maintained at 50 degrees C was used as the stationary phase, and methanol and 0.067 M potassium monobasic phosphate buffer pH 4.0 (55:45, v/v) were used as the mobile phase with UV detection at 265 nm. In forced degradation studies, the effects of acid, base, oxidation, UV light and temperature were investigated showing no interference in the drug peak. The method was linear (r=0.9999) at concentration ranging from 10.0 to 40.0 microg/mL, precise (intra-day relative standard deviation [RSD] and inter-day RSD values<2.0%), accurate (mean recovery=100.76%), specific and robust. Detection and quantitation limits were 0.0027 and 0.0082 microg/mL, respectively. The results showed the proposed method is suitable for its intended use. The validated method may be used to quantify telithromycin tablets and to determine the stability of the drug. The method is able to separate telithromycin from its degradation products and tablet excipients for its sensitivity and reproducibility. These results are in accordance with a previous microbiological assay study, which used the same tested conditions showing that the methods can be interchangeable. PMID:18977423

  14. Development and validation of a stability indicating HPLC method for the analysis of lornoxicam in powder for injection.

    PubMed

    Zhang, Jianjun; Li, Li; Gao, Yuan; Fan, Weiming

    2012-04-01

    A rapid, isocratic stability indicating high performance liquid chromatographic method was developed and validated for the estimation of lornoxicam in its powder for injection. The analysis was performed on a Shimadzu VP-ODS (4. 6 mm x 15 cm, 5 µm) column. The mobile phase consisted of sodium acetate (pH 5.8; 0.05 M) and methanol (45:55) flowed at 1.0 ml/min. Detection was carried out at 290 nm. The developed method had the good ability to separate lornoxicam well from the degradation products. The regression data showed good linear relationship at the concentration range of 4.04-20.20 ?/mL with r(2)=0.9999. Specificity, linearity, accuracy, precision and robustness of the method were evaluated to validate the proposed method. Stressed degradation studies were conducted to provide an indication of its stability indicating property. The limits of detection and quantitation were 9.70 and 33.94 ng /ml, respectively. Lornoxicam was found to be stable in the mobile phase in 24 h. The co-existed excipients had no interference with the analytical procedure. Additional peaks appeared in the chromatograms of five kinds of forced degraded samples (light, heat, acid, base and oxidation degradation). Mean recovery assessed at three levels was from 99. 7 to 100.3%, indicating the good accuracy of the method. Repeatability and inter-day RSD of the method was determined to be 0.38% and 0.81%, respectively. The HPLC method was demonstrated to be robust for intentional minor changes of ratio, pH change, salt concentration and column temperature. The method should be utilized as the routine analysis and quality control of lornoxicam in injectable formulation. PMID:22459464

  15. Stability-indicating micellar electrokinetic chromatography technique for simultaneous measurement of delapril and manidipine from a combination drug formulation.

    PubMed

    Todeschini, Vítor; Sangoi, Maximiliano da Silva; Meira, Alianise da Silva; Miron, Diogo; Lange, Alini Dall Cortivo; Volpato, Nadia Maria

    2014-01-01

    A stability-indicating micellar electrokinetic chromatography (MEKC) method was developed and validated for simultaneous analysis of delapril (DEL) and manidipine (MAN) using salicylic acid as an internal standard. The MEKC method was performed using a fused-silica capillary (effective length of 72 cm) with 50 mM of borate buffer and 5 mM of anionic surfactant sodium dodecylsulfate at pH 9.0 as the background electrolyte. The separation was achieved at 25 kV applied voltage and 35 degrees C. The injection was performed at 50 mbar for 5 s, with detection at 208 nm. The method was linear in the range of 15-150 microg/mL (r2 = 0.9966) for DEL and 5-50 microg/mL (r2 = 0.9985) for MAN with adequate results for the precision (< or = 1.87%) and accuracy (98.94% for DEL and 100.65% for MAN). The specificity of the method and its stability-indicating capability was demonstrated through forced degradation studies, which showed that there was no interference from the excipients. The Plackett-Burman experimental design was used for robustness evaluation, giving results within the acceptable range. The method was successfully applied for analysis of the drugs, and the results were compared to an LC method, resulting in nonsignificant differences (P = 0.78 and 0.84 for DEL and MAN, respectively). PMID:24672867

  16. A Stability-indicating High Performance Liquid Chromatographic Assay for the Simultaneous Determination of Atenolol and Lercanidipine Hydrochloride in Tablets

    PubMed Central

    Kaila, H. O.; Ambasana, M. A.; Thakkar, R. S.; Saravaia, H. T.; Shah, A. K.

    2011-01-01

    A simple, rapid, precise and accurate isocratic reversed phase stability indicating HPLC method was developed and validated for the simultaneous determination of atenolol and lercanidipine hydrochloride in commercial tablets. The chromatographic separation was achieved on phenomenex Gemini C18 (250×4.6 mm, 5 ?m) column using a mobile phase consisting of acetonitrile and buffer (20 mM potassium dihydrogen phosphate pH 3.5) in the ratio of (55:45, v/v) at a flow rate of 1.0 ml/min and UV detection at 235 nm. The linearity of the proposed method was investigated in the range of 40-160 ?g/ml (r2=0.9995) for atenolol and 8-32 ?g/ml (r2=0.9993) for lercanidipine. Degradation products produced as a result of stress studies did not interfere with the detection of atenolol and lercanidipine and the assay can thus be considered stability-indicating. PMID:22707819

  17. A Stability-indicating High Performance Liquid Chromatographic Assay for the Simultaneous Determination of Atenolol and Lercanidipine Hydrochloride in Tablets.

    PubMed

    Kaila, H O; Ambasana, M A; Thakkar, R S; Saravaia, H T; Shah, A K

    2011-07-01

    A simple, rapid, precise and accurate isocratic reversed phase stability indicating HPLC method was developed and validated for the simultaneous determination of atenolol and lercanidipine hydrochloride in commercial tablets. The chromatographic separation was achieved on phenomenex Gemini C18 (250×4.6 mm, 5 ?m) column using a mobile phase consisting of acetonitrile and buffer (20 mM potassium dihydrogen phosphate pH 3.5) in the ratio of (55:45, v/v) at a flow rate of 1.0 ml/min and UV detection at 235 nm. The linearity of the proposed method was investigated in the range of 40-160 ?g/ml (r(2)=0.9995) for atenolol and 8-32 ?g/ml (r(2)=0.9993) for lercanidipine. Degradation products produced as a result of stress studies did not interfere with the detection of atenolol and lercanidipine and the assay can thus be considered stability-indicating. PMID:22707819

  18. A new strategy to stabilize oxytocin in aqueous solutions: I. The effects of divalent metal ions and citrate buffer.

    PubMed

    Avanti, Christina; Amorij, Jean-Pierre; Setyaningsih, Dewi; Hawe, Andrea; Jiskoot, Wim; Visser, Jan; Kedrov, Alexej; Driessen, Arnold J M; Hinrichs, Wouter L J; Frijlink, Henderik W

    2011-06-01

    In the current study, the effect of metal ions in combination with buffers (citrate, acetate, pH 4.5) on the stability of aqueous solutions of oxytocin was investigated. Both monovalent metal ions (Na(+) and K(+)) and divalent metal ions (Ca(2+), Mg(2+), and Zn(2+)) were tested all as chloride salts. The effect of combinations of buffers and metal ions on the stability of aqueous oxytocin solutions was determined by RP-HPLC and HP-SEC after 4 weeks of storage at either 4°C or 55°C. Addition of sodium or potassium ions to acetate- or citrate-buffered solutions did not increase stability, nor did the addition of divalent metal ions to acetate buffer. However, the stability of aqueous oxytocin in aqueous formulations was improved in the presence of 5 and 10 mM citrate buffer in combination with at least 2 mM CaCl(2), MgCl(2), or ZnCl(2) and depended on the divalent metal ion concentration. Isothermal titration calorimetric measurements were predictive for the stabilization effects observed during the stability study. Formulations in citrate buffer that had an improved stability displayed a strong interaction between oxytocin and Ca(2+), Mg(2+), or Zn(2+), while formulations in acetate buffer did not. In conclusion, our study shows that divalent metal ions in combination with citrate buffer strongly improved the stability of oxytocin in aqueous solutions. PMID:21448747

  19. Stability-indicating HPLC-DAD/UV-ESI/MS impurity profiling of the anti-malarial drug lumefantrine

    PubMed Central

    2011-01-01

    Background Lumefantrine (benflumetol) is a fluorene derivative belonging to the aryl amino alcohol class of anti-malarial drugs and is commercially available in fixed combination products with ?-artemether. Impurity characterization of such drugs, which are widely consumed in tropical countries for malaria control programmes, is of paramount importance. However, until now, no exhaustive impurity profile of lumefantrine has been established, encompassing process-related and degradation impurities in active pharmaceutical ingredients (APIs) and finished pharmaceutical products (FPPs). Methods Using HPLC-DAD/UV-ESI/ion trap/MS, a comprehensive impurity profile was established based upon analysis of market samples as well as stress, accelerated and long-term stability results. In-silico toxicological predictions for these lumefantrine related impurities were made using Toxtree® and Derek®. Results Several new impurities are identified, of which the desbenzylketo derivative (DBK) is proposed as a new specified degradant. DBK and the remaining unspecified lumefantrine related impurities are predicted, using Toxtree® and Derek®, to have a toxicity risk comparable to the toxicity risk of the API lumefantrine itself. Conclusions From unstressed, stressed and accelerated stability samples of lumefantrine API and FPPs, nine compounds were detected and characterized to be lumefantrine related impurities. One new lumefantrine related compound, DBK, was identified and characterized as a specified degradation impurity of lumefantrine in real market samples (FPPs). The in-silico toxicological investigation (Toxtree® and Derek®) indicated overall a toxicity risk for lumefantrine related impurities comparable to that of the API lumefantrine itself. PMID:21356068

  20. Long term stability of iron for more than 1500 years indicated by archaeological samples from the Yamato 6th tumulus

    NASA Astrophysics Data System (ADS)

    Yoshikawa, Hideki; Gunji, Eiichi; Tokuda, Masashi

    2008-09-01

    One of the candidate materials for overpack in the Japanese engineered barrier system for high-level radioactive waste (HLW) is iron and therefore its long-term stability for at least 1000 years is very important for safety analysis of the repository system. Therefore, several of the iron artifacts excavated from the Yamato 6th tumulus (ancient tomb) in Nara prefecture were analyzed using X-ray computed tomography (CT) to determine corrosion depth. The samples analyzed, both of two large and 11 smaller iron artifacts are called 'Tetsutei'. The thickness of each rust layer was measured from a cross-section image of the sample and the difference in material density between rust and iron was shown by the image density by the X-ray CT. In the case of pitting corrosion in the sample, the depth of the pits was measured directly and estimated as total corrosion depth with general corrosion layer. The corrosion depths are 0.5-2.1 mm. These data indicate conservative predictions for the extrapolations based on experimental studies. Such corrosion data from archaeological samples are useful in analogue studies of high-level radioactive waste disposal as evidence of long-term stability of a waste container.

  1. Simultaneous quantification of related substances of perindopril tert-butylamine using a novel stability indicating liquid chromatographic method.

    PubMed

    Szabó, Zoltán-István; Réti, Zenk?-Zsuzsánna; Gagyi, László; Kis, Erika Lilla; Sipos, Emese

    2015-03-01

    A novel stability indicating gradient reverse-phased high-performance liquid chromatographic method has been developed for the quantification of impurities of perindopril tert-butylamine (PER) in pharmaceutical dosage form. Separation of the active substance and its known (Impurities B, C, D, E, F) and unknown impurities was achieved on a BDS Hypersil C18 column (250 mm × 4.6 mm, 5 µm), thermostated at 70°C, using a mobile phase comprised of aqueous solution of sodium 1-heptanesulfonate adjusted to pH 2 with perchloric acid and acetonitrile. The flow rate was maintained at 1.5 mL min(-1), injection volume of 20 µL was utilized and detection of analytes was performed at 215 nm. The developed method was validated in accordance with current ICH Guidelines for all suggested parameters, including forced degradation studies and proved to be linear, accurate, precise and suitable for the impurity testing of PER, being subsequently applied during on-going stability studies of a newly developed generic formulation. PMID:25616989

  2. Development and Validation of Stability-indicating HPLC Method for Betamethoasone Dipropionate and Related Substances in Topical Formulation

    PubMed Central

    Vairale, A. S.; Sivaswaroop, P.; Bandana, S.

    2012-01-01

    A gradient reversed phase HPLC method was developed and validated for analysis of betamethasone dipropionate, its related substances and degradation products, using Altima C18 column (250×4.6 mm, 5 ?m) with a flow rate of 1.0 ml/min and detection wavelength of 240 nm. The mobile phase A is a mixture of water, tetrahydrofuran and acetonitrile in the ratio of 90:4:6 (v/v/v) while mobile phase B is a mixture of acetonitrile, tetrahydrofuran, water and methanol in the ratio of 74:2:4:20 (v/v/v/v). The samples were analyzed using 20 ?l injection volume and the column temperature was maintained at 50°. The limit of detection and limit of quantitation were found to be 0.02 ?g/ml and 0.07 ?g/ml, respectively. The stability-indicating capability of method was established by forced degradation studies and method demonstrated successful separation of drug, its related substances and degradation products. The method was validated as per the International Conference on Harmonization guidelines. The developed method is linear in the range of 0.07 to 200% of specification limits established for all the known related substances; betamethasone17-propionate, betamethasone 21-propionate, betamethasone 17-propionate-21-acetate (RSD <5, 2, 1%, respectively, r2=09991-0.9999 for sample concentration of 100 ?g/ml). The method is sensitive, specific, linear, accurate, precise and stability indicating for the quantitation of drug, its related substances and other degradation compounds. PMID:23325990

  3. Sorption of certain isatins on various sorbents under RP-HPLC conditions

    NASA Astrophysics Data System (ADS)

    Konstantinov, A. V.; Shafigulin, R. V.; Il'in, M. M.; Davankov, V. A.; Bulanova, A. V.; Purygin, P. P.

    2013-06-01

    The results from chromatographic analysis of biologically active isatin derivatives on hyper-crosslinked polystyrene (HCLPS) and silica gel modified by octadecyl groups (SilC18) are presented. The constants of distribution of sorbates between a mobile phase and the investigated sorbents ( K x ) and the changes in the standard differential molar Gibbs energies of adsorption (? _a bar G^circ ) are calculated, along with the chromatographic retention-physicochemical property of sorbate dependences. It is found that the equations describing these dependences have high forecasting ability with respect to the values of retention factors of the investigated sorbates.

  4. VALIDATED RP HPLC METHOD FOR THE QUANTITATION OF LAMIVUDINE IN BULK AND TABLET DOSAGE FORMS

    Microsoft Academic Search

    C. JOSE GNANA BABU; G. VIJAYA KUMAR

    A simple, specific, accurate, precise and sensitive reverse phase high performance liquid chromatographic method has been developed for the quantitation of Lamivudine in both pure and tablet dosage forms. A Phenomenex Gemini C- 18, 5 µm column having 250×4.6 mm i.d. in isocratic mode with mobile phase containing 0.02 M potassium dihydrogen phosphate: methanol (40:60) adjusted to pH 3.8 using

  5. Regularities of Anthocyanins Retention in RP HPLC for “Water–Acetonitrile–Phosphoric Acid” Mobile Phases

    PubMed Central

    Deineka, V. I.; Deineka, L. A.; Saenko, I. I.

    2015-01-01

    The influence of exchange of HCOOH (System 2) by phosphoric acid (System 1) for acidification of the “acetonitrile–water” mobile phases for reversed-phase HPLC of anthocyanins was investigated in the framework of relative retention analysis. The differences and similarities of anthocyanins separation were revealed. It has been shown that some common features of the quantitative relationships may be used for preliminary anthocyanins structure differentiation, according to the number of OH-groups in anthocyanidin backbone as well as to a number of saccharide molecules in glycoside radicals in position 3 of the anthocyanin without MS detection. PMID:25692073

  6. Separation of Selected Flavonoids by use of RP?HPLC\\/NP?HPTLC Coupled Methods

    Microsoft Academic Search

    Miros?aw A. Hawry?; Janusz Makar

    2007-01-01

    Phenolic compounds, such as phenolic acids, flavonoids, flavonoid glycosides, and resveratrol, were chromatographed on thin?layers of silica in various eluent systems. Systems with the highest selectivity were chosen. Also, reversed?phase HPLC systems were optimized for the separation of investigated compounds and most the selective system was applied for the separation of two phenolic extracts – Polygonum avicularis and Polygonum hydropiper.

  7. RP-HPLC Estimation of Imipramine Hydrochloride and Diazepam in Tablets.

    PubMed

    Srikantha, D; Raju, R R

    2015-01-01

    A simple and rapid reversed phase-high performance liquid chromatographic method was developed for simultaneous determination of imipramine hydrochloride and diazepam in pharmaceutical formulations. The elution was done in isocratic mode utilizing a mobile phase consisting of methanol:water:0.1M sodium acetate (30:50:20 v/v/v) on Chromosil C18 column with a flow rate of 1.0 ml/min and with detection at 243 nm. The measured retention time was 3.33±0.02 min for imipramine hydrochloride and 4.64±0.02 min for diazepam. Linearity was measured in the range 25-150 ?g/ml for imipramine hydrochloride (r(2)=0.999) and in the range 5-30 ?g/ml for diazepam (r(2)=0.9994), respectively. The limits of detection and quantitation were 0.03 and 0.1 ?g/ml for imipramine hydrochloride and 0.02 and 0.07 ?g/ml for diazepam. Satisfactory validation was also obtained from recovery (100.95-101.52% for imipramine hydrochloride and 99.47-100.33% for diazepam) studies, intraday and interday precision (<2%) and robustness results. The reported method was the first study of these drugs in combination and could be employed for routine quantitative determination of imipramine hydrochloride and diazepam in tablets. PMID:26180281

  8. Validation and method development of Tadalafil in bulk and tablet dosage form by RP-HPLC.

    PubMed

    Bojanapu, A; Subramaniam, A T; Munusamy, J; Dhanapal, K; Chennakesavalu, J; Sellappan, M; Jayaprakash, V

    2015-02-01

    A novel, precise, rapid and sensitive reverse phase high performance liquid chromatographic method has been developed for the validated estimation of Tadalafil in bulk and tablet dosage form. The separation was achieved on Agilent Eclipse XDB C18 column (150 mm×4.6 mm, 5 µ) using a mobile phase that consists of the buffer (potassium dihydrogen orthophosphate) and acetonitrile in the ration of 50:50 V/V, pH 6 was adjusted with orthophosphoric acid. The flow rate was maintained at 1.2 ml/min and the detection wavelength was 285 nm. The method was validated for linearity, specificity, sensitivity as per ICH guidelines. The retention time was found to be 3.181 for Tadalafil. The calibration curve was linear over the concentration range of 10-150 µg/ml. The % RSD was satisfactory which showed the method found to be reliable. The high percentage recovery confirmed the suitability of the method for estimation of Tadalafil in pharmaceutical dosage form. The developed method could be applicable for routine analysis of Tadalafil in bulk and tablet dosage form. PMID:24782284

  9. Quantitation of buclizine hydrochloride in pharmaceutical formulations and human serum by RP-HPLC.

    PubMed

    Arayne, M Saeed; Sultana, Najma; Siddiqui, Farhan Ahmed

    2006-10-01

    An isocratic reversed phase high-performance liquid chromatographic (HPLC) method with ultraviolet detection at 230 nm has been developed for the determination of buclizine hydrochloride in human serum and dosage formulation. Methylparaben was successfully used as an internal standard. Good chromatographic separation between buclizine and internal standard peaks was achieved by using a stainless steel analytical column Nucleosil, C18 (10 microm, 25 cm x 0.46 cm). The system was operated at room temperature using a mobile phase consisting of acetonitrile-water (1:1) (pH 2.6) with phosphoric acid 85% at a flow rate of 2 ml/min. The calibration curve for buclizine hydrochloride in human serum was linear over the tested concentration range of 10, 3, 1.5, 0.5, 0.15, 0.05, and 0.025 microg/ml with a correlation coefficient of 0.9999. The intra- and inter-run precision and accuracy results were 98.07 to 100.34. The proposed method was validated for selectivity, linearity, accuracy, and precision. The method was found to be suitable for the quality control of buclizine hydrochloride in bulk drug as well as in human serum. PMID:17105713

  10. A RP-HPLC method for the determination of tea catechins

    Microsoft Academic Search

    Santosh Khokhar; Dini Venema; Peter C. H. Hollman; Matthijs Dekker; W. M. F. Jongen

    1997-01-01

    An HPLC method with gradient elution for the quantification of catechins ((?)-epigallocatechin (EGC), (+)-catechin (C), (?)-epicatechin (EC), (?)-epigallocatechingallate (EGCg) and (?)-epicatechingallate (ECg)) in tea was developed. The method was used to determine catechins in black tea, green tea and oolong tea. Sample preparation was simple because only filtration and adjustment of pH was required. The levels of catechins in different

  11. Rapid rp HPLC method for quantitative determination of lornoxicam in tablets.

    PubMed

    Attimarad, Mahesh

    2010-03-01

    The objective of the study was to develop a simple, rapid, specific and precise reverse phase high performance liquid chromatographic method for the determination of lornoxicam in bulk and pharmaceutical preparations. Chromatographic separation of the drug was performed on a eclipse C18 column (150 mm × 4.6 mm, 5 ?m) as stationary phase and mobile phase used is methanol: 0.1% formic acid in water (80:20 v/v), with a flow rate of 0.8 mL min(-1) and UV detection at 381 nm. The proposed method was validated for linearity, accuracy, precision, limit of detection (LOD) and limit of quantitation (LOQ). Linearity, accuracy and precision were found to be acceptable over the ranges of 0.5-20 ?g/ml. It can be conveniently adopted for routine quality control analysis of lornoxicam. PMID:24825976

  12. RAPID RP HPLC METHOD FOR QUANTITATIVE DETERMINATION OF LORNOXICAM IN TABLETS

    PubMed Central

    Attimarad, Mahesh

    2010-01-01

    The objective of the study was to develop a simple, rapid, specific and precise reverse phase high performance liquid chromatographic method for the determination of lornoxicam in bulk and pharmaceutical preparations. Chromatographic separation of the drug was performed on a eclipse C18 column (150 mm × 4.6 mm, 5 ?m) as stationary phase and mobile phase used is methanol: 0.1% formic acid in water (80:20 v/v), with a flow rate of 0.8 mL min-1 and UV detection at 381 nm. The proposed method was validated for linearity, accuracy, precision, limit of detection (LOD) and limit of quantitation (LOQ). Linearity, accuracy and precision were found to be acceptable over the ranges of 0.5-20 ?g/ml. It can be conveniently adopted for routine quality control analysis of lornoxicam. PMID:24825976

  13. Development and Validation of RP-HPLC Method for the Estimation of Ivabradine Hydrochloride in Tablets.

    PubMed

    Seerapu, Sunitha; Srinivasan, B P

    2010-09-01

    A simple, sensitive, precise and robust reverse-phase high-performance liquid chromatographic method for analysis of ivabradine hydrochloride in pharmaceutical formulations was developed and validated as per ICH guidelines. The separation was performed on SS Wakosil C18AR, 250×4.6 mm, 5 ?m column with methanol:25 mM phosphate buffer (60:40 v/v), adjusted to pH 6.5 with orthophosphoric acid, added drop wise, as mobile phase. A well defined chromatographic peak of Ivabradine hydrochloride was exhibited with a retention time of 6.55±0.05 min and tailing factor of 1.14 at the flow rate of 0.8 ml/min and at ambient temperature, when monitored at 285 nm. The linear regression analysis data for calibration plots showed good linear relationship with R=0.9998 in the concentration range of 30-210 ?g/ml. The method was validated for precision, recovery and robustness. Intra and Inter-day precision (% relative standard deviation) were always less than 2%. The method showed the mean % recovery of 99.00 and 98.55 % for Ivabrad and Inapure tablets, respectively. The proposed method has been successfully applied to the commercial tablets without any interference of excipients. PMID:21695008

  14. Comparison of retention properties of stationary phases imitated cell membrane in RP HPLC.

    PubMed

    Bocian, Szymon; Buszewski, Bogus?aw

    2015-05-15

    Chromatographic properties of two columns was compared: commercial IAM.PC.DD2 that imitates the cell membrane and home-made Amino-P-C18 (N,O-dialkylphosphoramidate C18). The comparison has been done by correlation of retention (logkw parameters) of a series of solutes: hydrophobic (alkyl benzene derivatives and PAHs) and polar, with both acidic (flavonoids) and basic (nucleosides and nucleic bases) character. The slope of correlation plots for hydrophobic compounds and polar basic was very close to 1.0 that confirms the chromatographic similarity. Only for flavonoids the slope of correlation plot was 1.5. For hydrophobic compound retention parameters logkw were also correlated with hydrophobic parameter logP with very good determination coefficients. PMID:25899871

  15. A Simple RP-HPLC Method for Quantitation of Itopride HCl in Tablet Dosage Form

    PubMed Central

    Thiruvengada, Rajan VS; Mohamed, Saleem TS; Ramkanth, S; Alagusundaram, M; Ganaprakash, K; Madhusudhana, Chetty C

    2010-01-01

    An isocratic reversed phase high-performance liquid chromatographic method with ultraviolet detection at 220 nm has been developed for the quantification of itopride hydrochloride in tablet dosage form. The quantification was carried out using C8 column (250 mm × 4.6 mm), 5-?m particle size SS column. The mobile phase comprised of two solvents (Solvent A: buffer 1.4 mL ortho-phosphoric acid adjusted to pH 3.0 with triethyl amine and Solvent B: acetonitrile). The ratio of Solvent A: Solvent B was 75:25 v/v. The flow rate was 1.0 mL -1with UV detection at 220 nm. The method has been validated and proved to be robust. The calibration curve was linear in the concentration range of 80-120% with coefficient of correlation 0.9995. The percentage recovery for itopride HCl was 100.01%. The proposed method was validated for its selectivity, linearity, accuracy, and precision. The method was found to be suitable for the quality control of itopride HCl in tablet dosage formulation. PMID:21264104

  16. A Simple RP-HPLC Method for Quantitation of Itopride HCl in Tablet Dosage Form.

    PubMed

    Thiruvengada, Rajan Vs; Mohamed, Saleem Ts; Ramkanth, S; Alagusundaram, M; Ganaprakash, K; Madhusudhana, Chetty C

    2010-10-01

    An isocratic reversed phase high-performance liquid chromatographic method with ultraviolet detection at 220 nm has been developed for the quantification of itopride hydrochloride in tablet dosage form. The quantification was carried out using C(8) column (250 mm × 4.6 mm), 5-?m particle size SS column. The mobile phase comprised of two solvents (Solvent A: buffer 1.4 mL ortho-phosphoric acid adjusted to pH 3.0 with triethyl amine and Solvent B: acetonitrile). The ratio of Solvent A: Solvent B was 75:25 v/v. The flow rate was 1.0 mL (-1)with UV detection at 220 nm. The method has been validated and proved to be robust. The calibration curve was linear in the concentration range of 80-120% with coefficient of correlation 0.9995. The percentage recovery for itopride HCl was 100.01%. The proposed method was validated for its selectivity, linearity, accuracy, and precision. The method was found to be suitable for the quality control of itopride HCl in tablet dosage formulation. PMID:21264104

  17. Comparing prediction power and stability of broadband and hyperspectral vegetation indices for estimation of green leaf area index and canopy chlorophyll density

    Microsoft Academic Search

    N. h. Broge; E. Leblanc

    2001-01-01

    Hyperspectral reflectance data representing a wide range of canopies were simulated using the combined PROSPECT+SAIL model. The simulations were used to study the stability of recently proposed vegetation indices (VIs) derived from adjacent narrowband spectral reflectance data across the visible (VIS) and near infrared (NIR) region of the electromagnetic spectrum. The prediction power of these indices with respect to green

  18. Validated stability-indicating HPLC method for the determination of pridinol mesylate. Kinetics study of its degradation in acid medium.

    PubMed

    Bianchini, Romina M; Castellano, Patricia M; Kaufman, Teodoro S

    2008-12-01

    The stability of pridinol mesylate (PRI) was investigated under different stress conditions, including hydrolytic, oxidative, photolytic and thermal, as recommended by the ICH guidelines. Relevant degradation was found to take place under acidic (0.1N HCl) and photolytic (visible and long-wavelength UV-light) conditions, both yielding the product resulting from water elimination (ELI), while submission to an oxidizing environment gave the N-oxidation derivative (NOX). The standards of these degradation products were synthesized and characterized by IR, (1)H and (13)C NMR spectroscopy. A simple, sensitive and specific HPLC method was developed for the quantification of PRI, ELI and NOX in bulk drug, and the conditions were optimized by means of a statistical design strategy. The separation employs a C(18) column and a 51:9:40 (v/v/v) mixture of MeOH, 2-propanol and potassium phosphate solution (50mM, pH 6.0), as mobile phase, delivered at 1.0 ml min(-1); the analytes were detected and quantified at 220 nm. The method was validated, demonstrating to be accurate and precise (repeatability and intermediate precision levels) within the corresponding linear ranges of PRI (0.1-1.5 mg ml(-1); r=0.9983, n=18) and both impurities (0.1-1.3% relative to PRI, r=0.9996 and 0.9995 for ELI and NOX, respectively, n=18). Robustness against small modifications of pH and percentage of the aqueous mobile phase was ascertained and the limits of quantification of the analytes were also determined (0.4 and 0.5 microg ml(-1); 0.04% and 0.05% relative to PRI for ELI and NOX, respectively). Peak purity indices (>0.9997), obtained with the aid of diode-array detection, and satisfactory resolution (R(s)>2.0) between PRI and its impurities established the specificity of the determination, all these results proving the stability-indicating capability of the method. The kinetics of the degradation of PRI in acid medium was also studied, determining that this is a first-order process with regards to drug concentration, with an activation energy of 25.5 Kcal mol(-1) and a t(1/2)=10,830 h, in 0.1N HCl at 38 degrees C. PMID:18922659

  19. Development and Validation of a Stability-Indicating Liquid Chromatographic Method for Estimating Olmesartan Medoxomil Using Quality by Design.

    PubMed

    Beg, Sarwar; Sharma, Gajanand; Katare, O P; Lohan, Shikha; Singh, Bhupinder

    2015-08-01

    The current studies entail systematic quality by design (QbD)-based development of a simple, rapid, sensitive and cost-effective stability-indicating method for the estimation of olmesartan medoxomil. Quality target method profile was defined and critical analytical attributes (CAAs) for the reverse-phase liquid chromatography method earmarked. Chromatographic separation accomplished on a C18 column using acetonitrile and water (containing 0.1% orthophosphoric acid, pH 3.5) in 40 : 60 (v/v) as mobile phase at a flow rate of 1.0 mL/min with UV detection at 243 nm. Risk assessment studies and screening studies facilitated comprehensive understanding of the factors affecting CAAs. The mobile phase ratio and flow rate were identified as critical method parameters (CMPs) and were systematically optimized using face-centered cubic design, evaluating for CAAs, namely peak area, retention time, theoretical plates and peak tailing. Statistical modelization was accomplished followed by response surface analysis for comprehending plausible interaction(s) among CMPs. Search for optimum solution was conducted through numerical and graphical optimization for demarcating the design space. Analytical method validation and subsequent forced degradation studies corroborated the method to be highly efficient for routine analysis of drug and its degradation products. The studies successfully demonstrate the utility of QbD approach for developing the highly sensitive liquid chromatographic method with enhanced method performance. PMID:25583970

  20. Kinetic Study of the Alkaline Degradation of Oseltamivir Phosphate and Valacyclovir Hydrochloride using Validated Stability Indicating HPLC

    PubMed Central

    Al-Bagary, Ramzia I; El-Zaher, Asmaa A; Morsy, Fahima A; Fouad, Mai M

    2014-01-01

    Aqueous alkaline degradation was performed for oseltamivir phosphate (OP) and valacyclovir hydrochloride (VA). Isocratic stability indicating the use of high-performance liquid chromatography (HPLC) was presented for each drug in the presence of its degradation product. The separations were performed using the Nucleosil ODS column and a mobile phase consisting of phosphate buffer (pH = 7), acetonitrile, and methanol 50:25:25 (v/v/v) for OP. For VA separation, a Nucleosil CN column using phosphate buffer (pH = 7) and methanol 85:15 (v/v) was used as a mobile phase. Ultraviolet detection at 210 nm and 254 nm was used for OP and VA, respectively. The method showed high sensitivity concerning linearity, accuracy, and precision over the range 1–250 ?g mL?1 for both drugs. The proposed method was used to determine the drug in its pharmaceutical formulation and to investigate the degradation kinetics of each drug’s alkaline-stressed samples. The reactions were found to follow a first-order reaction. The activation energy could also be estimated. International Conference on Harmonisation guidelines were adopted for method validation. PMID:24932100

  1. Validated stability-indicating HPLC method for the determination of mesna in presence of its degradation products.

    PubMed

    Rizk, Mohamed; Taha, Elham A; Mowaka, Shereen; Abdallah, Youmna M

    2015-01-01

    A rapid and simple stability-indicating liquid chromatographic method was developed and validated for analysis of mesna in the presence of its degradation products in drug substance and drug products in a run time not >5 min. The separation was achieved on a RP amide C16 column at room temperature using methanol-phosphate buffer (10:90, v/v, pH 3.0) as mobile phase at a flow rate of 1 mL min(-1) and UV detection at 210 nm. The detector response for mesna was linear over the selected concentration range from 50 to 1000 µg mL(-1) with a correlation coefficient 0.9998. The limit of detection and the limit of quantitation were 7.5 and 22.7 µg mL(-1), respectively. The solution was stable for at least 5 days. Baseline resolution between mesna and its degradation products was achieved. Diode array detection peak purity tests showed no peak interfered with mesna peak. Moreover, the method was successfully applied for the determination of mesna in two different commercially available drug products. PMID:25238767

  2. Sunlight Inactivation of Fecal Indicator Bacteria and Bacteriophages from Waste Stabilization Pond Effluent in Fresh and Saline Waters

    PubMed Central

    Sinton, Lester W.; Hall, Carollyn H.; Lynch, Philippa A.; Davies-Colley, Robert J.

    2002-01-01

    Sunlight inactivation in fresh (river) water of fecal coliforms, enterococci, Escherichia coli, somatic coliphages, and F-RNA phages from waste stabilization pond (WSP) effluent was compared. Ten experiments were conducted outdoors in 300-liter chambers, held at 14°C (mean river water temperature). Sunlight inactivation (kS) rates, as a function of cumulative global solar radiation (insolation), were all more than 10 times higher than the corresponding dark inactivation (kD) rates in enclosed (control) chambers. The overall kS ranking (from greatest to least inactivation) was as follows: enterococci > fecal coliforms ? E. coli > somatic coliphages > F-RNA phages. In winter, fecal coliform and enterococci inactivation rates were similar but, in summer, enterococci were inactivated far more rapidly. In four experiments that included freshwater-raw sewage mixtures, enterococci survived longer than fecal coliforms (a pattern opposite to that observed with the WSP effluent), but there was little difference in phage inactivation between effluents. In two experiments which included simulated estuarine water and seawater, sunlight inactivation of all of the indicators increased with increasing salinity. Inactivation rates in freshwater, as seen under different optical filters, decreased with the increase in the spectral cutoff (50% light transmission) wavelength. The enterococci and F-RNA phages were inactivated by a wide range of wavelengths, suggesting photooxidative damage. Inactivation of fecal coliforms and somatic coliphages was mainly by shorter (UV-B) wavelengths, a result consistent with photobiological damage. Fecal coliform repair mechanisms appear to be activated in WSPs, and the surviving cells exhibit greater sunlight resistance in natural waters than those from raw sewage. In contrast, enterococci appear to suffer photooxidative damage in WSPs, rendering them susceptible to further photooxidative damage after discharge. This suggests that they are unsuitable as indicators of WSP effluent discharges to natural waters. Although somatic coliphages are more sunlight resistant than the other indicators in seawater, F-RNA phages are the most resistant in freshwater, where they may thus better represent enteric virus survival. PMID:11872459

  3. Stability-indicating methods for determining omeprazole and octylonium bromide in the presence of their degradation products.

    PubMed

    el-Kousy, N M; Bebawy, L I

    1999-01-01

    Four stability-indicating assays were developed for determining omeprazole and octylonium bromide. Omeprazole is photodegraded and estimated in the presence of its degradation products sulphenamide (I) and benzimidazole sulphide (II) by 2 methods. The first method depends on use of first-, second-, and third-derivative spectrophotometry at 290.4, 320.6, and 311.6 nm, respectively. The second method is based on applying the charge-transfer technique with chloranil as pi acceptor to form a complex with omeprazole, the absorbance of which is measured at 377 nm. These methods determine omeprazole in concentration ranges of 5-20 micrograms/mL by first-, second-, and third-derivative spectrophotometry and 10-50 micrograms/mL by charge-transfer complexation with mean accuracies of 99.92 +/- 0.73, 99.71 +/- 1.02, 99.64 +/- 0.66, and 100.24 +/- 0.81%, respectively. Octylonium bromide is determined by a densitometric method using thin-layer chromatography in the presence of its degradation products p-[2-(n-octyoxy)benzoyl]-aminobenzoic acid (III) and diethyl-(2-hydroxyethyl)-methyl ammonium bromide (IV) without any interferences. Alternatively, octylonium bromide is evaluated by a colorimetric method using the acid dye rose bengal. The ion pair formed is extracted in chloroform at pH 4, and its absorbance is measured at 562 nm. These methods determine octylonium bromide in the presence of its degradation products in concentration ranges of 0.1-0.5 microgram/microL by densitometry and 4.5-22.5 micrograms/mL by colorimetry, with mean accuracies of 100.21 +/- 0.93 and 99.73 +/- 0.89%, respectively. The suggested methods were used to determine drugs in bulk powder, laboratory-prepared mixtures, and pharmaceutical dosage forms. Results were compared statistically with those obtained with reference methods. PMID:10367377

  4. Stability indicating spectrophotometric and spectrodensitometric methods for the determination of diatrizoate sodium in presence of its degradation product.

    PubMed

    Abd El-Rahman, Mohamed K; Riad, Safaa M; Abdel Gawad, Sherif A; Fawaz, Esraa M; Shehata, Mostafa A

    2015-02-01

    Three sensitive, selective, and precise stability indicating methods for the determination of the X-ray contrast agent, diatrizoate sodium (DTA), in the presence of its acidic degradation product (highly cytotoxic 3,5 diamino metabolite) and in pharmaceutical formulation were developed and validated. The first method is a first derivative (D1) spectrophotometric one, which allows the determination of DTA in the presence of its degradate at 231.2 nm (corresponding to zero crossing of the degradate) over a concentration range of 2-24 ?g/mL with mean percentage recovery 99.95±0.97%. The second method is the first derivative of the ratio spectra (DD1) by measuring the peak amplitude at 227 nm over the same concentration range as D1 spectrophotometric method, with mean percentage recovery 99.99±1.15%. The third method is a TLC-densitometric one, where DTA was separated from its degradate on silica gel plates using chloroform:methanol:ammonium hydroxide (20:10:2 by volume) as a developing system. This method depends on quantitative densitometric evaluation of thin layer chromatogram of DTA at 238 nm over a concentration range of 4-20 ?g/spot, with mean percentage recovery 99.88±0.89%. The selectivity of the proposed methods was tested using laboratory-prepared mixtures. The proposed methods have been successfully applied to the analysis of DTA in pharmaceutical dosage forms without interference from other dosage form additives. The results were statistically compared with the official US pharmacopeial method. No significant difference for either accuracy or precision was observed. PMID:25456658

  5. Development and validation of three stability-indicating methods for determination of bisacodyl in pure form and pharmaceutical preparations.

    PubMed

    Metwally, Fadia H; Abdelkawy, Mohammed; Naguib, Ibrahim A

    2007-01-01

    Three new, simple, sensitive, and accurate stability-indicating methods were developed for quantitative determination of bisacodyl in the presence of its degradation products, monoacetyl bisacodyl (I) and desacetyl bisacodyl (II), in enteric coated tablets, suppositories, and raw material. The first is a spectrodensitometric method in which the drug is separated from I and II on silica gel plates using chloroform-acetone (9 + 1, v/v) as the mobile phase with ultraviolet detection of the separated bands at 223 nm over a concentration range of 0.2-1.4 microg/band for bisacodyl with mean recovery 100.35 +/- 1.923%. The second method is fourth derivative D4 spectrophotometry, which allows determination of bisacodyl in the presence of its degradation products in raw material at 223 nm using acetonitrile as the solvent with adherence to Beer's law over the concentration range 2-18 microg/mL with mean recovery 99.77+/-1.056%. In the third method, the spectrophotometric data of bisacodyl, I, and II using absolute ethanol as solvent were processed by 3 chemometric techniques: classical least-squares, principal component regression, and partial least-squares. A training set consisting of 15 mixtures containing different ratios of bisacodyl, I, and II was used for construction of the 3 models. A validation set consisting of 6 mixtures was used to validate the prediction ability of the suggested models. The 3 chemometric methods were applicable over a concentration range between 2-14microg/mL for bisacodyl with mean recovery of 99.97+/-0.865, 100.01 +/- 0.749, and 99.97 +/- 0.616% for the 3 models, respectively. The proposed methods were checked using laboratory-prepared mixtures and were successfully applied to the analysis of raw material and pharmaceutical formulations containing bisacodyl, except for the second method that applies only for raw material. The validity of the suggested procedures was further assessed by applying the standard addition technique; the recoveries obtained were in accordance with those given by the reference method. PMID:17373442

  6. Development and stability of semisolid preparations based on a supercritical CO2 Arnica extract.

    PubMed

    Bilia, Anna Rita; Bergonzi, Maria Camilla; Mazzi, Giovanni; Vincieri, Franco Francesco

    2006-05-01

    Conventional herbal drug preparations (HDP) based on Arnica montana L. have a low content of the active principles, sesquiterpene lactones, which show poor stability and low physical compatibility in semisolid formulations. Recently, an innovative supercritical carbon dioxide (CO2) extract with high sesquiterpene content has been marketed. Development of six semisolid preparations (cetomacrogol, polysorbate 60, polawax, anphyphil, natrosol and sepigel) based on this innovative CO2 extract is discussed. Stability of these preparations was investigated according to ICH guidelines. The evaluation of in vitro release of active constituents was performed using the cell method reported in the European Pharmacopoeia. Preliminary data on in vivo permeation of three selected formulations is demonstrated using the "skin stripping" test, according to the FDA, in healthy subjects. Analysis of sesquiterpene lactones within the extract and in vitro and in vivo studies was performed by RP-HPLC-DAD-MS method. The cetomacrogol showed the best release profile in the in vitro test, while in the in vivo test the best preparation resulted polysorbate 60 and polawax. PMID:16457981

  7. On the possibility of the space-dependence of the stability indicator (decay ratio) of a BWR

    E-print Network

    Pázsit, Imre

    Christophe Demazie`re *, Imre Pa´zsit Department of Reactor Physics, Chalmers University of Technology, SE to the discontinuous dependence of the decay ratio (DR) on the working point of the reactor on the power-flow map (Van ratio (DR) which is used to quantify the stability properties of boiling water reactors (BWRs

  8. A Fast, Stability-Indicating, and Validated Liquid Chromatography Method for the Purity Control of Lercanidipine Hydrochloride in Tablet Dosage Form

    PubMed Central

    Mehta, Saumil; Singh, Sukhdev; Chikhalia, Kishor

    2014-01-01

    A robust, sensitive, and stability-indicating rapid resolution liquid chromatography method for the simultaneous determination of process impurities and degradation products of lercanidipine hydrochloride in pharmaceutical dosage form was developed and validated. The chromatographic separation was performed on the Zorbax SB C18 [(50 × 4.6) mm] 1.8 ?m column, using gradient elution of a potassium dihydrogen phosphate buffer (pH 3.5, 0.01 M) and acetonitrile. The flow rate was 1.0 ml/min and UV detection was performed at 220 nm. The method was further evaluated for its stability-indicating capability by hydrolytic, oxidative, thermal, thermal with moisture, and photolytic degradation studies. All acceptance criteria of the International Conference on Harmonization guidelines for validation were covered in the method validation. This method can be used for purity control during manufacture and real time stability studies. A shorter run time of 10 minutes and good solution stability for at least 48 hours allowed the quantification of more than 50 samples per day with comparatively lower costs than existing methods. PMID:24959405

  9. Simultaneous determination of some water-soluble vitamins and preservatives in multivitamin syrup by validated stability-indicating high-performance liquid chromatography method

    Microsoft Academic Search

    Stojanka Vidovi?; Biljana Stojanovi?; Jelena Veljkovi?; Ljiljana Praži?-Arsi?; Goran Rogli?; Dragan Manojlovi?

    2008-01-01

    HPLC stability-indicating method has been developed for the simultaneous determination of some water-soluble vitamins (ascorbic acid, thiamine hydrochloride, riboflavin-5?-phosphate sodium, pyridoxine hydrochloride, nicotinamide, d(+)-panthenol) and two preservatives (methylparaben and sodium benzoate) in multivitamin syrup preparation. Water-soluble vitamins, preservatives and their degradants were separated on Zorbax SB-Aq (C18) (250mm×4.6mm, 5?m) column at an ambient temperature. Combined isocratic and gradient elution was

  10. A VALIDATED STABILITY INDICATING HPTLC METHOD FOR SIMULTANEOUS ESTIMATION OF CEFPODOXIME PROXETIL AND POTASSIUM CLAVULANATE IN BULK AND TABLET DOSAGE FORM

    Microsoft Academic Search

    A. B. Thomas; S. B. Dighe; R. K. Nanda; L. P. Kothapalli; S. N. Jagdale; A. D. Deshpande

    2010-01-01

    Cefpodoxime proxetil (Cef) and Potassium clavulanate (Pot.clav.) are used in the treatment of acute otitis media, typhoid fever, pharyngitis and tonsillitis. A simple, selective and stability indicating HPTLC method has been established for the simultaneous analysis of Cef and Pot.clav. in pharmaceutical formulations. The method uses aluminum-backed silica gel 60F254 HPTLC plates as stationary phase with toluene:methanol:chloroform:acetonitrile [4:3:2:1.5 (v\\/v\\/v\\/v)] as

  11. Stability-indicating spectrophotometric methods for determination of tazarotene in the presence of its alkaline degradation product by derivative spectrophotometric techniques.

    PubMed

    Badawy, Amr M; El-Alim, Abd El-Aziz B Abd; Saad, Ahmed S

    2010-03-01

    The stability of tazarotene (TZ) was investigated and two stability-indicating methods-namely, first derivative and a derivative ratio spectrophotometric method-were used to determine tazarotene in the presence of its alkaline degradation product (HD) using methanol as a solvent. A linear relationship was obtained in the range 1-10 µg ml?¹ for both methods. By applying the proposed methods, it was possible to determine tazarotene in its pure powdered from with accuracy 99.35 ± 1.410 (n = 10) for the first derivative method and 99.45 ± 1.053 (n = 10) for the derivative ratio method. First derivative and derivative ratio methods were used for the analysis of laboratory-prepared mixtures containing different ratios of tazarotene and its degradation product and they were valid in the presence of up to 70% and 80% degradation product, respectively. The proposed methods were validated and found to be suitable as stability-indicating assay methods for tazarotene in pharmaceutical formulations. PMID:20878894

  12. Integrated community profiling indicates long-term temporal stability of the predominant faecal microbiota in captive cheetahs.

    PubMed

    Becker, Anne A M J; Janssens, Geert P J; Snauwaert, Cindy; Hesta, Myriam; Huys, Geert

    2015-01-01

    Understanding the symbiotic relationship between gut microbes and their animal host requires characterization of the core microbiota across populations and in time. Especially in captive populations of endangered wildlife species such as the cheetah (Acinonyx jubatus), this knowledge is a key element to enhance feeding strategies and reduce gastrointestinal disorders. In order to investigate the temporal stability of the intestinal microbiota in cheetahs under human care, we conducted a longitudinal study over a 3-year period with bimonthly faecal sampling of 5 cheetahs housed in two European zoos. For this purpose, an integrated 16S rRNA DGGE-clone library approach was used in combination with a series of real-time PCR assays. Our findings disclosed a stable faecal microbiota, beyond intestinal community variations that were detected between zoo sample sets or between animals. The core of this microbiota was dominated by members of Clostridium clusters I, XI and XIVa, with mean concentrations ranging from 7.5-9.2 log10 CFU/g faeces and with significant positive correlations between these clusters (P<0.05), and by Lactobacillaceae. Moving window analysis of DGGE profiles revealed 23.3-25.6% change between consecutive samples for four of the cheetahs. The fifth animal in the study suffered from intermediate episodes of vomiting and diarrhea during the monitoring period and exhibited remarkably more change (39.4%). This observation may reflect the temporary impact of perturbations such as the animal's compromised health, antibiotic administration or a combination thereof, which temporarily altered the relative proportions of Clostridium clusters I and XIVa. In conclusion, this first long-term monitoring study of the faecal microbiota in feline strict carnivores not only reveals a remarkable compositional stability of this ecosystem, but also shows a qualitative and quantitative similarity in a defined set of faecal bacterial lineages across the five animals under study that may typify the core phylogenetic microbiome of cheetahs. PMID:25905625

  13. Improved efficiency and stability of secnidazole – An ideal delivery system

    PubMed Central

    Khan, Salman; Haseeb, Mohd; Baig, Mohd Hassan; Bagga, Paramdeep Singh; Siddiqui, H.H.; Kamal, M.A.; Khan, Mohd Sajid

    2014-01-01

    Secnidazole (?,2-Dimethyl-5-nitro-1H-imidazole-1-ethanol) is a highly effective drug against a variety of G+/G? bacteria but with significant side effects because it is being used in very high concentration. In this study, gold nanoparticles (GNPS) were selected as a vehicle to deliver secnidazole drug at the specific site with more accuracy which made the drug highly effective at substantially low concentrations. The as-synthesized GNPs were capped with Human Serum Albumin (HSA) and subsequently bioconjugated with secnidazole because HSA provides the stability and improves the solubility of the bioconjugated drug, secnidazole. The quantification of covalently bioconjugated secnidazole with HSA encapsulated on enzymatically synthesized GNPs was done with RP-HPLC having SPD-20 A UV/VIS detector by using the C-18 column. The bioconjugation of GNPs with secnidazole was confirmed by Transmission Electron Microscopy (TEM) and Dynamic Light Scattering (DLS). The bioconjugated GNPs were characterized by UV–VIS spectroscopy, TEM, Scanning Electron Microscopy (SEM) and DLS. Zeta potential confirmed the stability and uniform distribution of particles in the emulsion of GNPs. The separation of bioconjugated GNPs, unused GNPs and unused drug was done by gel filtration chromatography. The minimal inhibitory concentration of secnidazole-conjugated gold nanoparticles (Au-HSA-Snd) against Klebsiella pneumonia (NCIM No. 2957) and Bacillus cereus (NCIM No. 2156) got improved by 12.2 times and 14.11 times, respectively, in comparison to pure secnidazole. Precisely, the MIC of Au-HSA-Snd against K. pneumonia (NCIM No. 2957) and B. cereus (NCIM No. 2156) were found to be 0.35 and 0.43 ?g/ml, respectively whereas MIC of the pure secnidazole drug against the same bacteria were found to be 4.3 and 6.07 ?g/ml, respectively. PMID:25561882

  14. Microwave heating of different commercial categories of olive oil: Part I. Effect on chemical oxidative stability indices and phenolic compounds

    Microsoft Academic Search

    Lorenzo Cerretani; Alessandra Bendini; Maria Teresa Rodriguez-Estrada; Elena Vittadini; Emma Chiavaro

    2009-01-01

    The effect of microwave heating of extra virgin olive oil (EVOo), olive oil (Oo) and pomace olive oil (Po) in domestic appliances, was investigated in terms of chemical oxidative indices (peroxide, p-anisidine and Totox values), free acidity, water content, total phenol content and different classes of phenolic compounds.Water content of unheated EVOo was higher as compared to the other two

  15. The Stability of Rankings Derived from Composite Indicators: Analysis of the "IL Sole 24 Ore" Quality of Life Report

    ERIC Educational Resources Information Center

    Lun, G.; Holzer, D.; Tappeiner, G.; Tappeiner, U.

    2006-01-01

    The calculation of composite indicators and the derivation of respective rankings is a common method used to benchmark countries or regions. However, although the statistical robustness of these rankings is often criticised, they often still spark off heated political debate. Here, we assess the sensitivity of the province ranking published by the…

  16. The stability of adenosine deaminase and adenosine monophosphate (AMP) deaminase as potential spoilage indicators for postmortem ice stored shrimp 

    E-print Network

    Cheuk, Wai Lun

    1978-01-01

    indicated the impor- tance of bacterial ammonia production. ACKNOWLEDGMENTS Sincere gratitude is expressed to Dr. Ranzell Nickelson, II and Dr. Gunner Finne for suggesting the research program. I am greatly indebted to them for their generous support.... The bacteriology of Gulf coast shrimp. 4. Bacteriological, chemical and organoleptical changes with ice storage. Food Technol. 6:125. Cobb III, B. F. , Alaniz, I. and Thompson, C. A. , Jr. 1973a. Biochemical and microbial studies on shrimp: Voltile nitrogen...

  17. Validated Stability indicating Spectrophotometric Method for the Determination of Acetazolamide in Dosage Forms through Complex Formation with Palladium (II)

    PubMed Central

    Walash, M. I.; El-Brashy, A.; El-Enany, N.; Wahba, M. E. K.

    2010-01-01

    A simple and sensitive spectrophotometric method was developed for the determination of acetazolamide (ACM) in pure form and pharmaceutical preparations. The proposed method is based on the complex formation of acetazolamide with Palladium (II) chloride in acetate buffer pH5.4 and measuring the absorbance at 308 nm. The absorbance- concentration plot was rectilinear over the concentration range of 5-70 ?g/ml with a minimum detection limit (LOD) of 0.98 ?g/ml, limit of quantification (LOQ) of 2.96 ?g/ml, and a molar absorptivity ?=2.7 × 103 L/mol.cm. The factors affecting the absorbance of the formed complex were carefully studied and optimized. The composition of the complex as well as its stability constant was also investigated. The proposed method was applied for the determination of acetazolamide in its tablets and the results obtained were favorably compared with those obtained using the official method. A proposal of the reaction pathway was postulated. PMID:23675188

  18. Stability-indicating HPLC-UV for the determination of 4-bromomethyl-3-nitrobenzoic acid, a bioactive nitrocompound.

    PubMed

    de Freitas, Maria Betânia; Lages, Eduardo Burgarelli; Gonçalves, Isadora Marques Brum; de Oliveira, Renata Barbosa; Vianna-Soares, Cristina Duarte

    2014-07-01

    The nitroaromatic compound 4-bromomethyl-3-nitrobenzoic acid (ANB) is a promising antitumoral agent whose activity has recently been investigated. Forced degradation studies were conducted on ANB with a high-performance liquid chromatography-ultraviolet assay to establish its stability and selectivity. ANB was subjected to degradation studies under hydrolytic (acid and alkaline), oxidative and light exposition conditions. The compound showed greater lability only in acid and alkaline conditions by forming a major degradation product. The chromatographic separation of ANB and its degradation product was achieved on an octadecylsilane column using a mobile phase of methanol-water (80:20, v/v), pH 4.0 adjusted with formic acid, flow rate of 0.7 mL/min, ultraviolet diode array detection at ? 271 nm, injection volume of 20 µL and temperature of 30°C. The method was validated according to International Conference on Harmonization guidelines with respect to precision (average relative standard deviation 0.67%), accuracy (average 99.97%), linearity (y = 118730x + 12912; coefficient of determination > 0.999), specificity and robustness (p > 0.05). The degradation product formed as a result from the hydrolysis of nitrobenzyl bromide, corresponded to its benzyl alcohol, 4-hydroxymethyl-3-nitrobenzoic acid (ANOH) and was characterized by co-elution with a synthetic ANOH working standard. PMID:23788018

  19. Development and Validation of Stability-Indicating High Performance Liquid Chromatographic (HPLC) and DD1-Spectrophotometric Assays for Etodolac in Bulk Form and in Pharmaceutical Dosage Form

    Microsoft Academic Search

    Ola A. Saleh; Aida A. El-Azzouny; Amr M. Badawey; Mohamed S. Rashed

    2009-01-01

    A stability-indicating reversed phase high performance liquid chromatographic assay procedure has been developed and validated for etodolac. The liquid chromatographic separation was achieved isocratically on C18 Zorbax ODS using a mobile phase containing methanol: water: acetic acid (70:30:0.1%, v\\/v\\/v), at a flow rate 1 mL\\/min and UV detection at 254 nm. The method was linear over the concentration range of 2.4–16 µg\\/mL (r = 0.9999)

  20. Altered Neuronal Markers Following Treatment with Mood Stabilizer and Antipsychotic Drugs Indicate an Increased Likelihood of Neurotransmitter Release

    PubMed Central

    Dean, Brian

    2012-01-01

    Objective Given the ability of mood stabilizers and antipsychotics to promote cell proliferation, we wanted to determine the effects of these drugs on neuronal markers previously reported to be altered in subjects with psychiatric disorders. Methods Male Sprauge-Dawley rats were treated with vehicle (ethanol), lithium (25.5 mg per day), haloperidol (0.1 mg/kg), olanzapine (1.0 mg/kg) or a combination of lithium and either of the antipsychotic drugs for 28 days. Levels of cortical synaptic (synaptosomal associated protein-25, synaptophysin, vesicle associated protein and syntaxin) and structural (neural cell adhesion molecule and alpha-synuclein) proteins were determined in each treatment group using Western blots. Results Compared to the vehicle treated group; animals treated with haloperidol had greater levels of synaptosomal associated protein-25 (p<0.01) and neural cell adhesion molecule (p<0.05), those treated with olanzapine had greater levels of synaptophysin (p<0.01) and syntaxin (p<0.01). Treatment with lithium alone did not affect the levels of any of the proteins. Combining lithium and haloperidol resulted in greater levels of synaptophysin (p<0.01), synaptosomal associated protein-25 (p<0.01) and neural cell adhesion molecule (p<0.01). The combination of lithium and olanzapine produced greater levels of synaptophysin (p<0.01) and alpha-synuclein (p<0.05). Conclusion Lithium alone had no effect on the neuronal markers. However, haloperidol and olanzapine affected different presynaptic markers. Combining lithium with olanzapine additionally increased alpha-synuclein. These drug effects need to be taken into account by future studies examining presynaptic and neuronal markers in tissue from subjects with psychiatric disorders. PMID:23429852

  1. A Stability-Indicating HPLC-DAD Method for Determination of Stiripentol: Development, Validation, Kinetics, Structure Elucidation and Application to Commercial Dosage Form.

    PubMed

    Darwish, Hany W; Abdelhameed, Ali S; Attia, Mohamed I; Bakheit, Ahmed H; Khalil, Nasr Y; Al-Majed, Abdulrahman A

    2014-01-01

    A rapid, simple, sensitive, and accurate isocratic reversed-phase stability-indicating high performance liquid chromatography method has been developed and validated for the determination of stiripentol and its degradation product in its bulk form and pharmaceutical dosage form. Chromatographic separation was achieved on a Symmetry C18 column and quantification was achieved using photodiode array detector (DAD). The method was validated in accordance with the ICH requirements showing specificity, linearity (r (2) = 0.9996, range of 1-25??g/mL), precision (relative standard deviation lower than 2%), accuracy (mean recovery 100.08 ± 1.73), limits of detection and quantitation (LOD = 0.024 and LOQ = 0.081??g/mL), and robustness. Stiripentol was subjected to various stress conditions and it has shown marked stability under alkaline hydrolytic stress conditions, thermal, oxidative, and photolytic conditions. Stiripentol degraded only under acidic conditions, forming a single degradation product which was well resolved from the pure drug with significantly different retention time values. This degradation product was characterized by (1)H-NMR and (13)C-NMR spectroscopy as well as ion trap mass spectrometry. The results demonstrated that the method would have a great value when applied in quality control and stability studies for stiripentol. PMID:25371844

  2. A Rapid, Stability Indicating RP-UPLC Method for Simultaneous Determination of Ambroxol Hydrochloride, Cetirizine Hydrochloride and Antimicrobial Preservatives in Liquid Pharmaceutical Formulation

    PubMed Central

    Trivedi, Rakshit Kanubhai; Patel, Mukesh C.; Jadhav, Sushant B.

    2011-01-01

    A stability indicating reversed phase ultra performance liquid chromatography (RP-UPLC) method was developed for simultaneous determination of ambroxol hydrochloride (AMB), cetirizine hydrochloride (CTZ), methylparaben (MP) and propylparaben (PP) in liquid pharmaceutical formulation. The desired chromatographic separation was achieved on an Agilent Eclipse plus C18, 1.8 ?m (50 × 2.1 mm) column using gradient elution at 237 nm detector wavelength. The optimized mobile phase consists of a mixture of 0.01 M phosphate buffer and 0.1 % triethylamine as a solvent-A and acetonitrile as a solvent-B. The developed method separates AMB, CTZ, MP and PP in presence of twelve known impurities/degradation products and one unknown degradation product within 3.5 min. Stability indicating capability was established by forced degradation experiments and seperation of known and unknown degradation products. The lower limit of quantification was established for AMB, CTZ, MP and PP. The developed RP-UPLC method was validated according to the International Conference on Harmonization (ICH) guidelines. This validated method is applied for simultaneous estimation of AMB, CTZ, MP and PP in commercially available syrup samples. Further, the method can be extended for estimation of AMB, CTZ, MP, PP and levo-cetirizine (LCTZ) in various commercially available dosage forms. PMID:21886901

  3. A Validated Stability-Indicating RP-UPLC Method for Simultaneous Determination of Desloratadine and Sodium Benzoate in Oral Liquid Pharmaceutical Formulations

    PubMed Central

    Kumar, Navneet; Sangeetha, Dhanaraj; Reddy, Pingili Sunil; Prakash, Lakkireddy

    2012-01-01

    A novel, sensitive and selective stability-indicating gradient reverse phase ultra performance liquid chromatographic method was developed and validated for the quantitative determination of desloratadine and sodium benzoate in pharmaceutical oral liquid formulation. The chromatographic separation was achieved on Acquity BEH C8 (100 mm × 2.1 mm) 1.7 ?m column by using mobile phase containing a gradient mixture of solvent A (0.05 M KH2PO4 and 0.07 M triethylamine, pH 3.0) and B (50:25:25 v/v/v mixture of acetonitrile, methanol and water) at flow rate of 0.4 mL/min. Column temperature was maintained at 40°C and detection was carried out at a wavelength of 272 nm. The described method shows excellent linearity over a range of 0.254 ?g/mL to 76.194 ?g/mL for desloratadine and 1.006 ?g/mL to 301.67 ?g/mL for sodium benzoate. The correlation coefficient for desloratadine and sodium benzoate was more than 0.999. To establish stability-indicating capability of the method, drug product was subjected to the stress conditions of acid, base, oxidative, hydrolytic, thermal and photolytic degradation. The degradation products were well resolved from desloratadine and sodium benzoate. The developed method was validated as per international ICH guidelines with respect to specificity, linearity, LOD, LOQ, accuracy, precision and robustness. PMID:22396911

  4. Stress Degradation Behavior of Abacavir Sulfate and Development of a Suitable Stability-Indicating UHPLC Method for the Determination of Abacavir, its Related Substances, and Degradation Products

    PubMed Central

    Vukkum, Pallavi; Deshpande, Girish R.; Babu, J. Moses; Muralikrishna, R.; Jagu, Pavani

    2012-01-01

    A novel, stability-indicating UHPLC method was developed for the quantitative determination of Abacavir sulfate, its related substances, and forced degradation impurities in bulk drugs. The chromatographic separation was achieved on a Waters Acquity BEH C8, 50 mm × 2.1 mm, 1.7 ?m particle size column with a mobile containing a gradient mixture of solution A (0.10 % v/v o-phosphoric acid in water) and solution B (0.10% v/v o-phosphoric acid in methanol). The flow rate was set at 0.40 mL/min and the run time was 6.0 min. The drug substance was subjected to the stress studies of hydrolysis, oxidation, photolysis, and thermal degradation. Abacavir sulfate was found to degrade significantly under acidic hydrolysis and oxidative stress conditions. The formed degradation products were reported and were well-resolved from Abacavir and its related substances. The mass balance was found to be satisfactory in all of the stress conditions, thus proving the stability-indicating capability of the method. The developed UHPLC method was validated to be in agreement with ICH requirements and found to be rapid, accurate, precise, linear, specific, and suitable for the quantitative determination of related substances and degradants in the bulk drug samples of Abacavir sulfate. PMID:23264939

  5. A Stability-Indicating HPLC-DAD Method for Determination of Ferulic Acid into Microparticles: Development, Validation, Forced Degradation, and Encapsulation Efficiency

    PubMed Central

    Toledo, Maria da Graça; Pupo, Yasmine Mendes; Padilha de Paula, Josiane; Zanin, Sandra Maria Warumby

    2015-01-01

    A simple stability-indicating HPLC-DAD method was validated for the determination of ferulic acid (FA) in polymeric microparticles. Chromatographic conditions consisted of a RP C18 column (250?mm × 4.60?mm, 5??m, 110?Å) using a mixture of methanol and water pH 3.0 (48?:?52?v/v) as mobile phase at a flow rate of 1.0?mL/min with UV detection at 320?nm. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of quantification, limit of detection, accuracy, precision, and robustness provided suitable results regarding all parameters investigated. The calibration curve was linear in the concentration range of 10.0–70.0??g/mL with a correlation coefficient >0.999. Precision (intraday and interday) was demonstrated by a relative standard deviation lower than 2.0%. Accuracy was assessed by the recovery test of FA from polymeric microparticles (99.02% to 100.73%). Specificity showed no interference from the components of polymeric microparticles or from the degradation products derived from acidic, basic, and photolytic conditions. In conclusion, the method is suitable to be applied to assay FA as bulk drug and into polymeric microparticles and can be used for studying its stability and degradation kinetics. PMID:26075139

  6. Characterization of a potential medium for 'biorelevant' in vitro release testing of a naltrexone implant, employing a validated stability-indicating HPLC method.

    PubMed

    Iyer, Sunil S; Barr, William H; Karnes, H Thomas

    2007-02-19

    A variety of factors have been recognized that influence media optimization for drug release studies of implant dosage forms. Of primary importance is selection of a medium that physiologically mimics the milieu at the site of administration (a condition termed 'biorelevance'). We describe in this paper, the characterization of Hanks' balanced salts solution, with necessary modification, for application as a 'biorelevant' medium for in vitro release studies of a biodegradable, subcutaneous implant of naltrexone. A detailed investigation of changes in pH, osmolality and ultraviolet (UV) spectrum as a function of time and temperature was conducted. Variation in the parameters evaluated was found to be within acceptable limits. Validation of a simple and selective, high performance liquid chromatography (HPLC) assay method for naltrexone was carried out to evaluate stability. The calibration curves were linear from 0.16 to 20.00 microg ml(-1). Imprecision and inaccuracy were less than 2% and no interference was observed from degradation peaks. Stability studies of naltrexone indicated the media should be replaced every 7-8 days for real-time testing. This was applied to an investigation of in vitro drug release. The method has been proven to be suitable for investigation of naltrexone released from the implant. PMID:17045445

  7. A comparative study between three stability indicating spectrophotometric methods for the determination of diatrizoate sodium in presence of its cytotoxic degradation product based on two-wavelength selection

    NASA Astrophysics Data System (ADS)

    Riad, Safaa M.; El-Rahman, Mohamed K. Abd; Fawaz, Esraa M.; Shehata, Mostafa A.

    2015-06-01

    Three sensitive, selective, and precise stability indicating spectrophotometric methods for the determination of the X-ray contrast agent, diatrizoate sodium (DTA) in the presence of its acidic degradation product (highly cytotoxic 3,5-diamino metabolite) and in pharmaceutical formulation, were developed and validated. The first method is ratio difference, the second one is the bivariate method, and the third one is the dual wavelength method. The calibration curves for the three proposed methods are linear over a concentration range of 2-24 ?g/mL. The selectivity of the proposed methods was tested using laboratory prepared mixtures. The proposed methods have been successfully applied to the analysis of DTA in pharmaceutical dosage forms without interference from other dosage form additives. The results were statistically compared with the official US pharmacopeial method. No significant difference for either accuracy or precision was observed.

  8. Development and validation of a rapid stability indicating HPLC-method using monolithic stationary phase and two spectrophotometric methods for determination of antihistaminic acrivastine in capsules.

    PubMed

    Gouda, Ayman A; Hashem, Hisham; Jira, Thomas

    2014-09-15

    Simple, rapid and accurate high performance liquid chromatographic (HPLC) and spectrophotometric methods are described for determination of antihistaminic acrivastine in capsules. The first method (method A) is based on accurate, sensitive and stability indicating chromatographic separation method. Chromolith® Performance RP-18e column, a relatively new packing material consisting of monolithic rods of highly porous silica, was used as stationary phase applying isocratic binary mobile phase of ACN and 25 mM NaH2PO4 pH 4.0 in the ratio of 22.5:77.5 at flow rate of 5.0 mL/min and 40°C. A diode array detector was used at 254 nm for detection. The elution time of acrivastine was found to be 2.080±0.032. The second and third methods (methods B and C) are based on the oxidation of acrivastine with excess N-bromosuccinimide (NBS) and determination of the unconsumed NBS with, metol-sulphanilic acid (?max: 520 nm) or amaranth dye (?max: 530 nm). The reacted oxidant corresponds to the drug content. Beer's law is obeyed over the concentration range 1.563-50, 2.0-20 and 1.0-10 ?g mL(-1) for methods A, B and C, respectively. The limits of detection and quantitation were 0.40, 0.292 and 0.113 ?g mL(-1) and 0.782, 0.973 and 0.376 ?g mL(-1) for methods A, B and C, respectively. The HPLC method was validated for system suitability, linearity, precision, limits of detection and quantitation, specificity, stability and robustness. Stability tests were done through exposure of the analyte solution for four different stress conditions and the results indicate no interference of degradants with HPLC-method. The proposed methods was favorably applied for determination of acrivastine in capsules formulation. Statistical comparison of the obtained results from the analysis of the studied drug to those of the reported method using t- and F-tests showed no significant difference between them. PMID:24813276

  9. Optimization and Validation of RP-HPLC-UV/Vis Method for Determination Phenolic Compounds in Several Personal Care Products

    PubMed Central

    Akkbik, Mohammed; Assim, Zaini Bin; Ahmad, Fasihuddin Badruddin

    2011-01-01

    An HPLC method with ultraviolet-visible spectrophotometry detection has been optimized and validated for the simultaneous determination of phenolic compounds, such as butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) as antioxidants, and octyl methyl cinnamate (OMC) as UVB-filter in several personal care products. The dynamic range was between 1 to 250?mg/L with relative standard deviation less than 0.25% (n = 4). Limits of detection for BHA, BHT, and OMC were 0.196, 0.170, and 0.478?mg/L, respectively. While limits of quantification for BHA, BHT, and OMC were 0.593, 0.515, and 1.448?mg/L, respectively. The recovery for BHA, BHT, and OMC was ranged from 92.1–105.9%, 83.2–108.9%, and 87.3–103.7%, respectively. The concentration ranges of BHA, BHT, and OMC in 12 commercial personal care samples were 0.13–4.85, 0.16–2.30, and 0.12–65.5?mg/g, respectively. The concentrations of phenolic compounds in these personal care samples were below than maximum allowable concentration in personal care formulation, that is, 0.0004–10?mg/g, 0.002–5?mg/g, and up to 100?mg/g for BHA, BHT, and OMC, respectively. PMID:21760792

  10. Validated RP-HPLC and HPTLC methods for determination of anti-inflammatory bis-indole alkaloid in Desmodium gangeticum.

    PubMed

    Yadav, Akhilesh K; Gupta, Madan M

    2014-01-01

    Here, two simple and accurate methods, namely high-performance liquid chromatography and high-performance thin-layer chromatography for the detection of gangenoid, an anti-inflammatory alkaloid, in a well-known Indian medicinal plant Desmodium gangeticum, are described. The proposed methods were successfully used for the estimation of gangenoid in D. gangeticum root. PMID:24079376

  11. New RP?HPLC Method for the Estimation of 6?Mercaptopurine in Rat Plasma and Various Tissue Homogenates

    Microsoft Academic Search

    M. L. Umrethia; P. K. Ghosh; R. J. Majithiya; R. S. R. Murthy

    2006-01-01

    A reversed?phase high performance liquid chromatography (HPLC) method was developed to determine 6?mercaptopurine (6?MP) in plasma and tissue homogenates of rats in the present study. A known quantity of the drug and internal standard (metronidazole) was spiked in rat plasma and tissue extracts in a range of 50–1000 ng\\/mL and 100–1000 ng\\/mL. The spiked plasma samples were deproteinized using a methanol and

  12. RP?HPLC Assay of Rofecoxib from Pharmaceutical Dosage Forms and Human Plasma and Its Drug Dissolution Studies

    Microsoft Academic Search

    Ayhan Sava?er; Yalçin Özkan; Cansel K. Özkan; Çetin Ta?; Sibel A. Özkan

    2004-01-01

    A high performance liquid chromatographic (HPLC) method is described for the determination of rofecoxib (RFC) in bulk drug, tablets, and human plasma samples. The methods are linear over the concentration ranges 0.005–30.0 and 0.010–10 µg mL in mobile phase and human plasma, respectively. Chromatography was carried out on a reversed phase Spherisorb ODSI column using a mixture of acetonitrile:methanol: 0.067

  13. A validated method for the analysis of diltiazem in raw materials and pharmaceutical formulations by rp-HPLC.

    PubMed

    Sultana, Najma; Arayne, M Saeed; Shafi, Nighat

    2007-10-01

    A simple, selective and rapid reversed phase high performance liquid chromatographic (HPLC) method for the analysis of diltiazem (DTZ) in bulk material and pharmaceutical formulations has been developed and validated. Sample was resolved on a Hypersil, ODS, C-18(150x4.6 mm, 5 micron) column. The mobile phase consisted of methanol-water (80:20 v/v, pH 3.1 adjusted with phosphoric acid) was delivered at a flow rate of 0.5 ml/min at ambient temperature and the retention time was about 2.6 minutes with symmetrical peaks. Studies were performed on an HPLC system equipped with a UV/visible detector at 236 nm. Flurbiprofen (FLR) was used as an internal standard. The developed method gave good resolution between diltiazem and internal standard. The method is specific to DTZ and able to resolve the drug peak from formulation excepients. The calibration curve was linear over the concentration range of 0.195-50 mg/ml (R2=0.999). The proposed method is accurate (the accuracy results were 94.1-99.39 for diltiazem recoveries), precise (The intraday and interday precision CVs were 0.035-2.2 %) and linear within the desired range. The lower limits of detection for DTZ was found to be 0.0184 microg/ml and the quantitation limit was about 0.056 microg/ml and therefore could be employed as a more convenient and efficient option for the analysis of diltiazem and its related compounds in drug substance and formulations. PMID:17604250

  14. Development of an RP?HPLC Method for the Analysis of Phenolic Compounds in Achillea millefolium L

    Microsoft Academic Search

    Raimondas Benetis; Jolita Radušien?; Valdas Jakštas; Valdimaras Janulis; Faustas Malinauskas

    2008-01-01

    Several major phenolic constituents present in yarrow (Achillea millefolium L. s.l.) were determined for a homogenized plant sample. In order to optimize the conditions for sample preparation of the botanical matrix two different solvent extraction methods (maceration and ultrasonic agitation) were assayed. The preliminary maceration studies were performed to determine the influence of extracting solvents on the recovery of phenolics

  15. RP-HPLC method and its validation for the determination of naloxone from a novel transdermal formulation

    Microsoft Academic Search

    Ramesh Panchagnula; Puneet Sharma; Sateesh Khandavilli; Manthena V. S. Varma

    2004-01-01

    The aim of the present work was to develop a simple and reliable liquid chromatographic method for the quantitative determination of naloxone (NLX) in a novel transdermal formulation. Chromatography was carried out by reversed-phase technique on a C-18 column with a mobile phase composed of methanol, acetonitrile and 50 mM phosphate buffer (pH 7) in the proportion of 40:20:40 v\\/v\\/v, at

  16. RP-HPLC method development for the simultaneous determination of timolol maleate and human serum albumin in albumin nanoparticles.

    PubMed

    Boiero, Carolina; Allemandi, Daniel; Longhi, Marcela; Llabot, Juan M

    2015-07-10

    An isocratic high-performance liquid chromatographic method was developed and validated for the simultaneous determination of human serum albumin (HSA) and timolol in albumin nanoparticles. This method involved a reversed-phase-C18 column thermostated at 25°C, UV detection at 276nm, flow rate of 1.0ml/min and a mobile phase compounded by 0.05% (v/v) trifluoroacetic acid in water/0.05% (v/v) trifluoroacetic acid in an acetonitrile (40:60, v/v) solution. The elution times for albumin and timolol were 1.84±0.05min and 2.67±0.04min, respectively. Calibration curves were linear from 0.2 to 100mg/ml for HSA and 0.01 to 1mg/ml for timolol. Limits of quantification were 0.2mg/ml for HSA and 0.01mg/ml for timolol. The values of accuracy and precision of intra- and inter-day variation studies were within acceptable limits, according to the US Food and Drug Administration Guidance for Industry. The described method has proved to be useful to give accurate measurements of human serum albumin and timolol from albumin nanoparticles to determine the percentage of encapsulation and the process yield. PMID:25890214

  17. Identification and RP-HPLC-ESI-MS/MS quantitation of bitter-tasting beta-acid transformation products in beer.

    PubMed

    Haseleu, Gesa; Intelmann, Daniel; Hofmann, Thomas

    2009-08-26

    Thermal treatment of the hop beta-acid colupulone under wort boiling conditions, followed by LC-TOF-MS and 1D/2D NMR spectroscopy, revealed cohulupone, hulupinic acid, nortricyclocolupone, two tricyclocolupone epimers, two dehydrotricyclocolupone epimers, two hydroxytricyclocolupone epimers, and two hydroperoxytricyclocolupone epimers as the major bitter-tasting beta-acid transformation products. Among these compounds, the chemical structures of the hydroxy- as well as the hydroperoxytricyclocolupone epimers have not previously been confirmed by 1D/2D NMR experiments. Depending on their chemical structure, these compounds showed rather low recognition thresholds ranging from 7.9 to 90.3 micromol/L. The lowest thresholds of 7.9 and 14.7 micromol/L were found for cohulupone, imparting a short-lasting, iso-alpha-acid-like bitter impression, and for hydroxytricyclocolupone, exhibiting a long-lasting, lingering, and harsh bitterness perceived on the posterior tongue and throat. Furthermore, HPLC-ESI-MS/MS analysis allowed for the first time a simultaneous detection and quantitation of these bitter-tasting beta-acid transformation products in a range of commercial beer samples without any sample cleanup. Depending on the type of beer, these studies revealed remarkable differences in the concentrations of the individual beta-acid transformation products. PMID:19627140

  18. Effect of the Mobile and Stationary Phases on RP-HPLC Retention and Selectivity of Flavonoid Compounds

    Microsoft Academic Search

    M. C. Pietrogrande; Y. D. Kahie

    1994-01-01

    The retention behaviour of an extended set of flavonoid compounds on phenyl and cyano reversed-phase HPLC columns was studied and compared to behaviour on octadecyl column. The selectivity properties of methanol, acetonitrile and tetrahydrofuran as organic modifiers on each stationary phase are reported. Both the stationary and the mobile phases appeared to significantly change HPLC system selectivity. Specific stationary phase

  19. Determination of itopride hydrochloride in human plasma by RP-HPLC with fluorescence detection and its use in bioequivalence study.

    PubMed

    Ma, Jing; Yuan, Li-Hua; Ding, Mei-Juan; Zhang, Jun; Zhang, Qing; Xu, Qun-Wei; Zhou, Xue-Min

    2009-03-01

    A sensitive, selective and simple method using a precipitation of protein with 10% perchloric acid, followed by high-performance liquid chromatography (HPLC) with fluorescence detection was developed for the determination of itopride hydrochloride in human plasma, using levofloxacin as the internal standard (IS). Chromatographic separation was obtained within 7.0 min using a reverse phase Hypersil BDS C(18) (250 mm x 4.6 mm, 5 microm) column and an isocratic mobile phase, constituting of a mixture of 0.1 mol/l ammonium acetate-methanol (30:70, v/v) flowing at 1.1 ml/min. The excitation and emission wavelengths were set at 304 and 344 nm, respectively. The method was validated over the concentration range of 5 ng/ml to 1000.0 ng/ml. The lower limit of quantitation (LLOQ) was 5 ng/ml. The extractive recovery of itopride hydrochloride from the biological matrix was more than 80.77%. The intra-day accuracy of the drug containing serum samples was more than 82.94% with a precision of 2.81-4.37%. The inter-day accuracy was 82.91% or more, with a precision of 6.89-9.54%. The limit we have used (70-143%) is based on the local regulatory authority (SFDA). The developed method was validated and successfully applied to bioequivalence studies of itopride hydrochloride in healthy male volunteers. PMID:19101632

  20. Development and Validation of RP-HPLC Method for Simultaneous Estimation of Cefpodoxime Proxetil and Dicloxacillin Sodium in Tablets

    PubMed Central

    Acharya, D. R.; Patel, Dipti B.

    2013-01-01

    A simple, accurate, rapid and precise reversed-phase high-performance liquid chromatographic method has been developed and validated for simultaneous determination of cefpodoxime proxetil and dicloxacillin sodium in tablet. The chromatographic separation was carried out on kromasil C18 analytical column (250×4.6 mm; 5 ?m) with a mixture of acetonitrile:methanol:trifloroacetic acid (0.001%) with pH 6.5 (30:50:20, v/v/v) as mobile phase; at a flow rate of 1.0 ml/min. UV detection was performed at 235 nm. The dicloxacillin sodium and cefpodoxime proxetil were eluted at 1.92 and 3.35 min, respectively. The peaks were eluted with better resolution. Calibration plots were linear over the concentration range 0.5-20 ?g/ml for cefpodoxime proxetil (r2=0.9996) and 5-50 ?g/ml for dicloxacillin sodium (r2=0.9987). The method was validated for accuracy, precision, linearity and specificity. The method was very sensitive with limit of detection 0.0726, 0.3685 ?g/ml and limit of quantification 0.220, 1.116 ?g/ml for cefpodoxime proxetil and dicloxacillin sodium, respectively. The high recovery and low relative standard deviation confirm the suitability of the method for routine determination of cefpodoxime proxetil and dicloxacillin sodium in bulk drug and tablet dosage form. PMID:23901158

  1. A rapid stability-indicating, fused-core HPLC method for simultaneous determination of ?-artemether and lumefantrine in anti-malarial fixed dose combination products

    PubMed Central

    2013-01-01

    Background Artemisinin-based fixed dose combination (FDC) products are recommended by World Health Organization (WHO) as a first-line treatment. However, the current artemisinin FDC products, such as ?-artemether and lumefantrine, are inherently unstable and require controlled distribution and storage conditions, which are not always available in resource-limited settings. Moreover, quality control is hampered by lack of suitable analytical methods. Thus, there is a need for a rapid and simple, but stability-indicating method for the simultaneous assay of ?-artemether and lumefantrine FDC products. Methods Three reversed-phase fused-core HPLC columns (Halo RP-Amide, Halo C18 and Halo Phenyl-hexyl), all thermostated at 30°C, were evaluated. ?-artemether and lumefantrine (unstressed and stressed), and reference-related impurities were injected and chromatographic parameters were assessed. Optimal chromatographic parameters were obtained using Halo RP-Amide column and an isocratic mobile phase composed of acetonitrile and 1mM phosphate buffer pH 3.0 (52:48; V/V) at a flow of 1.0 ml/min and 3 ?l injection volume. Quantification was performed at 210 nm and 335 nm for ?-artemether and for lumefantrine, respectively. In-silico toxicological evaluation of the related impurities was made using Derek Nexus v2.0®. Results Both ?-artemether and lumefantrine were separated from each other as well as from the specified and unspecified related impurities including degradants. A complete chromatographic run only took four minutes. Evaluation of the method, including a Plackett-Burman robustness verification within analytical QbD-principles, and real-life samples showed the method is suitable for quantitative assay purposes of both active pharmaceutical ingredients, with a mean recovery relative standard deviation (± RSD) of 99.7 % (± 0.7%) for ?-artemether and 99.7 % (± 0.6%) for lumefantrine. All identified ?-artemether-related impurities were predicted in Derek Nexus v2.0® to have toxicity risks similar to ?-artemether active pharmaceutical ingredient (API) itself. Conclusions A rapid, robust, precise and accurate stability-indicating, quantitative fused-core isocratic HPLC method was developed for simultaneous assay of ?-artemether and lumefantrine. This method can be applied in the routine regulatory quality control of FDC products. The in-silico toxicological investigation using Derek Nexus® indicated that the overall toxicity risk for ?-artemether-related impurities is comparable to that of ?-artemether API. PMID:23631682

  2. The spatial significance of water quality indicators in waste stabilization ponds--limitations of residence time distribution analysis in predicting treatment efficiency.

    PubMed

    Sweeney, D G; Cromar, N J; Nixon, J B; Ta, C T; Fallowfield, H J

    2003-01-01

    Over the past fifty years, considerable research in waste stabilization pond operation has led to the development of a number of models used to describe the hydraulic regime and predict treatment efficiency. Models range in complexity from plug or completely mixed simplifications to computational fluid dynamics (CFD) models which are able to predict flow hydraulics at a local level. Information about the exit age of pond effluent can be used to estimate pollutant decay. However, a mechanistic approach to understanding pond operation highlights the importance of knowing both the time and spatial history of pond effluent. A CFD model of a large pond system was constructed to demonstrate various hydraulic scenarios under different boundary conditions. Two scenarios were compared to visually demonstrate the effects of differing hydraulic conditions. Typical mechanistic models were applied to each condition to quantify biological differences. This simple example indicates that integrating biological and localised flow models will lead to a more holistic understanding of pond operation and treatment efficiency. PMID:14510213

  3. Evaluation of degradation of urinary catecholamines and metanephrines and deconjugation of their sulfoconjugates using stability-indicating reversed-phase ion-pair HPLC with electrochemical detection.

    PubMed

    Chan, E C; Wee, P Y; Ho, P C

    2000-04-01

    The possibility of the deconjugation of urinary catecholamine sulfates (CA-S) and metanephrine sulfates (MN-S) during storage was studied using a reversed-phase ion-pair HPLC method with electrochemical detection. Stability profiles of catecholamines (norepinephrine (NE), epinephrine (E) and dopamine (DA)) and metanephrines (normetanephrine (NM) and metanephrine (MN)) in preserved and unpreserved pooled urine and aqueous samples stored at 10 and 30 degrees C over 8 days were compared. Results showed that these compounds exhibited stable or declining profiles in aqueous samples but fluctuating profiles in pooled urine samples. It was concluded that deconjugation of CA-S and MN-S occurred in both preserved and unpreserved urine samples. Therefore, at 10 and 30 degrees C, levels of detected urinary catecholamines and metanephrines could be affected by both the degradation of the free amines and deconjugation of the CA-S and MN-S. Based on these findings, another batch of unpreserved urine and aqueous samples were prepared and stored at -80 degrees C. Under this condition, all compounds were found to be stable with less than 10% variations in both unpreserved urine and aqueous samples for at least 22 days. These indicated that urine samples could be stored unpreserved at -80 degrees C for at least 3 weeks without significant degradation of the free amines or deconjugation of their sulfoconjugates. PMID:10766369

  4. Stress degradation studies and development of stability-indicating TLC-densitometry method for determination of prednisolone acetate and chloramphenicol in their individual and combined pharmaceutical formulations.

    PubMed

    Musharraf, Syed Ghulam; Fatima, Urooj; Sultana, Rahat

    2012-01-01

    A rapid and reproducible stability indicating TLC method was developed for the determination of prednisolone acetate and chloramphenicol in presence of their degraded products. Uniform degradation conditions were maintained by refluxing sixteen reaction mixtures for two hours at 80°C using parallel synthesizer including acidic, alkaline and neutral hydrolysis, oxidation and wet heating degradation. Oxidation at room temperature, photochemical and dry heating degradation studies were also carried out. Separation was done on TLC glass plates, pre-coated with silica gel 60F-254 using chloroform: methanol (14:1 v/v). Spots at Rf 0.21 ± 0.02 and Rf 0.41 ± 0.03 were recognized as chloramphenicol and prednisolone acetate, respectively. Quantitative analysis was done through densitometric measurements at multiwavelength (243 nm, ?max of prednisolone acetate and 278 nm, ?max of chloramphenicol), simultaneously. The developed method was optimized and validated as per ICH guidelines. Method was found linear over the concentration range of 200-6000 ng/spot with the correlation coefficient (r2 ± S.D.) of 0.9976 ± 3.5 and 0.9920 ± 2.5 for prednisolone acetate and chloramphenicol, respectively. The developed TLC method can be applied for routine analysis of prednisolone acetate and chloramphenicol in presence of their degraded products in their individual and combined pharmaceutical formulations. PMID:22264235

  5. Implementation of design of experiments for optimization of forced degradation conditions and development of a stability-indicating method for furosemide.

    PubMed

    Kurmi, Moolchand; Kumar, Sanjay; Singh, Bhupinder; Singh, Saranjit

    2014-08-01

    The study involved optimization of forced degradation conditions and development of a stability-indicating method (SIM) for furosemide employing the design of experiment (DoE) concept. The optimization of forced degradation conditions, especially hydrolytic and oxidative, was done by application of 2(n) full factorial designs, which helped to obtain the targeted 20-30% drug degradation and also enriched levels of degradation products (DPs). For the selective separation of the drug and its DPs for the development of SIM, DoE was applied in three different stages, i.e., primary parameter selection, secondary parameter screening and method optimization. For these three, IV-optimal, Taguchi orthogonal array and face-centred central composite designs were employed, respectively. The organic modifier, buffer pH, gradient time and initial hold time were selected as primary parameters. Initial and final organic modifier percentage, and flow rate came out as critical parameters during secondary parameter screening, which were further evaluated during method optimization. Based on DoE results, an optimized method was obtained wherein a total of twelve DPs were separated successfully. The study also exposed the degradation behaviour of the drug in different forced degradation conditions. PMID:24742772

  6. Development and validation of stability-indicating high performance liquid chromatography method to analyze gatifloxacin in bulk drug and pharmaceutical preparations

    PubMed Central

    Aljuffali, Ibrahim A.; Kalam, Mohd. Abul; Sultana, Yasmin; Imran, Ahamad; Alshamsan, Aws

    2014-01-01

    Quantitative determination of gatifloxacin in tablets, solid lipid nanoparticles (SLNs) and eye-drops using a very simple and rapid chromatographic technique was validated and developed. Formulations were analyzed using a reverse phase SUPELCO® 516 C-18-DB, 50306-U, HPLC column (250 mm × 4.6 mm, 5 ?m) and a mobile phase consisting of disodium hydrogen phosphate buffer:acetonitrile (75:25, v/v) and with orthophosphoric acid pH was adjusted to 3.3 The flow rate was 1.0 mL/min and analyte concentrations were measured using a UV-detector at 293 nm. The analyses were performed at room temperature (25 ± 2 °C). Gatifloxacin was separated in all the formulations within 2.767 min. There were linear calibration curves over a concentration range of 4.0–40 ?g.mL?1 and correlation coefficients of 0.9998 with an average recovery above 99.91%. Detection of analyte from different dosage forms at the same Rt indicates the specificity and stability of the developed method. PMID:25685047

  7. Validated Stability-Indicating HPLC-DAD Method for the Simultaneous Determination of Diclofenac Sodium and Diflunisal in Their Combined Dosage Form

    PubMed Central

    Shaalan, Rasha A.; Belal, Tarek S.

    2013-01-01

    A simple, rapid, and highly selective HPLC-DAD method was developed for the simultaneous determination of diclofenac sodium (DIC) and diflunisal (DIF) in pure form and in their combined formulation. Effective chromatographic separation was achieved using a Zorbax SB-C8 (4.6×250 mm, 5 ?m particle size) column with a mobile phase composed of 0.05 M phosphoric acid, acetonitrile, and methanol in the ratio of 40:48:12 (by volume). The mobile phase was pumped isocratically at a flow rate of 1 mL/min, and quantification of the analytes was based on measuring their peak areas at 228 nm. The retention times for diflunisal and diclofenac were about 7.9 and 9.5 min, respectively. The reliability and analytical performance of the proposed HPLC procedure were statistically validated with respect to system suitability, linearity, ranges, precision, accuracy, specificity, robustness, detection, and quantification limits. Calibration curves were linear in the ranges of 5–100 ?g/mL for both drugs with correlation coefficients >0.9998. The proposed method proved to be selective and stability-indicating by the resolution of the two analytes from four of their related substances and potential impurities as well as from forced-degradation (hydrolysis, oxidation, photolysis, and dry heat) products. The validated HPLC method was successfully applied to the analysis of DIC and DIF in their combined dosage form (suppositories). The proposed method made use of the diode array detector (DAD) as a tool for peak identity and purity confirmation. PMID:24106669

  8. Simultaneous determination of some water-soluble vitamins and preservatives in multivitamin syrup by validated stability-indicating high-performance liquid chromatography method.

    PubMed

    Vidovi?, Stojanka; Stojanovi?, Biljana; Veljkovi?, Jelena; Prazi?-Arsi?, Ljiljana; Rogli?, Goran; Manojlovi?, Dragan

    2008-08-22

    HPLC stability-indicating method has been developed for the simultaneous determination of some water-soluble vitamins (ascorbic acid, thiamine hydrochloride, riboflavin-5'-phosphate sodium, pyridoxine hydrochloride, nicotinamide, D(+)-panthenol) and two preservatives (methylparaben and sodium benzoate) in multivitamin syrup preparation. Water-soluble vitamins, preservatives and their degradants were separated on Zorbax SB-Aq (C(18)) (250 mm x 4.6 mm, 5 microm) column at an ambient temperature. Combined isocratic and gradient elution was performed with a mobile phase consisting of 0.0125 M hexane-1-sulfonic acid sodium salt in 0.1% (m/v) o-phosphoric acid, pH 2.4-2.5 (solvent A) and acetonitrile (solvent B) at the flow-rate 1 ml min(-1). Starting with solvent A an isocratic elution was performed for 15 min, then the composition was changed to 85% of A and 15% of B during the next 20 min and it was constant for 5 min, then the composition was changed to 70% of A and 30% of B during next 15 min and it was constant for 5 min and finally was changed to 100% of A as at the beginning of the elution. Detection was performed with diode array detector at 210, 230 and 254 nm. Multivitamin syrup preparation was subjected to stress testing (forced degradation) in order to demonstrate that degradants from the vitamins, preservatives and/or product excipients do not interfere with the quantification of vitamins and preservatives. Typical validation characteristics: selectivity, accuracy, precision, linearity, range, limit of quantification and limit of detection were evaluated for vitamins and preservatives. PMID:18644604

  9. Stress Degradation Behavior of Atorvastatin Calcium and Development of a Suitable Stability-Indicating LC Method for the Determination of Atorvastatin, its Related Impurities, and its Degradation Products

    PubMed Central

    Vukkum, Pallavi; Moses Babu, J.; Muralikrishna, R.

    2013-01-01

    A rapid, reversed-phase liquid chromatographic method was developed for the quantitative determination of Atorvastatin calcium, its related substances (12 impurities), and degradation impurities in bulk drugs. The chromatographic separation was achieved on a Zorbax Bonus-RP column by employing a gradient elution with water–acetonitrile–trifluoroacetic acid as the mobile phase in a shorter run time of 25 min. The flow rate was 1.0 mL/min and the detection wavelength was 245 nm. The drug substance was subjected to stress studies such as hydrolysis, oxidation, photolysis, and thermal degradation, and considerable degradation was observed in acidic hydrolysis, oxidative, thermal, and photolytic stress conditions. The formed degradation products were reported and were well-resolved from the Atorvastatin and its related substances. The stressed samples were quantified against a qualified reference standard and the mass balance was found to be close to 99.5% (w/w) when the response of the degradant was considered to be equal to the analyte (i.e. Atorvastatin), which demonstrates the stability-indicating capability of the method. The method was validated in agreement with ICH requirements. The method developed here was single and shorter (25 min method for the determination of all 12 related impurities of Atorvastatin and its degradation products), with clearly better resolution and higher sensitivity than the European (85 min method for the determination of six impurities) and United States pharmacopeia (115 min and 55 min, two different methods for the determination of six related substances). PMID:23641331

  10. Development of validated stability-indicating chromatographic method for the determination of fexofenadine hydrochloride and its related impurities in pharmaceutical tablets

    PubMed Central

    2011-01-01

    A simple reversed phase high performance liquid chromatographic method with diode array detector (HPLC-DAD) has been developed and subsequently validated for the determination of fexofenadine hydrochloride (FEX) and its related compounds; keto fexofenadine (Impurity A), meta isomer of fexofenadine (Impurity B), methyl ester of fexofenadine (Impurity C) in addition to the methyl ester of ketofexofenadine (Impurity D). The separation was based on the use of a Hypersil BDS C-18 analytical column (250 × 4.6 mm, i.d., 5 ?m). The mobile phase consisted of a mixture of phosphate buffer containing 0.1 gm% of 1-octane sulphonic acid sodium salt monohydrate and 1% (v/v) of triethylamine, pH 2.7 and methanol (60:40, v/v). The separation was carried out at ambient temperature with a flow rate of 1.5 ml/min. Quantitation was achieved with UV detection at 215 nm using lisinopril as internal standard, with linear calibration curves at concentration ranges 0.1-50 ?g/ml for FEX and its related compounds. The optimized conditions were used to develop a stability-indicating HPLC-DAD method for the quantitative determination of FEX and its related compounds in tablet dosage forms. The drugs were subjected to oxidation, hydrolysis, photolysis and heat to apply stress conditions. Complete separation was achieved for the parent compounds and all degradation products. The method was validated according to ICH guidelines in terms of accuracy, precision, robustness, limits of detection and quantitation and other aspects of analytical validation. PMID:22136482

  11. Development and Validation of a Stability-Indicating RP-UPLC Method for Determination of Cloxacillin Sodium in Its Bulk Form and Formulation.

    PubMed

    Patel, Nikita; Contractor, Pooja; Keshrala, Rajesh; Patel, Parag R; Shridhar, Bhimagoni

    2015-07-01

    A simple, linear gradient, rapid, precise and stability-indicating RP-UPLC method was developed for the determination of Cloxacillin Sodium in its bulk form and formulation. Ultra performance liquid chromatography, a most promising advancement in a world of chromatography, reduces analysis time, increases reliability through higher resolution, sensitivity and selectivity as well as used as an economic method due to reducing solvent consumption. A chromatographic separation of a drug as well as its degradants was achieved using Waters acquity BEH, 2.1 × 100 mm, 1.7 ?m C18 column with gradient of mobile phase A: phosphate buffer, pH 6.8 and mobile phase B: methanol:acetonitrile (75:25). The drug and degradants were monitored at a detection wavelength of 225 nm with a flow rate of 0.35 mL/min and an injection volume of 10 µL. The temperature of the column and auto sampler compartments was at 30°C and 25°C ± 1°C, respectively. The retention time of the drug was ?6.9 min. The resolution of the drug and degradant peak was >1.5 in all cases. Force degradation of CLOX SOD was carried under alkaline, acidic, oxidative, thermal, photo degradation conditions and it was analyzed by the proposed method. The drug degrades under alkaline, acidic and oxidative conditions but was stable in temperature and light. A developed method was validated as per ICH guidelines using validation parameters such as precision, linearity and range, limit of quantification, specificity, assay and robustness. PMID:25368408

  12. Rapid Simultaneous Determination of Telmisartan, Amlodipine Besylate and Hydrochlorothiazide in a Combined Poly Pill Dosage Form by Stability-Indicating Ultra Performance Liquid Chromatography

    PubMed Central

    Nalwade, Santaji; Ranga Reddy, Vangala; Durga Rao, Dantu; Koteswara Rao, Inabathina

    2011-01-01

    A simple, precise and rapid stability-indicating ultra-performance liquid chromatography (UPLC) method is developed for the simultaneous quantitative determination of Telmisartan, Amlodipine besylate and Hydrochlorothiazide from their innovative poly pill combination drug product in the presence of degradation products. It involves a 100 mm x 2.1 mm, 1.7 ?m C-18 column. The separation is achieved on a simple gradient method. The mobile phase A contains a mixture of sodium perchlorate buffer pH 3.2 (0.053M): acetonitrile in the ratio 90:10, v/v, and mobile B contains a mixture of sodium perchlorate buffer pH 3.2 (0.053M): acetonitrile in the ratio 20:80, v/v. The flow rate is 0.6 mL min?1 and the column temperature is maintained at 55°C.The gradient program (T/%B) is set as 0/5, 1.2/5, 1.6/40, 4/40, 4.1/5 and 4.5/5. The detector wavelength is 271 nm for Hydrochlorothiazide and Telmisartan and 237 nm for Amlodipine. The retention times of Telmisartan, Amlodipine, and Hydrochlorothiazide are 3.6 minutes, 3.2 minutes and 0.9 minutes; respectively. The total runtime for the separation of the three active compounds and their degradation products is 4.5 minutes. The described method is validated with respect to system suitability, specificity, linearity, precision and accuracy. The precision of the assay method is evaluated by carrying out six independent assays of T, A and H (0.032 mg mL?1 of T, 0.004 mg mL?1 of A, 0.01 mg mL?1 of H). The accuracy of the method is evaluated in triplicate at three concentration levels, i.e. 50%, 100% and 150% of target test concentration (0.64 mg mL?1 of T, 0.08 mg mL?1 of A, 0.2 mg mL?1 of H). The described method is linear over the range, 16 to 48 ?g mL?1 for T, 2 to 6 ?g mL?1A and 5 to 15 ?g mL?1 for H. The method is fast and suitable for high-throughput analysis allowing the analysis of about 250 samples per working day. PMID:21617773

  13. Longitudinal Stability of Social Competence Indicators in a Portuguese Sample: Q-Sort Profiles of Social Competence, Measures of Social Engagement, and Peer Sociometric Acceptance

    ERIC Educational Resources Information Center

    Santos, António J.; Vaughn, Brian E.; Peceguina, Inês; Daniel, João R.

    2014-01-01

    This study examines the temporal stability (over 3 years) of individual differences in 3 domains relevant to preschool children's social competence: social engagement/motivation, profiles of behavior and personality attributes characteristic of socially competent young children, and peer acceptance. Each domain was measured with multiple…

  14. Internet Addiction: Stability and Change

    ERIC Educational Resources Information Center

    Huang, Chiungjung

    2010-01-01

    This longitudinal study examined five indices of stability and change in Internet addiction: structural stability, mean-level stability, differential stability, individual-level stability, and ipsative stability. The study sample was 351 undergraduate students from end of freshman year to end of junior year. Convergent findings revealed stability

  15. Study of forced degradation behavior of eletriptan hydrobromide by LC and LC-MS and development of stability-indicating method.

    PubMed

    Joci?, Biljana; Zecevi?, Mira; Zivanovi?, Ljiljana; Proti?, Ana; Jadranin, Milka; Vajs, Vlatka

    2009-11-01

    The objective of the present study was to report the stability profile of novel antimigrain drug Eletriptan hydrobromide based on the information obtained from forced degradation studies. The drug was subjected to acid (0.1-1 mol L(-1) HCl), neutral and base (0.1-1 mol L(-1) NaOH) hydrolysis and to oxidative decomposition (3-15% (v/v) H(2)O(2)). Photolysis and thermo degradation at 75 degrees C were carried out in methanol solution and in solid state with both Eletriptan hydrobromide bulk drug and the tablet formulation. The products formed under different stress conditions were investigated by LC and LC-MS. The experimental conditions for LC were chosen by employing experimental design and multicriteria decision making methodology. These powerful tools enabled the accomplishment of satisfactory resolution with the shortest possible analysis time. Analytes were separated on a C(18) column (XTerra, 150 mm x 3.9 mm, 5 microm) with the mobile phase composed of methanol-water solution of TEA (pH 6.52, 1%, v/v) (30:70, v/v) pumped at 1 mL min(-1) flow rate. The column temperature was set at 50 degrees C and the detection at 225 nm using DAD detector. The LC method was suitably modified for LC-MS analysis which was further used to characterize the arisen degradation products. The possible degradation pathway was outlined based on the results. The drug appeared to be instable towards every stress condition but oxidation. The stability was not jeopardized even under more exaggerated conditions such as increased temperature of the solutions to 75 degrees C, increased strength of acid/alkali solutions and prolonged testing period. Validation of the LC-DAD method was carried out in accordance with ICH guideline. The method met all required criteria and was applied when testing the commercially available tablets. PMID:19250786

  16. Protein linear indices of the 'macromolecular pseudograph alpha-carbon atom adjacency matrix' in bioinformatics. Part 1: prediction of protein stability effects of a complete set of alanine substitutions in Arc repressor.

    PubMed

    Marrero-Ponce, Yovani; Medina-Marrero, Ricardo; Castillo-Garit, Juan A; Romero-Zaldivar, Vicente; Torrens, Francisco; Castro, Eduardo A

    2005-04-15

    A novel approach to bio-macromolecular design from a linear algebra point of view is introduced. A protein's total (whole protein) and local (one or more amino acid) linear indices are a new set of bio-macromolecular descriptors of relevance to protein QSAR/QSPR studies. These amino-acid level biochemical descriptors are based on the calculation of linear maps on Rn[f k(xmi):Rn-->Rn] in canonical basis. These bio-macromolecular indices are calculated from the kth power of the macromolecular pseudograph alpha-carbon atom adjacency matrix. Total linear indices are linear functional on Rn. That is, the kth total linear indices are linear maps from Rn to the scalar R[f k(xm):Rn-->R]. Thus, the kth total linear indices are calculated by summing the amino-acid linear indices of all amino acids in the protein molecule. A study of the protein stability effects for a complete set of alanine substitutions in the Arc repressor illustrates this approach. A quantitative model that discriminates near wild-type stability alanine mutants from the reduced-stability ones in a training series was obtained. This model permitted the correct classification of 97.56% (40/41) and 91.67% (11/12) of proteins in the training and test set, respectively. It shows a high Matthews correlation coefficient (MCC=0.952) for the training set and an MCC=0.837 for the external prediction set. Additionally, canonical regression analysis corroborated the statistical quality of the classification model (Rcanc=0.824). This analysis was also used to compute biological stability canonical scores for each Arc alanine mutant. On the other hand, the linear piecewise regression model compared favorably with respect to the linear regression one on predicting the melting temperature (tm) of the Arc alanine mutants. The linear model explains almost 81% of the variance of the experimental tm (R=0.90 and s=4.29) and the LOO press statistics evidenced its predictive ability (q2=0.72 and scv=4.79). Moreover, the TOMOCOMD-CAMPS method produced a linear piecewise regression (R=0.97) between protein backbone descriptors and tm values for alanine mutants of the Arc repressor. A break-point value of 51.87 degrees C characterized two mutant clusters and coincided perfectly with the experimental scale. For this reason, we can use the linear discriminant analysis and piecewise models in combination to classify and predict the stability of the mutant Arc homodimers. These models also permitted the interpretation of the driving forces of such folding process, indicating that topologic/topographic protein backbone interactions control the stability profile of wild-type Arc and its alanine mutants. PMID:15781410

  17. Development and validation of a stability-indicating high-performance liquid chromatography method for the simultaneous determination of albuterol, budesonide, and ipratropium bromide in compounded nebulizer solutions.

    PubMed

    Blewett, Anthony J; Varma, Deepti; Gilles, Tiffany; Butcher, Rashidi; Jacob, Jaini; Amazan, Jean; Jansen, Susan A

    2011-01-01

    In recent years, there has been a large increase in the use of pharmaceutical compounding to prepare medications that are not commercially available. The treatment of asthma typically includes the use of albuterol (ALB), ipratropium bromide (IPB), and/or budesonide (BUD) nebulizer solutions. There is currently no commercially available nebulizer solution containing all three of these compounds, and patients must rely on often-unregulated compounding. There is a distinct need for methodologies that can be used to analyze compounded formulations to ensure patient safety. We report an HPLC-UV method to separate and quantitate ALB, IPB, and BUD in nebulizer solutions. The method used a gradient elution to achieve separation via an RP C18 column. The method was validated, showed good selectivity, and was linear over several orders of magnitude. The method was applied to the analysis of nebulizer solutions and determination of their storage stability. Significant ALB-dependent degradation occurred within 5 h in solutions formulated with the free base of ALB, while those containing the sulfate salt of ALB produced no degradation. Alkali solutions can cause base-catalyzed hydrolysis of IPB and degradation of BUD. Compounded formulations containing ALB need to include an acid to control pH and prevent degradation. PMID:21391487

  18. Complexity in Estimation of Esomeprazole and its Related Impurities’ Stability in Various Stress Conditions in Low-Dose Aspirin and Esomeprazole Magnesium Capsules

    PubMed Central

    Reddy, Palavai Sripal; Hotha, Kishore Kumar; Sait, Shakil

    2013-01-01

    A complex, sensitive, and precise high-performance liquid chromatographic method for the profiling of impurities of esomeprazole in low-dose aspirin and esomeprazole capsules has been developed, validated, and used for the determination of impurities in pharmaceutical products. Esomeprazole and its related impurities’ development in the presence of aspirin was traditionally difficult due to aspirin’s sensitivity to basic conditions and esomeprazole’s sensitivity to acidic conditions. When aspirin is under basic, humid, and extreme temperature conditions, it produces salicylic acid and acetic acid moieties. These two byproducts create an acidic environment for the esomeprazole. Due to the volatility and migration phenomenon of the produced acetic acid and salicylic acid from aspirin in the capsule dosage form, esomeprazole’s purity, stability, and quantification are affected. The objective of the present research work was to develop a gradient reversed-phase liquid chromatographic method to separate all the degradation products and process-related impurities from the main peak. The impurities were well-separated on a RP8 column (150 mm × 4.6mm, X-terra, RP8, 3.5?m) by the gradient program using a glycine buffer (0.08 M, pH adjusted to 9.0 with 50% NaOH), acetonitrile, and methanol at a flow rate of 1.0 mL min?1 with detection wavelength at 305 nm and column temperature at 30°C. The developed method was found to be specific, precise, linear, accurate, rugged, and robust. LOQ values for all of the known impurities were below reporting thresholds. The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis, and thermal degradation in the presence of aspirin. The developed RP-HPLC method was validated according to the present ICH guidelines for specificity, linearity, accuracy, precision, limit of detection, limit of quantification, ruggedness, and robustness. PMID:23833714

  19. Evaluation of different preparation methods for a preservative free triamcinolone acetonide preparation for intravitreal administration: a validated stability indicating HPLC-method.

    PubMed

    Korodi, T; Lachmann, B; Kopelent-Frank, H

    2010-12-01

    Intravitreally applied triamcinolone acetonide (TA) is used to treat a variety of macular diseases. Commercially available products of TA are mainly intended for intramuscular application and contain benzyl alcohol (BA) as a bacteriostatic preservative. Since this agent damages ocular tissues, different methods such as filtration techniques and centrifugation are usually used to eliminate BA from commercial products (40 mg/mL TA, 9.9 mg/mL BA). In this study, we evaluated these methods in regard to their ability to eliminate benzyl alcohol and to guarantee standard doses of triamcinolone acetonide. A new formulation without BA (TA 40 mg/mL) was developped according to the following criteria: autoclavability, stability, and suitability for intravitreal use. For QA/QC evaluation a new rapid and simple HPLC procedure (C18 RP column, mobile phase consisting of methanol-water, 48:52, v/v) to quantify the respective compounds was developed and validated according to ICH guidelines. The HPLC method was proven to be selective, linear, precise and accurate. Analysis of preparations based on commercial products undergoing different filtration techniques showed variable results: TA concentrations of 22-80% of the declared amount were found, and BA content was not reduced to safe levels (up to 39% of initial content remained). Centrifugation methods decreased the concentration of the preservative adequately, however agglomerated TA crystals were observed, leading to irreproducible and deviating particle sizes that are potentially harmful with ocular use. The newly developed preservative free formulation (TA 40 mg/mL) delivered uniform doses of TA, revealed no drug loss during forced light exposure and was proven to be stable, sterile and bacterial endotoxin free after autoclaving and after storage for three months,. The new formulation may offer an alternative for the in-house production of intravitreally applicable TA preparations in hospital pharmacies and should enhance medication safety. PMID:21284253

  20. Use of chemical indicators of beer aging for ex-post checking of storage conditions and prediction of the sensory stability of beer.

    PubMed

    Cejka, Pavel; Culík, Ji?í; Horák, Tomáš; Jurková, Marie; Olšovská, Jana

    2013-12-26

    The rate of beer aging is affected by storage conditions including largely time and temperature. Although bottled beer is commonly stored for up to 1 year, sensorial damage of it is quite frequent. Therefore, a method for retrospective determination of temperature of stored beer was developed. The method is based on the determination of selected carbonyl compounds called as "aging indicators", which are formed during beer aging. The aging indicators were determined using GC-MS after precolumn derivatization with O-(2,3,4,5,6-pentaflourobenzyl)hydroxylamine hydrochloride, and their profile was correlated with the development of old flavor evolving under defined conditions (temperature, time) using both a mathematical and statistical apparatus. Three approaches, including calculation from regression graph, multiple linear regression, and neural networks, were employed. The ultimate uncertainty of the method ranged from 3.0 to 11.0 °C depending on the approach used. Furthermore, the assay was extended to include prediction of beer tendency to sensory aging from freshly bottled beer. PMID:24308508

  1. Capability measurement of size-exclusion chromatography with a light-scattering detection method in a stability study of bevacizumab using the process capability indices.

    PubMed

    Oliva, Alexis; Llabrés, Matías; Fariña, José B

    2014-08-01

    In this study, we investigated if the size-exclusion chromatography coupled with light-scattering and refractive index detection (SEC/LS/RI) method is fitted for its intended purpose and checked if the analytical method is able to provide enough conforming results. For this, the process capability indices Cp, Cpk, and Cpm were computed. The traditional X-chart and moving range (MR) chart were used by the same analyst to monitor the equipment in the laboratory over a 1-year period. For this, a bovine serum albumin (BSA) sample (0.3 mg mL(-1)) with a nominal Mw of 66.4 kDa was analyzed each working day. The results confirmed that the analytical method is in-control and stable. To determine whether the given process meets the present capability requirement and runs under the desired quality conditions, the Pearn and Shu (2003) method based on the lower confidence bound C on Cpm was used. The estimator Cpm was 1.81, and the lower confidence bound C was 1.40. We therefore conclude that the true value of the method capability Cpm is no less than 1.40 with a 95% level of confidence. This result indicates that the method is satisfactory and no stringent precision control is required. The usefulness of this method was applied in the characterization of bevacizumab commercial pharmaceutical preparations stored under different conditions that lead to aggregation. In this case, the computed Cpm index was 0.98 (0.70, 1.26), which indicates that the method does not comply with the specification limits and needs to be revised. The quality improvement effort should: (1) reduce the uncertainty in the absolute Mw determination; (2) either move the process mean closer to the target value or reduce the process variation, i.e. improve the method accuracy (?-T) and precision (?(2)). On this point, the Bayesian posterior distribution of the mean and standard deviation pointed out the need to control the precision but specially accuracy in order to reduce the overall uncertainty of analytical method and thus, the method is capable. PMID:24786652

  2. The "Golden Shale": An indicator of coastal stability for Marble Point, McMurdo Sound, over the last four million years

    USGS Publications Warehouse

    Claridge, G.G.C.; Campbell, I.B.

    2007-01-01

    A small sedimentary deposit near Gneiss Point on the western side of McMurdo Sound, previously identified as shale, is described. The deposit is phillipsite, a zeolite that is believed to have formed from the deposition and alteration of volcanic ash in a small ice-marginal saline lake. Other previously recorded occurrences of phillipsite in the dry valleys are believed to be several million years old. A similar age for this deposit is suggested for the Gneiss Point deposit. This is consistent with other weathering and landscape features found in the immediate area, including traces of halloysite in soils. The deposit is very close to sea level but could not have formed if the site had been below sea level, indicating that there has been very little uplift following that which caused the sea to retreat from the Wright Fiord.

  3. Identification and Characterization of an Oxidative Degradation Product of Fexofenadine, Development and Validation of a Stability-Indicating RP-UPLC Method for the Estimation of Process Related Impurities and Degradation Products of Fexofenadine in Pharmaceutical Formulations

    PubMed Central

    Vaghela, Bhupendrasinh; Rao, Surendra Singh; Reddy, Annarapu Malleshwar; Venkatesh, Panuganti; Kumar, Navneet

    2012-01-01

    A novel stability-indicating gradient RP-UPLC method was developed for the quantitative determination of process related impurities and forced degradation products of fexofenadine HCl in pharmaceutical formulations. The method was developed by using Waters Aquity BEH C18 (100 mm x 2.1 mm) 1.7 ?m column with mobile phase containing a gradient mixture of solvent A (0.05% triethyl amine, pH adjusted to 7.0 with ortho-phosphoric acid) and B (10:90 v/v mixture of water and acetonitrile). The flow rate of mobile phase was 0.4 mL/min with column temperature of 30°C and detection wavelength at 220nm. Fexofenadine HCl was subjected to the stress conditions including oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Fexofenadine HCl was found to degrade significantly in oxidative stress conditions, and degradation product was identified and characterized by ESI-MS/MS, 1H and 13C NMR spectroscopic method as the N-oxide 2-[4-(1-hydroxy-4-{4-[hydroxy(diphenyl)methyl]-1-oxido-piperidin-1-yl}butyl)phenyl]-2-methylpropanoic acid. The degradation products were well resolved from fexofenadine and its impurities. The mass balance was found to be satisfactory in all the stress conditions, thus proving the stability-indicating capability 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. PMID:22896817

  4. Environmental Indicators

    NSDL National Science Digital Library

    Environment Canada has developed a set of environmental indicators that are easily measurable and provide useful clues on the state of the environment. This Web site provides a listing of those indicators that Environment Canada monitors. For each indicator, there is a detailed description of the environmental indicator, how it relates to larger environmental problems, and what is being done to reduce the threat. A number of Web links are provided for further information on each indicator.

  5. Bioconversion of rice straw and certain agro-industrial wastes to amendments for organic farming systems: 1. Composting, quality, stability and maturity indices.

    PubMed

    Rashad, Ferial M; Saleh, Walid D; Moselhy, Mohamed A

    2010-08-01

    The microbiological and physicochemical parameters were monitored for 12 weeks during composting of five piles (1.5 x 1.0 x 0.80 m(3)) containing mainly rice straw, soybean residue and enriched with rock phosphate. Two treatments were inoculated with buffalo's manure or composite inoculum, two were supplemented with vinasse and inoculated with either the composite inoculum or with both, the last one was served as a control. Four typical phases of composting were observed during the bioprocess: short initial mesophilic phase followed by, thermophilic, cooling and maturation phases. Physicochemical changes confirmed the succession of microbial populations depending on the temperature of each phase in all treatments. Intense microbial activities led to organic matter mineralization and simultaneously narrow C/N ratios. Inoculation of composting mixtures enhanced the biodegradation of recalcitrant substances. The duration of exposure to a temperature above 55 degrees C for at least 16 consecutive days was quite enough to sanitize the produced composts. After 84 days, all composts reached maturity as indicated by various parameters. PMID:20335032

  6. Antioxidant activities and phenolic composition of extracts from Greek oregano, Greek sage, and summer savory.

    PubMed

    Exarchou, V; Nenadis, N; Tsimidou, M; Gerothanassis, I P; Troganis, A; Boskou, D

    2002-09-11

    Oregano vulgare L. ssp. hirtum (Greek oregano), Salvia fruticosa (Greek sage), and Satureja hortensis (summer savory) were examined as potential sources of phenolic antioxidant compounds. The antioxidant capacities (antiradical activity by DPPH* test, phosphatidylcholine liposome oxidation, Rancimat test) and total phenol content were determined in the ethanol and acetone extracts of the dried material obtained from the botanically characterized plants. The ground material was also tested by the Rancimat test for its effect on the stability of sunflower oil. The data indicated that ground material and both ethanol and acetone extracts had antioxidant activity. Chromatographic (TLC, RP-HPLC) and NMR procedures were employed to cross-validate the presence of antioxidants in ethanol and acetone extracts. The major component of all ethanol extracts was rosmarinic acid as determined by RP-HPLC and NMR. Chromatography indicated the presence of other phenolic antioxidants, mainly found in the acetone extracts. The presence of the flavones luteolin and apigenin and the flavonol quercetin was confirmed in the majority of the extracts by the use of a novel (1)H NMR procedure, which is based on the strongly deshielded OH protons in the region of 12-13 ppm without previous chromatographic separation. This deshielding may be attributed to the strong intramolecular six-membered ring hydrogen bond of the OH(5)...CO(4) moiety. PMID:12207464

  7. ECOLOGICAL INDICATORS

    EPA Science Inventory

    An international symposium on ecological indicators was developed to explore both the potential of ecological indicators and the issues surrounding their development and implementation. his symposium presented state-of-the-science information on the identification, application re...

  8. Identification and quantification of glutathione and phytochelatins from Chlorella vulgaris by RP-HPLC ESI-MS\\/MS and oxygen-free extraction

    Microsoft Academic Search

    Denina B. D. Simmons; Allison R. Hayward; Thomas C. Hutchinson; R. J. Neil Emery

    2009-01-01

    Phytochelatins are short, cysteine-containing, detoxification peptides produced by plants, algae, and fungi in response to\\u000a heavy metal exposure. These peptides auto-oxidize easily. Current extraction protocols do not adequately address losses of\\u000a phytochelatins because of their oxidation and the use of indirect methods for quantification. Method enhancements include\\u000a the use of an argon environment during extraction to reduce auto-oxidation, the use

  9. Analysis of flurbiprofen, ketoprofen and etodolac enantiomers by pre-column derivatization RP-HPLC and application to drug-protein binding in human plasma.

    PubMed

    Jin, Yin-Xiu; Tang, Yi-Hong; Zeng, Su

    2008-04-14

    A stereoselective reversed-phase high-performance liquid chromatography (HPLC) assay to determine the enantiomers of flurbiprofen, ketoprofen and etodolac in human plasma was developed. Chiral drug enantiomers were extracted from human plasma with liquid-liquid extraction. Then flurbiprofen and ketoprofen enantiomers reacted with the acylation reagent thionyl chloride and pre-column chiral derivatization reagent (S)-(-)-alpha-(1-naphthyl)ethylamine (S-NEA), and etodolac enantiomers reacted with S-NEA using 1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide (EDC) and 1-hydroxybenzotriazole (HOBT) as coupling agents. The derivatized products were separated on an Agilent Zorbax C18 (4.6 mm x 250 mm, 5 microm) column with a mixture of acetonitrile-0.01 mol.L(-1) phosphate buffer (pH 4.5) (70:30, v/v) for flurbiprofen enantiomers, acetonitrile-0.01 mol.L(-1) phosphate buffer (pH 4.5) (60:40, v/v) for ketoprofen enantiomers and methonal-0.01 mol.L(-1) potassium dihydrogen phosphate buffer (pH 4.5) (88:12, v/v) for etodolac enantiomers as mobile phase. The flow of mobile phase was set at 0.8 mL.min(-1) and the detection wavelength of UV detector was set at 250 nm for flurbiprofen and ketoprofen enantiomers and 278 nm for etodolac enantiomers. The assay was linear from 0.5 to 50 microg.mL(-1) for each enantiomer. The inter- and intra-day precision (R.S.D.) was less than 10% and the average extraction recovery was more than 87% for each enantiomer. The limit of quantification for the method was 0.5 microg.mL(-1) (R.S.D.<10%, n=5). The method developed was used to study the drug-protein binding of flurbiprofen, ketoprofen and etodolac enantiomers in human plasma. The results showed that the stereoselective binding of etodolac enantiomer was observed and flurbiprofen and ketoprofen enantiomers were not. PMID:18329215

  10. Development and Validation of an RP?HPLC Method for the Determination of Valacyclovir in Tablets and Human Serum and Its Application to Drug Dissolution Studies

    Microsoft Academic Search

    Ayhan Sava?er; Cansel K. Özkan; Yalç?n Özkan; Bengi Uslu; Sibel A. Özkan

    2003-01-01

    A specific, sensitive, simple, and rapid HPLC method has been developed for the determination of valacyclovir (VACL) in raw material, pharmaceutical dosage forms, and human serum, in order to carry out drug dissolution studies from tablets. The chromatographic separation was achieved with acetonitrile:methanol:0.067 M KH2PO4 (27:20:53, v\\/v\\/v) adjusted to pH 6.5 with 3 M NaOH as mobile phase, a Waters Spherisorb C18

  11. Analysis of flurbiprofen, ketoprofen and etodolac enantiomers by pre-column derivatization RP-HPLC and application to drug–protein binding in human plasma

    Microsoft Academic Search

    Yin-Xiu Jin; Yi-Hong Tang; Su Zeng

    2008-01-01

    A stereoselective reversed-phase high-performance liquid chromatography (HPLC) assay to determine the enantiomers of flurbiprofen, ketoprofen and etodolac in human plasma was developed. Chiral drug enantiomers were extracted from human plasma with liquid–liquid extraction. Then flurbiprofen and ketoprofen enantiomers reacted with the acylation reagent thionyl chloride and pre-column chiral derivatization reagent (S)-(?)-?-(1-naphthyl)ethylamine (S-NEA), and etodolac enantiomers reacted with S-NEA using 1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide

  12. Separation and determination of trace amounts of beryllium(II), aluminium(III) and chromium(III) with chromotrope 2C chelates by RP-HPLC.

    PubMed

    Shoupu, L; Mingqiao, Z; Chuanyue, D

    1994-02-01

    A reversed-phase high-performance liquid chromatographic separation and determination of beryllium(II), aluminium(III) and chromium(III) with chromotrope 2C chelates on a C18-bonded stationary phase is reported. Methanol-water (45:55 v/v) containing 6 x 10(-3)M tetra-n-butylammonium bromide (TBAB) and 2 x 10(-2)M acetate buffer solution (pH 6.0) as mobile phase and with spectrophotometric detection at 530 nm was applied. The method has high sensitivity, the detection limits being 0.2 ppb for beryllium(I), 1 ppb for aluminium(III) and 2 ppb for chromium(III). Under the optimum conditions, most other metal ions did not interfere, e.g. up to 2 mg of Hg(II), Sn(II, IV), Pb(II), Bi(III), Ag(I), Zn(II), Cd(II), Cu(II), 1.5 mg of Fe(II), Co(II), Ni(II), 1.2 mg of Ca(II), Mg(II), Sr(II), Ba(II), 1 mg of Ga(III), In(III), 0.5 mg of Fe(III), 1 mg of Ga(III), In(III), 0.5 mg of Fe(III), 0.4 mg of Th(IV), Zr(IV). The method can be applied to the simultaneous determination of trace amounts of beryllium(II), aluminium(III) and chromium(III), in water, rice, flour and human hair samples. PMID:18965921

  13. Identification of lipopeptide isoforms by MALDI-TOF-MS/MS based on the simultaneous purification of iturin, fengycin, and surfactin by RP-HPLC.

    PubMed

    Yang, Huan; Li, Xu; Li, Xue; Yu, Huimin; Shen, Zhongyao

    2015-03-01

    A three-stage linear gradient strategy using reverse-phase high-performance liquid chromatography (HPLC) was optimized for rapid, high-quality, and simultaneous purification of the lipopeptide isoforms of iturin, fengycin, and surfactin, which may differ in composition by only a single amino acid and/or the fatty acid residue. Matrix-assisted laser desorption ionization time-of-flight tandem mass spectrometry (MALDI-TOF-MS/MS) was applied to detect the lipopeptides harvested from each reversed-phase HPLC peak. Amino acid analysis based on phenyl isothiocyanate derivatization was further used for confirmation of the amino acid species and molar ratio in a certain HPLC fraction. By this MALDI-TOF-MS/MS coupled with amino acid analysis, it was revealed that iturin at m/z 1,043 consists of a circular Asn-Tyr-Asn-Gln-Pro-Asn-Ser peptide and C14 ?-OH fatty acid. Surfactin homologs from Bacillus subtilis THY-7 at m/z 1,030, 1,044, 1,058, and 1,072 possess a circular Glu-Leu-Leu-Val-Asp-Leu-Leu peptide and the ?-OH fatty acid with a different length (C13-C16). Fengycin species at m/z 1,463 and 1,477 are homologs possessing the circular peptide Glu-Orn-Tyr-Thr-Glu-Ala-Pro-Gln-Tyr-Ile linked to a C16 or C17 ?-OH fatty acid, whereas fengycin at m/z 1,505 contains a Glu-Orn-Tyr-Thr-Glu-Val-Pro-Gln-Tyr-Ile sequence with a Val instead of Ala at position 6. The method developed in this work provided an efficient approach for characterization of diverse lipopeptide isoforms from the iturin, fengycin, and surfactin families. PMID:25662934

  14. Development and Validation of RP-HPLC Method for Simultaneous Estimation of Picroside I, Plumbagin, and Z-guggulsterone in Tablet Formulation

    PubMed Central

    Akhade, Meenakshi S.; Agrawal, Poonam A.; Laddha, K. S.

    2013-01-01

    The aim of the present work was to develop and validate a reversed-phase high-performance liquid chromatography method for the simultaneous estimation of picroside I, plumbagin, and Z-guggulsterone in a polyherbal formulation containing Picrorhiza kurroa, Plumbago zeylanica, and Commiphora wightii extracts. The analysis was performed on a C18 column using the mobile phase consisting of solvent A (acetonitrile) and solvent B (0.1% orthophosphoric acid in water) with the following gradient: 0-12 min, 25% A; 12-17 min, 25-80% A; 17-32 min, 80% A; and 32-37 min, 80-25% A at a flow rate of 1 ml/min. Ultraviolet detection was at 255 nm. The method was validated for accuracy, precision, linearity, specificity, and sensitivity as per the norms of the International Conference on Harmonization. From the validation study, it was found that the method is specific, accurate, precise, reliable, and reproducible. Good linear correlation coefficients (r2>0.900) were obtained for calibration plots in the ranges tested. Limits of detection were 2.700, 0.090 and 0.099 ?g/ml and limits of quantification were 9.003, 0.310, and 0.330 ?g/ml for picroside I, plumbagin, and Z-guggulsterone, respectively. Intra and interday relative standard deviation (RSD) of retention times and peak areas was less than 3.0%. Recovery was found to be 100.21% for picroside I, 102.5% for plumbagin, and 103.84% for Z-guggulsterone. The established method was appropriate and the three markers were well resolved, enabling efficient quantitative analysis of picroside I, plumbagin and Z-guggulsterone. The method is a rapid and cost-effective quality control tool for routine quantitative analysis of picroside I, plumbagin, and Z-guggulsterone in tablet dosage form. PMID:24302803

  15. DEVELOPMENT AND VALIDATION OF RP-HPLC AND ULTRAVIOLET SPECTROPHOTOMETRIC METHODS OF ANALYSIS FOR SIMULTANEOUS DETERMINATION OF PARACETAMOL AND LORNOXICAM IN PHARMACEUTICAL DOSAGE FORMS

    Microsoft Academic Search

    M. V. N. Kumar Talluri; Mukesh K. Bairwa; H. H. Theja Dugga; R. Srinivas

    2012-01-01

    A high performance liquid chromatographic and an UV spectrophotometric method were developed and validated for the simultaneous determination of paracetamol and lornoxicam in pharmaceutical formulations. The different analytical performance parameters such as linearity, precision, accuracy, specificity, limit of detection (LOD), and limit of quantification (LOQ) were determined according to International Conference on Harmonization (ICH) guidelines. HPLC was carried out by

  16. Simultaneous Estimation of Amlodipine Besylate and Indapamide in a Pharmaceutical Formulation by a High Performance Liquid Chromatographic (RP-HPLC) Method

    PubMed Central

    Patel, Deval B.; Mehta, Falgun A.; Bhatt, Kashyap K.

    2012-01-01

    An isocratic reversed-phase liquid chromatograpic assay method was developed for the quantitative determination of amlodipine besylate (AML) and indapamide (IND) in combined dosage form. A Brownlee C-18, 5 ?m column with a mobile phase containing 0.02 M potassium dihydrogen phosphate–methanol (30+70, v/v) total pH-adjusted to 3 using o-phosphoric acid was used. The flow rate was 1.0 mL min?1 and effluents were monitored at 242 nm. The retention times of amlodipine besylate and indapamide were 5.9 min and 3.6 min, respectively. The proposed method was validated with respect to linearity, accuracy, precision, and robustness. The method was successfully applied to the estimation of amlodipine besylate and indapamide in combined tablet dosage forms. PMID:23008807

  17. Simultaneous determination of cefdinir and cefixime in human plasma by RP-HPLC\\/UV detection method: Method development, optimization, validation, and its application to a pharmacokinetic study

    Microsoft Academic Search

    Abbas Khan; Zafar Iqbal; Muhammad Imran Khan; Khalid Javed; Abad Khan; Lateef Ahmad; Yasar Shah; Fazli Nasir

    2011-01-01

    A novel isocratic reversed-phase high performance liquid-chromatography\\/ultraviolet detection method for simultaneous determination of cefdinir and cefixime in human plasma was developed and validated after optimization of various chromatographic conditions and other experimental parameters. Sample preparation based on a simple extraction procedure consisting of deproteination and extraction with 3 parts of 6% trichloroacetic acid aqueous solution followed by volume make up

  18. RP-HPLC-DAD method for the identification of two potential antioxidant agents namely verminoside and 1-O-(E)-caffeoyl-?-gentiobiose from Spathodea campanulata leaves.

    PubMed

    Boniface, Pone Kamdem; Singh, Manju; Verma, Surjeet; Shukla, Aparna; Khan, Feroz; Srivastava, Santosh Kumar; Pal, Anirban

    2015-01-01

    A simple and reliable high-performance liquid chromatographic method was successfully developed for the study of fingerprint chromatograms of extract and fractions from the leaves of Spathodea campanulata (SC) using verminoside (1) and 1-O-(E)-caffeoyl-?-gentiobiose (2) as marker compounds. Antioxidant activity of SC was determined by using free radical of 2,2-diphenyl-1-picryl-hydrazyl-hydrate as an experimental model. The docking study of selected target, tyrosinase and ligands (ascorbic acid, compounds 1 and 2) was performed through Autodock Vina v0.8. Fingerprints of methanol, chloroform, ethylacetate, n-butanol and water extracts could resolve 13, 11, 22, 16 and 5 peaks, respectively. Extract, fractions and compounds 1 and 2 previously isolated from SC displayed remarkable antioxidant activity with radical-scavenging activity ranging from 2.5 to 6.7 ?g/mL. In silico study identified compounds 1 and 2 as potential inhibitors of tyrosinase correlating with the observed antioxidant activity in vitro. PMID:25429989

  19. Development and validation of an RP-HPLC method to quantitate acyclovir in cross-linked chitosan microspheres produced by spray drying.

    PubMed

    Stulzer, Hellen K; Tagliari, Monika Piazzon; Murakami, Fábio S; Silva, Marcos A S; Laranjeira, Mauro C M

    2008-07-01

    An accurate, simple, reproducible, and sensitive liquid chromatographic method is developed and validated to quantitate acyclovir (ACV) in cross-linked chitosan microspheres produced by spray drying. The analysis is carried out using a reversed-phase C18 column with UV-vis detection at 254 nm. The mobile phase is diluted with pure water and acetonitrile (95:5 v/v) at a flow-rate of 0.8 mL/min. The parameters used in the validation process are: linearity, range, quantitation limit, detection limit, accuracy, specificity precision, and ruggedness. The retention time of acyclovir is approximately 3.5 min with symmetrical peaks. The linearity in the range of 1-10 microg/mL presents a correlation coefficient of 0.9999. The chitosan and the tripolyphosphate in the formulation do not interfere with the analysis, and the recovery is quantitative. Results are satisfactory, and the method proves to be suitable to quantitate ACV in cross-linked chitosan microspheres. PMID:18647469

  20. Simultaneous determination of the endogenous free ?-lipoic acid and dihydrolipoic acid in human plasma and erythrocytes by RP-HPLC coupled with electrochemical detector.

    PubMed

    Khan, Muhammad Imran; Iqbal, Zafar; Khan, Abad

    2015-01-01

    A highly sensitive, precise, and accurate reversed-phase high performance liquid-chromatography/electrochemical detection method for simultaneous determination of the endogenous free ?-lipoic acid and dihydrolipoic acid in biological matrices is presented. The two analytes are extracted from samples with acetonitrile-10% m-phosphoric acid solution(aqueous) (50:50 v/v). To determine the total lipoic acid, samples are treated with tris(2-carboxyethyl)phosphine solution in phosphate buffer: pH 2.5 with 85% o-phosphoric acid prior to deproteination. The two analytes are separated on a C18 (150?×?4.6 mm, 5 ?m) analytical column using acetonitrile-50 mM phosphate buffer: pH 2.5 with 85% o-phosphoric acid (35:65 v/v) as the isocratic mobile phase pumped at a flow rate of 2.0 ml/min at the column oven temperature of 35 °C. The column eluents are monitored at a potential of 0.9 V. These analytes are efficiently resolved in <7 min. PMID:25323519

  1. Simultaneous determination of ascorbic acid, aminothiols, and methionine in biological matrices using ion-pairing RP-HPLC coupled with electrochemical detector.

    PubMed

    Khan, Muhammad Imran; Iqbal, Zafar; Khan, Abad

    2015-01-01

    A novel highly sensitive ion-pairing reversed-phase high performance liquid-chromatography/electrochemical detection method for simultaneous determination of L -ascorbic acid, aminothiols, and methionine in biological matrices is presented. Reduced forms of the analytes are extracted from sample matrices with 10% m-phosphoric acid solution(aqueous). To determine the total vitamin C, the total aminothiols, and the total methionine, samples are treated with tris(2-carboxyethyl)phosphine solution in 0.05% trifluoroacetic acid solution(aqueous) subsequent to deproteination to reduce the oxidized forms of these compounds. Various analytes are separated on a C18 (250?×?4.6 mm, 5 ?m) analytical column using methanol-0.05% trifluoroacetic acid solution(aqueous) (05:95 v/v, containing 0.1 mM 1-octane sulfonic acid as the ion-pairing agent) as the isocratic mobile phase that is pumped at a flow rate of 1.5 ml/min at room temperature. The column eluents are monitored at a voltage of 0.85 V. These analytes are efficiently resolved in less than 20 min using n-acetyl cysteine as the internal standard. PMID:25323509

  2. RP-HPLC method using 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate incorporated with normalization technique in principal component analysis to differentiate the bovine, porcine and fish gelatins.

    PubMed

    Azilawati, M I; Hashim, D M; Jamilah, B; Amin, I

    2015-04-01

    The amino acid compositions of bovine, porcine and fish gelatin were determined by amino acid analysis using 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate as derivatization reagent. Sixteen amino acids were identified with similar spectral chromatograms. Data pre-treatment via centering and transformation of data by normalization were performed to provide data that are more suitable for analysis and easier to be interpreted. Principal component analysis (PCA) transformed the original data matrix into a number of principal components (PCs). Three principal components (PCs) described 96.5% of the total variance, and 2 PCs (91%) explained the highest variances. The PCA model demonstrated the relationships among amino acids in the correlation loadings plot to the group of gelatins in the scores plot. Fish gelatin was correlated to threonine, serine and methionine on the positive side of PC1; bovine gelatin was correlated to the non-polar side chains amino acids that were proline, hydroxyproline, leucine, isoleucine and valine on the negative side of PC1 and porcine gelatin was correlated to the polar side chains amino acids that were aspartate, glutamic acid, lysine and tyrosine on the negative side of PC2. Verification on the database using 12 samples from commercial products gelatin-based had confirmed the grouping patterns and the variables correlations. Therefore, this quantitative method is very useful as a screening method to determine gelatin from various sources. PMID:25442566

  3. RP-HPLC method for the simultaneous quantitation of boeravinone E and boeravinone B in Boerhaavia diffusa extract and its formulation.

    PubMed

    Bhope, S G; Gaikwad, P S; Kuber, V V; Patil, M J

    2013-01-01

    A high-performance liquid chromatography method was developed and validated for the simultaneous quantitation of two major rotenoids, boeravinone E and boeravinone B, in Boerhaavia diffusa extract and its formulation. Chromatographic separation was carried out on an Inertsil ODS-3 column by using gradient mobile phase containing 0.1% v/v orthophosphoric acid in water and acetonitrile. The detection was carried out at 276 nm. The method was validated for specificity, precision, accuracy and robustness. The linearity (r(2) = 0.9989 and 0.9991) was found to be in the range of 7.26-35.75 µg mL(-1) and 2.20-11.00 µg mL(-1) for boeravinone E and B, respectively. The percent recovery observed from the extract sample was 95.22-95.83. PMID:22480291

  4. RBC indices

    MedlinePLUS

    ... corpuscular hemoglobin concentration (MCHC); Mean corpuscular volume (MCV); Red blood cell indices ... and hemoglobin. The MCV reflects the size of red blood cells. The MCH and MCHC reflect the ...

  5. ROLE OF A NOVEL EXCIPIENT POLY(ETHYLENE GLYCOL)-b-POLY (l-HISTIDINE) IN RETENTION OF PHYSICAL STABILITY OF INSULIN AT AQUEOUS/ORGANIC INTERFACE

    PubMed Central

    Taluja, Ajay; Han Bae, You

    2008-01-01

    The aim of this study was to investigate whether a cationic polyelectrolyte; poly(ethylene glycol) PEG-b-poly(l-histidine) diblock copolymer [PEG-polyHis] can stabilize insulin, at the aqueous/methylene chloride interface formed during the microencapsulation process. Insulin aggregation at this interface was monitored spectrophotometrically at 276 nm. The effects of protein concentration, pH of the aqueous medium, and the presence of poly(lactic-co-glycolic acid) [PLGA] in methylene chloride (MC) on insulin aggregation were observed. For the 2.0 mg/ml insulin solutions in phosphate buffer (PB), the effect of addition of Pluronic F-127 as a positive control and addition of PEG-polyHis as a novel excipient in PB was also evaluated at various insulin/polymeric excipient weight ratios. The conformation of insulin protected by PEG-polyHis and recovered after interfacial exposure was evaluated via circular dichroism (CD) spectroscopy. Greater loss in soluble insulin was observed with increasing insulin concentrations. pH 6.0 was selected for optimal ionic interactions between insulin and PEG-polyHis based on zeta potential and particle size studies. pH 4.5 and 7.4 (no ionic complexation between insulin and PEG-polyHis) were selected as controls to compare the stabilization effect of PEG-polyHis with that at pH 6.0. Incubation of PEG-polyHis with insulin at pH 6.0 drastically reduced protein aggregation, even in the presence of PLGA. PEG-polyHis and F-127 reduced insulin aggregation in non-complexing pH conditions pointing to the role played by PEG in modulation of insulin adsorption at the interface. Far-UV (205-250 nm) circular dichroism (CD) study revealed negligible qualitative effects on soluble insulin’s secondary structure after interfacial exposure. RP-HPLC and size-exclusion HPLC showed no deamidation of insulin or formation of soluble high molecular weight transformation products respectively. MALDI-TOF mass spectrometry confirmed the results from chromatographic procedures. Radioimmunoassay carried out on select samples showed that recovered soluble insulin had retained its immunoreactivity. An experimental method to simulate interfacial denaturation of proteins was designed for assessment of protein stability at the interface and screening for novel protein stabilizers. Understanding and manipulation of such polyelectrolyte-insulin complexation will likely play a role in insulin controlled delivery via microspheres formulation(s). PMID:17439239

  6. Position indicator

    DOEpatents

    Tanner, David E. (Poway, CA)

    1981-01-01

    A nuclear reactor system is described in which a position indicator is provided for detecting and indicating the position of a movable element inside a pressure vessel. The movable element may be a valve element or similar device which moves about an axis. Light from a light source is transmitted from a source outside the pressure vessel to a first region inside the pressure vessel in alignment with the axis of the movable element. The light is redirected by a reflector prism to a second region displaced radially from the first region. The reflector prism moves in response to movement of the movable element about its axis such that the second region moves arcuately with respect to the first region. Sensors are arrayed in an arc corresponding to the arc of movement of the second region and signals are transmitted from the sensors to the exterior of the reactor vessel to provide indication of the position of the movable element.

  7. Chemical Indicators.

    ERIC Educational Resources Information Center

    Prombain, Dorothy R.; And Others

    This science sourcebook was written for intermediate grade teachers to provide guidance in teaching a specially developed unit on chemical indicators. Directions and suggestions for guiding student science activities are given. Some of the activities concern soil testing, crystals, and household powders such as sugar and salt. A list of necessary…

  8. Validated stability-indicating high-performance thin-layer chromatographic method for estimation of cefpodoxime proxetil in bulk and in pharmaceutical formulation according to International conference on harmonization guidelines

    PubMed Central

    Jain, Pritam; Chaudhari, Amar; Bang, Anup; Surana, Sanjay

    2012-01-01

    Aim: A simple, selective, precise, and stability-indicating high-performance thin-layer chromatographic (HPTLC) method for analysis of cefpodoxime proxetil both in bulk and in pharmaceutical formulation has been developed and validated. Materials and Methods: The method employed HPTLC aluminum plates precoated with silica gel 60 RP-18 F254 as the stationary phase. The solvent system consisted of toluene:methanol:chloroform (4:2:4 v/v). The system was found to give compact spot for cefpodoxime proxetil (Rf value of 0.55 ± 0.02). Densitometric analysis of cefpodoxime proxetil was carried out in the absorbance mode at 289 nm. Results: The linear regression analysis data for the calibration plots showed good linear relationship, with r2 = 0.998 ± 0.0015 with respect to peak area in the concentration range of 100–600 ng per spot. The mean value±SD of slope and intercept were 3.38 ± 1.47 and 986.9 ± 108.78 with respect to peak area. The method was validated for precision, recovery, and robustness. The limits of detection and quantification were 3.99 and 12.39 ng per spot, respectively. Cefpodoxime proxetil was subjected to acid and alkali hydrolysis, oxidation, and thermal degradation. The drug undergoes degradation under acidic and basic conditions, indicating that the drug is susceptible to both acid and base. The degraded product was well resolved from the pure drug, with significantly different Rf value. Statistical analysis proves that the method is repeatable, selective, and accurate for the estimation of the investigated drug. Conclusion: The proposed HPTLC method can be applied for identification and quantitative determination of cefpodoxime proxetil in both bulk drug and pharmaceutical formulation. PMID:22557919

  9. Social Indicators

    NSDL National Science Digital Library

    Bolton, Paul.

    The House of Commons Library Research Papers are published for the benefit of Parliament members, but this one should be of interest to both researchers and general readers wanting to learn more about contemporary British social issues. Social Indicators is the first paper in a new series that will be published three times a year. The 71-page paper includes a wide range of topic pages that present social statistics on a variety of issues, from the prison population to defense expenses to agricultural outputs. Each Social Indicator paper will also offer feature articles that give a closer look at specific subjects (in this instance,, election turnout and adult literacy) and an article on statistical sources for a particular issue (in this paper, social security statistics). The last few pages are devoted to a list of important, recent governmental statistical publications.

  10. Optimizing Protein Stability In Vivo

    PubMed Central

    Foit, Linda; Morgan, Gareth J.; Kern, Maximilian J.; Steimer, Lenz R.; von Hacht, Annekathrin A.; Titchmarsh, James; Warriner, Stuart L.; Radford, Sheena E.; Bardwell, James C.A.

    2010-01-01

    SUMMARY Identifying mutations that stabilize proteins is challenging because most substitutions are destabilizing. In addition to being of immense practical utility, the ability to evolve protein stability in vivo may indicate how evolution has formed today's protein sequences. Here we describe a genetic selection that directly links the in vivo stability of proteins to antibiotic resistance. It allows the identification of stabilizing mutations within proteins. The large majority of mutants selected for improved antibiotic resistance are stabilized both thermodynamically and kinetically, indicating that similar principles govern stability in vivo and in vitro. The approach requires no prior structural or functional knowledge and allows selection for stability without a need to maintain function. Mutations that enhance thermodynamic stability of the protein Im7 map overwhelmingly to surface residues involved in binding to colicin E7, implying that evolutionary pressures that drive Im7-E7 complex formation may have compromised the stability of the isolated Im7 protein. PMID:20005848

  11. Synthesis of [Ru(phen)2dppz]2+ -Tethered Oligo-DNA and Studies on

    E-print Network

    Pradeepkumar, P. I.

    -ends of oligodeoxyribonucleotide (ODN). The middle [Ru(phen)2dppz]2+-ODN tethered was resolved and isolated as four pure diastereomers, while the 3- or 5-[Ru(phen)2dppz]2+-ODNs were inseparable on RP-HPLC. Thermal stability of the (Ru2+-ODN), DNA duplexes is found to increase considerably (Tm ) 12.8-23.4 °C

  12. Development and Validation of a Simultaneous HPLC Method for Estimation of Bisoprolol Fumarate and Amlodipine Besylate from Tablets

    PubMed Central

    Vora, D. N.; Kadav, A. A.

    2008-01-01

    A fast, robust and stability indicating RP-HPLC method was developed for simultaneous determination of bisoprolol fumarate and amlodipine besylate in tablets. The mobile phase was mixture of 25 mM ammonium acetate adjusted to pH 5.0 and methanol (65: 35) at 0.8 ml/min. The stationary phase was Luna C18-2 column (3 ?, 50×4.6 mm ID). UV detection was performed at 230 nm. Retention time was 1.45 min and 3.91 min for bisoprolol and amlodipine, respectively. Linearity was established in the range of 8–33 ?g/ml. Mean recovery was 99.1% and 98.6% for bisoprolol fumarate and amlodipine besylate, respectively. PMID:20046793

  13. Stability and Feedback Stabilization 1639 Stability and Feedback Stabilization

    E-print Network

    Sontag, Eduardo

    Stability and Feedback Stabilization 1639 Stability and Feedback Stabilization EDUARDO D. SONTAG of the Subject Introduction Linear Systems Nonlinear Systems: Continuous Feedback Discontinuous Feedback) if it is possible to find a feedback law that renders that state a globally asymptotically stable equi- librium

  14. [Stabilizers of horseradish peroxidase].

    PubMed

    Mao, Xinhuan; Li, Xiang; Wang, Shanshan; Zhang, Wenjing; Zeng, Chengming

    2009-03-01

    Keeping an enzyme in its native form with high catalytic activity is of great significance. In the present study, thermal stabilizers of horseradish peroxidase (HRP) were screened. The results indicated that thermal stability of HRP was enhanced by magnesium sulphate and gelatin. A synergic effect of magnesium sulphate and gelatin was observed. In the presence of the stabilizer, the enzymatic activity of HRP remained 89% after kept for 80 h at 50 degrees C and 57% for 90 days at room temperature. Thermal alterations of HRP structure in the absence and presence of the stabilizers were explored by using UV absorption spectra at 402 nm (Soret band), intrinsic fluorescence and 8-anilinonaphthalene-1-sulfonic acid (ANS) fluorescence. The results suggested that magnesium sulphate and gelatin attenuated the extent of unfolding of HRP and therefore the native enzyme structure was stabilized. PMID:19621579

  15. Mass Spectrometric Identification of the Arginine and Lysine deficient Proline Rich Glutamine Rich Wheat Storage Proteins

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Tandem mass spectrometry (MS/MS) of enzymatic digest has made possible identification of a wide variety of proteins and complex samples prepared by such techniques as RP-HPLC or 2-D gel electrophoresis. Success requires peptide fragmentation to be indicative of the peptide amino acid sequence. The f...

  16. Stability Functions

    E-print Network

    Burns, Daniel

    In this article we discuss the role of stability functions in geometric invariant theory and apply stability function techniques to various types of asymptotic problems in the Kahler geometry of GIT quotients. We discuss ...

  17. Stabilized Vegas

    Microsoft Academic Search

    Hyojeong Choe; Steven H. Low

    2003-01-01

    We show that the current TCP Vegas algorithm can become unstable in the presence of network delay and propose a modification that stabilizes it. The stabilized Vegas remains completely source-based and can be implemented without any network support. We suggest an incremental deployment strategy for stabilized Vegas when the network contains a mix of links, some with active queue management

  18. Dynamic Process Capability Indices

    Microsoft Academic Search

    Jing Sun

    2002-01-01

    Process capability indices as an important kind of indices are intended to provide single-number assessments of the inherent process capability to meet specification limits on quality characteristic(s) of interest. In this paper the condition for the application of process capability indices is analyzed. On the basis of process capability indices, dynamic process capability indices as a new kind of indices

  19. The stochastic control of process capability indices

    Microsoft Academic Search

    Nozer D. Singpurwalla; G. Box; D. R. Cox; D. K. Dey; A. Fries; J. K. Ghosh; M. A. Gómez-Villegas; T. Z. Irony; W. Kliemann; S. Kotz; D. V. Lindley; M. F. McGrath; D. Peña

    1998-01-01

    In manufacturing science, process capability indices play a role analogous to economic indices in government statistics. The\\u000a existing capability indices are passive devices whose main role is to retroactively monitor process capability. The have been\\u000a developed under the restrictive assumption of process stability, and the procedures for using them are based on ad hoc rules.\\u000a Using the normative point of

  20. Membrane stabilizer

    DOEpatents

    Mingenbach, William A. (P.O. Box 49, Taos, NM 87571)

    1988-01-01

    A device is provided for stabilizing a flexible membrane secured within a frame, wherein a plurality of elongated arms are disposed radially from a central hub which penetrates the membrane, said arms imposing alternately against opposite sides of the membrane, thus warping and tensioning the membrane into a condition of improved stability. The membrane may be an opaque or translucent sheet or other material.

  1. Arthroscopic lateral ankle stabilization.

    PubMed

    Kashuk, K B; Landsman, A S; Werd, M B; Hanft, J R; Roberts, M

    1994-07-01

    The indications for arthroscopic stabilization include those patients with isolated ruptures or strains of the ATF. The procedure is particularly convenient for patients with ankle joint pathology that is already most commonly treated arthroscopically, such as chronic instability, in which inflamed synovium or meniscoid bodies are to be excised. Although significant stability can be gained with this technique, injuries that result in damage to the calcaneofibular ligament may require additional open surgery, since this ligament cannot be visualized arthroscopically. However, the anchoring techniques described in this article can still be used when performing open surgery. PMID:7954209

  2. Automatic stabilization

    NASA Technical Reports Server (NTRS)

    Haus, FR

    1936-01-01

    This report concerns the study of automatic stabilizers and extends it to include the control of the three-control system of the airplane instead of just altitude control. Some of the topics discussed include lateral disturbed motion, static stability, the mathematical theory of lateral motion, and large angles of incidence. Various mechanisms and stabilizers are also discussed. The feeding of Diesel engines by injection pumps actuated by engine compression, achieves the required high speeds of injection readily and permits rigorous control of the combustible charge introduced into each cylinder and of the peak pressure in the resultant cycle.

  3. Terrestrial Indicators and Measurements

    E-print Network

    jurisdictions. General Approach. Indicators were selected through a five-step participatory process involving in at least one national monitoring program, was used for the core indicators. Core Indicators and/or vegetation trend monitoring: (1)

  4. ECOLOGICAL PERFORMANCE INDICATORS

    EPA Science Inventory

    EMAP has traditionally relied on indicators of ecological condition to report on the extent to which coastal waters are impaired. Correlations between biological indicators and physical or chemical indicators may generate hypotheses about potential causes of impairment but are n...

  5. Stabilization of compactible waste

    SciTech Connect

    Franz, E.M.; Heiser, J.H. III; Colombo, P.

    1990-09-01

    This report summarizes the results of series of experiments performed to determine the feasibility of stabilizing compacted or compactible waste with polymers. The need for this work arose from problems encountered at disposal sites attributed to the instability of this waste in disposal. These studies are part of an experimental program conducted at Brookhaven National Laboratory (BNL) investigating methods for the improved solidification/stabilization of DOE low-level wastes. The approach taken in this study was to perform a series of survey type experiments using various polymerization systems to find the most economical and practical method for further in-depth studies. Compactible dry bulk waste was stabilized with two different monomer systems: styrene-trimethylolpropane trimethacrylate (TMPTMA) and polyester-styrene, in laboratory-scale experiments. Stabilization was accomplished by wetting or soaking compactible waste (before or after compaction) with monomers, which were subsequently polymerized. Three stabilization methods are described. One involves the in-situ treatment of compacted waste with monomers in which a vacuum technique is used to introduce the binder into the waste. The second method involves the alternate placement and compaction of waste and binder into a disposal container. In the third method, the waste is treated before compaction by wetting the waste with the binder using a spraying technique. A series of samples stabilized at various binder-to-waste ratios were evaluated through water immersion and compression testing. Full-scale studies were conducted by stabilizing two 55-gallon drums of real compacted waste. The results of this preliminary study indicate that the integrity of compacted waste forms can be readily improved to ensure their long-term durability in disposal environments. 9 refs., 10 figs., 2 tabs.

  6. [Performance indicators: INCA (cardiovascular indicators) project].

    PubMed

    Gillespie, F; Orsi, G B; Caracci, G; Scanzano, P; Casertano, L; Duranti, G; Cardo, S; Barone, A P; Tozzi, Q; Ammirati, F

    2007-01-01

    The objective of INCA project was the development and implementation of Acute Myocardial Infarction (AMI type ST elevation) process and outcome indicators for the regional cardiology units, testing the possibility of using regional healthcare information data to evaluate the quality of provided healthcare within the regional healthcare accreditation process. The project is introduced by an overview of major concepts of evaluating and managing quality of healthcare. We performed a literature review of structure, process and outcome indicators in cardiology and of accreditation standards for cardiology at national and international level. Through consensus procedures and according to international evidence based literature a set of 18 process and outcome indicators for AMI was defined. A specific procedure for data collection has been developed. Education and training of participants on procedures, quality and accreditation was achieved. Expected verifiable end-points have been achieved over a three months period of data collecting throughout 21 cardiology units, differentiated for level of complexity and location, for a total of 409 clinical observed cases of AMI. Analysis of data was followed by the diffusion of results. Successful data collection of clinical performance indicators on a regional basis was achieved. Participants have been trained to quality sciences. Results will be useful to evaluate and design implementation strategies of regional accreditation of health care services within a shared framework. Benchmarking within Regional hospital cardiology care services will be developed following self evaluation and continuous quality improvement cycle activities. PMID:17405513

  7. Laser Stabilization

    SciTech Connect

    Hall, John L.; Taubman, Matthew S.; Ye, Jun

    2010-01-01

    This book chapter covers the basics of the field of stabilizing lasers to optical frequency references such as optical cavities and molecular transitions via the application of servo control systems. These discussions are given with reference to the real-life frequency metrology experienced in Hall-Labs (now Ye-Labs), JILA, University of Colorado. The subjects covered include: the basics of control system stability, a discussion of both the theoretical and experimental limitations, an outline of optical cavity susceptibility to environmental noise, and a brief introduction to the use and limitations of molecular transitions as frequency references.

  8. A Validated Stability Indicating RPLC Method for Tazarotene

    Microsoft Academic Search

    D. B. Pathare; A. S. Jadhav; M. S. Shingare

    2007-01-01

    A simple, isocratic, rapid and accurate reversed phase high performance liquid chromatography method was developed for the\\u000a quantitative determination of tazarotene. The developed method is also applicable for the related substance determination\\u000a in bulk drugs. The chromatographic separation was achieved on a Hypersil C18 (250 mm ? 4.6 mm 5 ?m) column using water pH\\u000a 2.5 with orthophosphoric acid:acetonitrile (15:85, v\\/v) as a mobile phase.

  9. Stability-indicating chemometric methods for the determination of tazarotene.

    PubMed

    Saad, Ahmed S; Darwish, Hany W; Badawy, Amr M; Abd El-Aleem, Abd El-Aziz B

    2010-07-01

    Two multivariate calibration methods-principal component regression (PCR) and partial least square (PLS)-have been used to determine tazarotene in the presence of its degradation products. Both methods are useful in spectral analysis because of the simultaneous inclusion of many spectral wavelengths instead of the single wavelength used in derivative spectrophotometry. A great improvement in the precision and predictive abilities of these multivariate calibrations was observed. A calibration set was constructed for the mixture and the best model was used to predict the concentration of the selected drug. The proposed methods were applied successfully in the determination of tazarotene in laboratory-prepared mixtures and in commercial preparations. Tazarotene was analyzed with mean accuracies of 100.006 ± 0.695 and 100.007 ± 0.690 using the PCR and PLS methods, respectively. The validity of the proposed methods was assessed using the standard addition technique. The proposed methods were found to be rapid, simple and required no preliminary separation. They can therefore be used for the routine analysis of tazarotene in quality-control laboratories. PMID:20836144

  10. Analysis of Wheat Prolamins, the Causative Agents of Celiac Sprue, Using Reversed Phase High Performance Liquid Chromatography (RP-HPLC) and Matrix-Assisted Laser Desorption Ionization Time of Flight Mass Spectrometry (MALDI-TOF-MS)

    PubMed Central

    Mejías, Jaime H.; Lu, Xiaoqiao; Osorio, Claudia; Ullman, Jeffrey L.; von Wettstein, Diter; Rustgi, Sachin

    2014-01-01

    Wheat prolamins, commonly known as “gluten”, are a complex mixture of 71–78 proteins, which constitute ~80% of the proteins in the wheat grains and supply 50% of the global dietary protein demand. Prolamins are also responsible for numerous gluten-induced disorders and determine the unique visco-elastic properties of the wheat dough. These properties necessitate the reliable determination of the prolamin composition in wheat grains and their derived products. Therefore, this study examined the impact of HPLC conditions, including column type, column temperature, flow rate, and the gradient of polar and non-polar solvents in the mobile phase, to improve the analytical resolution of prolamins. The following conditions were found optimal for analyses: column temperature 60 °C, flow rate 1.0 mL/min and an elution gradient of 20%–60% of 0.1% trifluoroacetic acid + acetonitrile in 60 min. For further improvement of resolution, gliadin and glutenin extracts were analyzed using MALDI-TOF-MS in combination with HPLC fractionation. Two semi-quantitative methods, densitometry of stained polyacrylamide gels and HPLC, were used to determine relative prolamin quantities and the correspondence between the methods was established. The combinatorial gluten analyses approach developed during the present study was used to analyze prolamin profiles of wheat transformants expressing DEMETER silencing artificial microRNA, and the results are discussed. PMID:24739977

  11. Development and validation of new assay method for the simultaneous analysis of diltiazem, metformin, pioglitazone and rosiglitazone by RP-HPLC and its applications in pharmaceuticals and human serum.

    PubMed

    Sultana, Najma; Arayne, M Saeed; Shafi, Nighat; Siddiqui, Farhan Ahmed; Hussain, Azhar

    2011-01-01

    Simple, sensitive, rapid, and accurate high-performance liquid chromatographic (HPLC) method is developed and validated for the simultaneous determination of diltiazem, metformin, pioglitazone, and rosiglitazone hydrochloride in raw materials, their pharmaceutical formulations, and human serum. In HPLC, all the above drugs were chromatographed using acetonitrile-methanol-water (30:20:50, v/v, pH 2.59 ± 0.02) as the mobile phase at a flow rate of 1.0 mL/min at ambient temperature. The separation is carried out on a Hiber, 250-4.6 RP-18 column, equipped with a UV-vis detector at 230 nm. All the antidiabetic drugs eluted at different retention time and each showed a good resolution from diltiazem. The method is successfully applied to pharmaceutical formulations because no chromatographic interferences from the tablet excipients are found. The method is found to be linear, accurate, and precise with apposite detection and quantification limit. Suitability of the method for the quantitative determination of the drugs is proven by validation in accordance with the requirements laid down by International Conference on Harmonization (ICH) guidelines. The validation results, together with statistical treatment of the data, demonstrated the reliability of this method. PMID:22080805

  12. Characterization of CIMMYT bread wheats for high- and low-molecular weight glutenin subunits and other quality-related genes with SDS-PAGE, RP-HPLC and molecular markers

    Microsoft Academic Search

    Dan LiangJianwei; Jianwei Tang; Roberto Javier Peña; Ravi Singh; Xinyao He; Xiaoyong Shen; Danian Yao; Xianchun Xia; Zhonghu He

    2010-01-01

    Two hundred and seventy-three CIMMYT bread wheat cultivars and advanced lines grown under irrigated conditions in Mexico during\\u000a the 2005-06 Yaqui crop cycle were characterized for quality-related genetic traits using gene-specific markers for some high-\\u000a and low-molecular-weight glutenin subunit (HMW-GS and LMW-GS) genes, polyphenol oxidase (PPO), phytoene synthase (PSY), and\\u000a waxy genes. Of them, 142 were analyzed for quality parameters

  13. Development of a hyphenated procedure of heat-reflux and ultrasound-assisted extraction followed by RP-HPLC separation for the determination of three flavonoids content in Scutellaria barbata D. Don.

    PubMed

    Wei, Ming-Chi; Yang, Yu-Chiao; Chiu, Hui-Fen; Hong, Show-Jen

    2013-12-01

    A hyphenated procedure of heat-reflux and ultrasound-assisted extraction (HUAE), and an accurate high-performance liquid chromatographic (HPLC) method were developed for the determination of apigenin, baicalin and luteolin content in Scutellaria barbara D. Don. The suitable HUAE conditions for the extraction of target compounds from the herb were identified as an ultrasonic frequency of 40kHz, power of 185W, duty cycle of 75% (intermittent sonication), mean particle size of 0.355mm, extraction temperature of 50°C, ratio of solvent to raw material of 12:1 (mL/g), ethanol concentration of 60% (v/v), extraction time of 30min and three cycles. Compared with a traditional heat-reflux extraction method, the proposed method reduced the extraction time, extraction temperature and solvent consumption. Also, this HUAE method achieved superior apigenin, baicalin and luteolin yields. Furthermore, the developed HUAE-HPLC method was applied successfully for the simultaneous evaluation of three bioactive compounds in five samples of S. barbara D. Don obtained from different geographical regions. These results clearly demonstrated that the combined HUAE-HPLC process is feasible in the future commercialized manufacture of this highly valuable Chinese herbal medicine. PMID:24145017

  14. Environmental Treaties and Indicators Resource Indicators

    NSDL National Science Digital Library

    ENTRI is an international, collaborative effort hosted by the Consortium for International Earth Science Information Network (CIESIN) charged with providing "information about environmental treaties and national resource indicators." These treaties are organized into nine issue areas which cover land use change and desertification, transboundary air pollution, and trade and the environment, among others. Treaties can be searched or browsed. Free text searching of the treaties and treaty summaries is also available.

  15. Calculation of enviromental indices

    SciTech Connect

    NONE

    1995-10-01

    This portion of the Energy Vision 2020 draft report discusses the development of environmental indices. These indices were developed to be a quantitative measure of characterizing how TVA power system operations and alternative energy strategies might affect the environment. All indices were calculated relative to the reference strategy, and for the environmental review, the reference strategy was `no action`.

  16. Understanding Process Capability Indices

    Microsoft Academic Search

    Stefan Steiner; Bovas Abraham; Jock MacKay

    this article is answer such questions by providing an illustration of theimportant issues related to capability indices. In addition, this article makes suggestions regardingthe process information necessary to make appropriate use of capability indices. In the nextsection, the question of which capability index to use is addressed by contrasting the variouscommon indices. It is shown that the index P pk

  17. Science Indicators, 1974.

    ERIC Educational Resources Information Center

    National Science Foundation, Washington, DC. National Science Board.

    In this report the National Science Board presents the second step in the process begun with Science Indicators--1972 of developing indicators of the state of science in the United States. The goal of this effort is a periodical series of indices of the strengths and weaknesses of science and technology in the United States and the changing…

  18. Stability of laser heated flows

    NASA Technical Reports Server (NTRS)

    Wu, P. K. S.; Pirri, A. N.

    1976-01-01

    A local stability analysis is utilized to determine the stability of disturbances generated at each point along a nozzle of variable area ratio for a one-dimensional flow heated by laser radiation entering from the upstream direction. The governing equations for the quasi-one-dimensional flow without viscous dissipation, diffusion, and thermal conduction but including radiative heat transfer are given. The governing equations are combined to yield a relationship which governs the Mach number variation through the nozzle. The complete steady-state solution can be calculated from knowledge of the Mach number profile, the inlet conditions, and the laser power. The local stability analysis permits obtaining contour (or contours) of neutral stability. Solutions have been obtained for various nozzle configurations, but only one set of example calculations is presented. The results obtained indicate that the analysis serves as an important indicator as to where potential absorption wave phenomena may be initiated.

  19. Fuse status indicator system

    NASA Astrophysics Data System (ADS)

    Middlebrooks, H.

    1984-09-01

    An on-line indicator connected to each fuse of an electrical circuit includes an LED which becomes illuminated if its protected fuse blows. Groups of these on-line indicators can be connected via on OR gate to a single master fuse status indicator which also includes an LED which becomes illuminated if any of the on-line indicators connected thereto has its LED illuminated. The circuitry can accommodate power supplies of different voltages of either polarity. Opto-isolators can be used to reduce stand-by current drain and to isolate the on-line indicators from each other.

  20. Stability Tunnel

    NASA Technical Reports Server (NTRS)

    1943-01-01

    Engineers operate the controls of the Stability Tunnel: Plans for a new tunnel to study stability problems began in the late thirties. The Stability Tunnel was authorized in 1939 and began operations in June 1941. The installation was completed in December that year with the completion of a new 10,000 Horsepower Diesel-electric generating plant. It was a single return, closed jet tunnel with a 6-foot square test section. The tunnel was disassembled and shipped to Virginia Polytechnic Institute and State University in 1958. The tunnel had two separate test sections: one for curved flow, the other for rolling flow. 'The facility...simulates the motion of the aircraft in curved or rolling flight. This is done by actually curving or rolling the airstream as it passes over the model and at the same time providing the proper velocity distribution.' (From AIAA-80-0309) >From Alan Pope, Wind-Tunnel Testing: 'The only tunnel directly designed for dynamic stability work is located at the Langley Field branch of the NACA. Its most vital feature is its ability to subject the models to curving air streams that simulate those actually encountered when an airplane rolls, pitches, or yaws. the rotating airstream for simulating roll is produced by a motor-driven paddle just ahead of the test section. Curved air of properly varying velocity for simulating pitch and yaw is produced by a combination of a curved test section and velocity screens. The proper use of this apparatus makes possible the determination of the stability derivatives.' (pp. 13-14)

  1. Study on the stability of coal water slurry using dispersion-stability analyzer

    Microsoft Academic Search

    Peng-wei LI; Dong-jie YANG; Hong-ming LOU; Xue-qing QIU

    2008-01-01

    Effect of modified lignin series and naphthalene series dispersants on the stability of coal water slurry (CWS) and sedimentation behavior of coal particles were investigated using Turbiscan Lab dispersion-stability analyzer. The results indicate that the sedimentation behavior of coal particles of CWS belongs to differential sedimentation and there is a conglobation between coal particles in CWS preparation. Stability of CWS

  2. A whole soil stability index (WSSI) for evaluating soil aggregation

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Soil aggregate stability is an indicator of soil quality. However, there is no standard methodology for measuring soil aggregation or aggregate stability, particularly for determining a whole soil stability index. A whole soil stability index (WSSI) was developed here which combined data from dry ...

  3. A process capability indicator

    Microsoft Academic Search

    Lai K. Chan; T. K. Mak

    1993-01-01

    A new measure of process capability, called process capability indicator and denoted by C1is proposed. It is of the form C1=deviation indicator (DI)+w×variation indicator (VI), where DI and VI, are, respectively, measures of the deviation of the process mean from the target value and the process variation, and both are relative to the tolerance. The weight factor w is used

  4. Marine Organisms as Indicators

    NASA Astrophysics Data System (ADS)

    Weston, Donald P.

    The term “indicator organism” can have a variety of meanings. In its narrowest and perhaps most often used sense, an indicator organism is a single species whose abundance, physiological state, or reproductive success gives the investigator information about the environmental conditions to which it has been exposed. The indicator concept has been employed traditionally by regulatory agencies to assess the consequence of anthropogenic activity, using the indicator species as a surrogate for the ecosystem as a whole. The concept of a single-indicator species useful for such purposes is, however, as one of the editors points out, “illusory as the search for alchemist's gold,” and if the reader expects that this volume contains only a review of the use of indicator organisms in pollution monitoring, he or she will be greatly surprised. The editors have instead chosen a broad definition of indicator organisms and applications. The result is that the “indicator organism” may not be an organism at all (e.g., the paper by G. S. Kleppel on pigments as trophodynamic indicators), and the environmental information conveyed, such as climatic changes or the presence of mesoscale oceanic features, is most often unrelated to man's activities.

  5. Purification and characterization of type II collagen from chick sternal cartilage

    Microsoft Academic Search

    Hui Cao; Shi-Ying Xu

    2008-01-01

    Type II collagen was purified from sternal cartilage of the chick using a combination of pepsin digestion, NaCl precipitation and DEAE-sepharose CL 6B ion exchange chromatography. Pepsin-solubilized type II collagen of higher stability can be obtained with the extraction time of 32h, 0.5% pepsin concentration at 20°C. The purified preparation showed a single peak on RP-HPLC and a single band

  6. Power quality indicators

    Microsoft Academic Search

    X. Mamo; J. Javerzac

    2001-01-01

    The paper describes individual (relative to a particular disturbance) and global quality indicators designed to assist the French power transmission system operator as far as quality of supply is concerned. These indicators have been defined to be easily understood and manipulated by operators. As they are based on the \\

  7. Rehabilitation Indicators: An Overview.

    ERIC Educational Resources Information Center

    Brown, Margaret M.; And Others

    The purpose of the Rehabilitation Indicators Project is to develop a method, rehabilitation indicators (RI's), for defining multi-dimensionally the benefits that accrue to rehabilitation clients. RI's are presented as descriptors of observable elements of the rehabilitation client's life space with each descriptor inherently meaningful to client…

  8. Indicators of Quality.

    ERIC Educational Resources Information Center

    Cleary, Thomas S.

    2001-01-01

    Surveyed students, faculty, administrative staff, governing board, and employers affiliated with a public two-year college to determine their perceptions of various quality indicators and congruence between the groups. Found that all groups placed importance on indicators of customer satisfaction and skill development; beyond that, considerable…

  9. Robust process capability indices

    Microsoft Academic Search

    Sameer Prasad; Tom Bramorski

    1998-01-01

    Many organizations are mandating the use of process capability indices to measure and reduce variability. Managers may find the use of such indices as unreliable when the interaction of the dependency structure and outliers mask potential assignable causes of variation. A monitoring procedure is proposed that effectively classifies a series' variability into three components: (1) the underlying correlation structure, (2)

  10. Cobb's Red Cabbage Indicator.

    ERIC Educational Resources Information Center

    Cobb, Vicki

    1998-01-01

    Describes the use of an indicator made from the pigment in red cabbage. Cabbage is grated then soaked in water. When the water is a strong red, the cabbage is strained out. The cabbage-juice indicator is then used to test for acids and bases. Includes a list of good foods to test for acidity and alkalinity. (PVD)

  11. Chronic Disease Indicators

    NSDL National Science Digital Library

    Center for Disease Control

    The Chronic Disease Indicators (CDI) is a cross-cutting set of 97 indicators that were developed by consensus and that allows states and territories and large metropolitan areas to uniformly define, collect, and report chronic disease data that are important to public health practice and available for states, territories and large metropolitan areas. 

  12. Retractable Visual Indicator Assembly

    NASA Technical Reports Server (NTRS)

    Hackler, George R. (Inventor); Gamboa, Ronald J. (Inventor); Dominquez, Victor (Inventor)

    1998-01-01

    A retractable indicator assembly may be mounted on a container which transmits air through the container and removes deleterious gases with an activated charcoal medium in the container. The assembly includes: an elongate indicator housing has a chamber therein; a male adaptor with an external threads is used for sealing engagement with the container; a plug located at the upper end of the housing; a housing that includes a transparent wall portion for viewing at least a portion of the chamber; a litmus indicator, moveable by a retractable rod from a retracted position within the container to an extended position within the chamber of the housing; and an outer housing that is secured to the upper end of the rod, and protects the indicator housing while the litmus indicator is in its normally retracted position. The assembly may be manually manipulated between its extended position wherein the litmus indicator may be viewed through the transparent wall of the indicator housing, and a retracted position wherein the outer housing encloses the indicator housing and engages the exterior of the container.

  13. Cabbage Juice Indicator

    NSDL National Science Digital Library

    The Science House

    2014-01-28

    In this chemistry activity, learners make indicator solution from red cabbage. Then, learners test everyday foods and household substances using the cabbage juice indicator. Learners will record the color change, approximate pH (using the pH scale), and identify if it is an acid or base. As an extension, learners can make pH paper strips to conduct an "at home" pH test of other household items. The indicator solution can be frozen in ice trays and when mixed with alcohol, can last for months. For safety reasons, adult supervision is recommended.

  14. Development and application of a novel, dual-mode gradient, stability-indicating HPLC-DAD method for the simultaneous determination and purity assessment of mebeverine hydrochloride, diloxanide furoate and their corresponding major degradation products in combination with some gastrointestinal drugs in the form of oral doses.

    PubMed

    Mabrouk, Mokhtar; El-Fatatry, Hamed; Hewala, Ismail; Emam, Ehab

    2013-09-01

    A simple, precise, rapid, stability-indicating reversed phase high performance liquid chromatographic method with photodiode array detection was developed and validated for the determination of mebeverine hydrochloride in combination with sulpiride or with diloxanide furoate and metronidazole in the presence of their corresponding degradation products. Optimum separation was achieved in less than 10 min using an X-Bridge C18 column (150 mm × 4.6 mm i.d., 3.5 ?m particle size); elution was accomplished via the application of a dual-mode solvent and flow rate gradient system. This elution system enables the separation of nine components within a cycle time of 15 min and with a resolution greater than 2.5. Detection was conducted at 230 nm, and purity assessment was performed using a photodiode array detector. The method has been validated with respect to specificity, linearity, accuracy, precision, limit of quantitation, limit of detection, robustness and ruggedness. The validation criteria were met in all cases. The developed HPLC method was successfully applied to commercial tablets. It was shown that this method is very sensitive to the determination of the degradation products, downward to 0.1 w/w% levels, which is far below the limits for testing these degradation products within their corresponding intact drugs. PMID:23770637

  15. Health expectancy indicators.

    PubMed Central

    Robine, J. M.; Romieu, I.; Cambois, E.

    1999-01-01

    An outline is presented of progress in the development of health expectancy indicators, which are growing in importance as a means of assessing the health status of populations and determining public health priorities. PMID:10083720

  16. ENVIRONMENTAL PUBLIC HEALTH INDICATORS

    EPA Science Inventory

    Environmental Public Health Indicators (EPHIs), quantitative measures of health factors and environmental influences tracked over time, can be used to identify specific areas and populations for intervention and prevention efforts and to evaluate the outcomes of implemented polic...

  17. Industrial energy use indices 

    E-print Network

    Hanegan, Andrew Aaron

    2008-10-10

    Energy use index (EUI) is an important measure of energy use which normalizes energy use by dividing by building area. Energy use indices and associated coefficients of variation are computed for major industry categories ...

  18. Industrial energy use indices 

    E-print Network

    Hanegan, Andrew Aaron

    2009-05-15

    Energy use index (EUI) is an important measure of energy use which normalizes energy use by dividing by building area. Energy use indices and associated coefficients of variation are computed for major industry categories ...

  19. World Development Indicators

    NSDL National Science Digital Library

    Published by the World Bank Group, World Development Indicators is an annual report containing statistical data on global topics such as people, environment, the economy, and states and markets. The Website for World Development Indicators provides all of the text of the report, but it only contains a small selection of the tables offered in the actual report, which is available on CD ROM for purchasing.

  20. On the crisis stability of a submarine deterrent

    SciTech Connect

    Canavan, G.H.

    1992-05-01

    Without defenses, stability indices fall monotonically as the number of submarine-launched ballistic missiles (SLBMs) is reduced. For few SLBMs, the favorable stability properties of the survivable SLBMs are masked by the unfavorable stability properties of the non-survivable land missiles. With ground-based interceptor (GBI) defenses, stability initially falls faster. The number of GBIs could be increased gradually to minimize their impact on stability.

  1. Stability of climate reconstructions

    NASA Astrophysics Data System (ADS)

    Lohmann, Gerrit; Rimbu, Norel; Wagner, Axel; Dima, Mihai

    2014-05-01

    Reconstruction of climate mode indices using proxy data as predictors is limited due to non-stationarity in atmospheric teleconnections. In this paper a method is presented to identify stable predictors for the reconstruction of the Arctic Oscillation (AO) index. Using the 20th Century reanalysis data, the AO index is calculated for the last 140 years and correlated with global two meter temperature, precipitation, and sea surface temperature anomalies in various moving windows. The stability of the correlation was checked in every point of the global grids. Anomalies from the regions where the correlation of the AO index is stable are used as stable predictors for the AO index. It is shown that the predictors identified through our analysis lead to proper AO reconstructions. Statistical analysis of a global climate simulation covering the last millennium reveals that the stability correlation map of model AO and temperature are very similar to the corresponding observed correlation stability map. It is shown that the stability correlation maps of the AO, as derived from the model, are insensitive to different climate forcing and can be used to systematically select stable predictors for the AO reconstruction during the last millennium and most likely for the late Holocene. Finally, several high resolution proxy data from the stable regions are selected and used for a reconstruction of the AO index during the last three centuries. We argue that selection of proxy data from the stable regions of AO teleconnections leads to a suitable AO reconstruction. Furthermore, the hypothesis of stable teleconnections is tested using atmospheric circulation model experiments. For climate conditions with other ice sheet distributions on the Northern Hemisphere, such as the last glacial maximum climate, considerable changes are detected in the atmospheric variability pattern compared to the present day. Correlation maps of pseudo proxy records over Europe, the Red Sea area, and Greenland indicate that the associated wind pattern can change drastically. During glacial times, Greenland ice cores indicate cold and warm phases in the northern North Atlantic. When looking in detail for the interannual variability for these phases, model simulations indicate that Greenland temperature variations are linked to distinct large-scale Northern Hemisphere circulation patterns and associated local wind directions. It is argued that such analysis provides a dynamical interpretation of past climate variability. With the combined use of models and data, one can examine the representativeness of sites where the reconstructions are available.

  2. Stabilization and intestinal absorption of human calcitonin

    Microsoft Academic Search

    M. Baudys; D. Mix; S. W. Kim

    1996-01-01

    The effect of different excipients and\\/or surface active compounds on the stability of human calcitonin in aqueous solution was studied. Calcitonin solution was partially stabilized with dilute acetic acid (0.01% (w\\/v) or higher), and among many tested surfactants, only lauryl sulfate proved to be a very efficient long-term stabilizer (1 year or more). Concentration dependency studies indicated that lauryl sulfate

  3. Research on Indicators of Early Warning in Low Frequency Oscillation Based on Energy Function Theory

    Microsoft Academic Search

    Yong Huang; Chao Dong; Dichen Liu; Qingfen Liao; Enze Chen; Zheng Zeng

    2011-01-01

    This paper simplified the classical transient energy function based on center of inertia, improved the classical indicators of the stability margin, and put forward the indicator of the stability margin increment. The indicator was established on the basis of the tie-line observational section in power system, and the calculation was simple and convenient, not only achieving early warnings of low

  4. Internationally Comparable Health Indices

    PubMed Central

    Meijer, Erik; Kapteyn, Arie; Andreyeva, Tatiana

    2013-01-01

    One of the most intractable problems in international health research is the lack of comparability of health measures across countries or cultures. We develop a cross-country measurement model for health in which functional limitations, self-reports of health, and a physical measure are interrelated to construct health indices. To establish comparability across countries, we define the measurement scales by the physical measure while other parameters vary by country to reflect cultural and linguistic differences in response patterns. We find significant cross-country variation in response styles of health reports along with variability in genuine health that is related to differences in national income. Our health indices achieve satisfactory reliability of about 80% and their gradients by age, income, and wealth for the most part show the expected patterns. Moreover, the health indices correlate much more strongly with income and net worth than self reported health measures. PMID:20572201

  5. LEADING WITH LEADING INDICATORS

    Microsoft Academic Search

    2005-01-01

    This paper documents Fluor Hanford's use of Leading Indicators, management leadership, and statistical methodology in order to improve safe performance of work. By applying these methods, Fluor Hanford achieved a significant reduction in injury rates in 2003 and 2004, and the improvement continues today. The integration of data, leadership, and teamwork pays off with improved safety performance and credibility with

  6. Indicators of Reading Education.

    ERIC Educational Resources Information Center

    Guthrie, John T.

    Monitoring the effectiveness of reading education is central to the appraisal of the productivity of schooling, yet most measures currently being used do not take into account the full range of processes which lead to successful reading education. A model of indicators relevant to reading education (outcome, process, and input) can be used to…

  7. Universal Indicator Rainbow Trout

    NSDL National Science Digital Library

    2013-07-08

    In this activity on page 2 of the PDF, learners discover how color changes can help scientists distinguish between acids and bases. Learners create colorful rainbow trout artwork using universal indicator solution and various household liquids. Safety note: learners must wear safety goggles.

  8. Slickenside kinematic indicators

    Microsoft Academic Search

    Miguel Doblas; Consejo Superior de Investigaciones; JoseGutierrez Abascal

    1998-01-01

    A new classification of slickenside kinematic indicators is presented based on 61 criteria. These slickensides have been subdivided into eleven major groups: `V' or crescentic markings, steps, fractures, trains of inclined planar structures, trailed material, asymmetric elevations, deformed elements, mineralogical\\/crystallographic orientations, asymmetric plan-view features, asymmetric cavities, and asymmetric folds. This classification constitutes a useful tool for geologists interested in the

  9. Indications for Fetal Echocardiography

    Microsoft Academic Search

    M. Small; J. A. Copel

    2004-01-01

    Congenital heart disease is one of the most common congenital malformations diagnosed in liveborns. As more women undergo prenatal diagnosis, the need for screening fetal echocadiography increases. The fetal, maternal, and familial indications for fetal echocadiography are outlined in order to improve the identification of women in greatest need for this screening modality.

  10. MATLAB Stability and Control Toolbox Trim and Static Stability Module

    NASA Technical Reports Server (NTRS)

    Kenny, Sean P.; Crespo, Luis

    2012-01-01

    MATLAB Stability and Control Toolbox (MASCOT) utilizes geometric, aerodynamic, and inertial inputs to calculate air vehicle stability in a variety of critical flight conditions. The code is based on fundamental, non-linear equations of motion and is able to translate results into a qualitative, graphical scale useful to the non-expert. MASCOT was created to provide the conceptual aircraft designer accurate predictions of air vehicle stability and control characteristics. The code takes as input mass property data in the form of an inertia tensor, aerodynamic loading data, and propulsion (i.e. thrust) loading data. Using fundamental nonlinear equations of motion, MASCOT then calculates vehicle trim and static stability data for the desired flight condition(s). Available flight conditions include six horizontal and six landing rotation conditions with varying options for engine out, crosswind, and sideslip, plus three take-off rotation conditions. Results are displayed through a unique graphical interface developed to provide the non-stability and control expert conceptual design engineer a qualitative scale indicating whether the vehicle has acceptable, marginal, or unacceptable static stability characteristics. If desired, the user can also examine the detailed, quantitative results.

  11. Composite stabilizer unit

    DOEpatents

    Ebaugh, Larry R. (Los Alamos, NM); Sadler, Collin P. (Los Alamos, NM); Carter, Gary D. (Espanola, NM)

    1992-01-01

    An improved fin stabilized projectile including multiple stabilizer fins upon a stabilizer unit situated at the aft end of the projectile is provided, the improvement wherein the stabilizer fins are joined into the stabillizer unit by an injection molded engineering grade polymer.

  12. LEADING WITH LEADING INDICATORS

    SciTech Connect

    PREVETTE, S.S.

    2005-01-27

    This paper documents Fluor Hanford's use of Leading Indicators, management leadership, and statistical methodology in order to improve safe performance of work. By applying these methods, Fluor Hanford achieved a significant reduction in injury rates in 2003 and 2004, and the improvement continues today. The integration of data, leadership, and teamwork pays off with improved safety performance and credibility with the customer. The use of Statistical Process Control, Pareto Charts, and Systems Thinking and their effect on management decisions and employee involvement are discussed. Included are practical examples of choosing leading indicators. A statistically based color coded dashboard presentation system methodology is provided. These tools, management theories and methods, coupled with involved leadership and employee efforts, directly led to significant improvements in worker safety and health, and environmental protection and restoration at one of the nation's largest nuclear cleanup sites.

  13. THE VIOLOGEN INDICATORS

    PubMed Central

    Michaelis, L.; Hill, Edgar S.

    1933-01-01

    The tabulation gives the normal potentials of the various indicators at 30°C.; referred to the normal hydrogen electrode, the accuracy is estimated to be ±0.002 volt. Normal potentials of the viologens at 30°C.: Methyl viologen –0.446 volts Ethyl viologen –0.449 volts Betaine viologen –0.444 volts Benzyl viologen –0.359 volts Supposing some solution brings about a coloration of one of these indicators to the extent of A per cent of the maximum color, the oxidation-reduction potential of this solution is E = Eo – 0.06 log See PDF for Equation where Eo is the normal potential according to the above tabulation. This normal potential is independent of pH. PMID:19872744

  14. Tamper-indicating seal

    DOEpatents

    Fiarman, Sidney (Port Jefferson, NY); Degen, Michael F. (Patchogue, NY); Peters, Henry F. (Brookhaven, NY)

    1985-01-01

    There is disclosed a tamper-indicating seal that permits in the field inspection and detection of tampering. Said seal comprises a shrinkable tube having a visible pattern of markings which is shrunk over the item to be sealed, and a second transparent tube, having a second visible marking pattern, which is shrunk over the item and the first tube. The relationship between the first and second set of markings produces a pattern so that the seal may not be removed without detection.

  15. Videourodynamics: indications and technique.

    PubMed

    Marks, Brian K; Goldman, Howard B

    2014-08-01

    Videourodynamics combines fluoroscopic voiding cystourethrography with multichannel urodynamics to better evaluate lower urinary tract symptoms. This article reviews current literature and guidelines outlining the indications for obtaining this specialized study as well as technique. Appropriate and judicious use of fluoro-urodynamics lends to improved diagnostic acumen in a well-selected patient population; however, clinicians must be mindful of the added cost, safety concerns, and limitations of its use. PMID:25063594

  16. Indicators for Inquiry

    NSDL National Science Digital Library

    Jeffery Townsend

    2006-02-01

    Fifth-grade students use homemade plant-based acid/base indicators to learn about matter at an age-appropriate level and develop process skills. As a result of completing this lesson sequence the students should be able to perform many tasks using process skills such as observing chemical changes; identifying acids and bases by performing tests; classifying common household substances as acidic, basic (alkaline), or neutral; and developing a scheme for solving a performance-based scenario.

  17. High-performance liquid chromatographic determination of Maillard compounds in store-brand and name-brand ultra-high-temperature-treated cows’ milk

    Microsoft Academic Search

    E Ferrer; A Alegr??a; G Courtois; R Farré

    2000-01-01

    Furosine and furfural products of the Maillard reaction are used as specific indicators of the effect of heating treatments on milk quality. Their contents were measured in representative samples of store- and name-brand ultra-high-temperature-treated milks using RP-HPLC with UV detection. Furosine contents ranged from 40.32 to 50.67 and from 65.48 to 310.58 mg\\/100 g protein in name- and store-brand milks,

  18. Peptidomimetics to mimic protein-protein interactions 

    E-print Network

    Xia, Zebin

    2005-08-29

    ) and TOCSY spectrum (b) of compound 29a........................ 108 Figure 4.9. (a) Selected HPLC traces indicating the product distribution of the desired product 10bu relative to the impurities 34 and 35; and (b... hexafluorophosphate DAB-Am-n poly(propylene imine)dendrimer Tris tris(hydroxymethyl)aminomethane HFIP hexafluoroisopropanol IgG immunoglobulin G RP-HPLC reverse phase high performance liquid chromatography QMD quenched molecular dynamics SD steepest decent ABNR...

  19. Aplysia Attractin: Biophysical Characterization and Modeling of a Water-Borne Pheromone

    Microsoft Academic Search

    Catherine H. Schein; Gregg T. Nagle; Jason S. Page; Jonathan V. Sweedler; Yuan Xu; Sherry D. Painter; Werner Braun

    2001-01-01

    Attractin, a 58-residue protein secreted by the mollusk Aplysia californica, stimulates sexually mature animals to approach egg cordons. Attractin from five different Aplysia species are ?40% identical in sequence. Recombinant attractin, expressed in insect cells and purified by reverse-phase high-performance liquid chromatography (RP-HPLC), is active in a bioassay using A. brasiliana; its circular dichroism (CD) spectrum indicates a predominantly ?-helical

  20. Tamper-indicating seal

    DOEpatents

    Fiarman, S.; Degen, M.F.; Peters, H.F.

    1982-08-13

    There is disclosed a tamper-indicating seal that permits in the field inspection and detection of tampering. Said seal comprises a shrinkable tube having a visible pattern of markings which is shrunk over th item to be sealed, and a second transparent tube, having a second visible marking pattern, which is shrunk over the item and the first tube. The relationship between the first and second set of markings produces a pattern so that the seal may not be removed without detection. The seal is particularly applicable to UF/sub 6/ cylinder valves.

  1. Slickenside kinematic indicators

    NASA Astrophysics Data System (ADS)

    Doblas, Miguel

    1998-09-01

    A new classification of slickenside kinematic indicators is presented based on 61 criteria. These slickensides have been subdivided into eleven major groups: `V' or crescentic markings, steps, fractures, trains of inclined planar structures, trailed material, asymmetric elevations, deformed elements, mineralogical/crystallographic orientations, asymmetric plan-view features, asymmetric cavities, and asymmetric folds. This classification constitutes a useful tool for geologists interested in the determination of the shear sense in fault surfaces bearing slickensides. Examples of application of this classification to natural fault surfaces at different scales are presented.

  2. Tamper indicating packaging

    SciTech Connect

    Baumann, M.J.; Bartberger, J.C.; Welch, T.D.

    1994-08-01

    Protecting sensitive items from undetected tampering in an unattended environment is crucial to the success of non-proliferation efforts relying on the verification of critical activities. Tamper Indicating Packaging (TIP) technologies are applied to containers, packages, and equipment that require an indication of a tamper attempt. Examples include: the transportation and storage of nuclear material, the operation and shipment of surveillance equipment and monitoring sensors, and the retail storage of medicine and food products. The spectrum of adversarial tampering ranges from attempted concealment of a pin-hole sized penetration to the complete container replacement, which would involve counterfeiting efforts of various degrees. Sandia National Laboratories (SNL) has developed a technology base for advanced TIP materials, sensors, designs, and processes which can be adapted to various future monitoring systems. The purpose of this technology base is to investigate potential new technologies, and to perform basic research of advanced technologies. This paper will describe the theory of TIP technologies and recent investigations of TIP technologies at SNL.

  3. Breathiness in Indic languages

    NASA Astrophysics Data System (ADS)

    Esposito, Christina; Khan, Sameeruddowla; Hurst, Alex

    2005-04-01

    Previous work on breathiness in Indic languages has focused on the acoustic properties of breathy oral stops in languages like Hindi ([bal] hair versus [bhal] forehead) or Bengali ([baSa] house versus [bhaSa] language). However, breathiness in Indic languages often extends to nasals (e.g., Marathi ([maar] beat versus [mhaar] a caste). It is unclear if languages such as Hindi and Bengali have breathy nasals in addition to breathy oral stops. This study addresses the following questions: (1) Are breathy nasals (Nh) acoustically different from N+h sequences, both in languages where they are phonemic and ones where they are not? (2) In sequences of a breathy stop and a modal nasal (e.g., Hindi [udhmi] naughty) where is the breathiness realized, if at all? To answer these questions, audio, aerodynamic, and electroglottographic recordings will be made of Hindi, Bengali, and Marathi speakers. It is hypothesized that acoustically breathy nasals in Hindi and Bengali will not be distinct from sequences of N+ h. We believe that this will also be true for the oral stops. In addition, it is believed that in sequences of breathy oral stop followed by a modal nasal (e.g., ChN), the breathiness will be produced on the nasal.

  4. Molecular Models of Indicators

    NSDL National Science Digital Library

    The article by Nicholas C. Thomas and Stephen Faulk on "Colorful Chemical Fountains" (1) reminds us that color—the colors of acid–base indicators or of metal complexes—is responsible for many of us developing an interest in chemistry. The featured molecules this month are the acid and base forms of three common indicators–phenolphthalein, methyl orange, and methyl red. These three substances display interesting structural features as the pH-induced transformation from one form to another takes place in three different ways. In the case of phenolphthalein, the lactam ring is cleaved on deprotonation to produce a carboxyl group with the concomitant removal of a proton from a phenolic group. In methyl orange, one of the nitrogen atoms is protonated in the acid form, and that proton is lost in the base form. In methyl red, a carboxylic acid function is deprotonated. There are many other interesting aspects of acid–base indicators. Since most plants and fruits contain pigments that show a color change in some pH range, it is difficult to state with any degree of certainty when these changes were first put to use in a systematic fashion. The Spanish alchemist Arnaldus de Villa Nova (Arnold of Villanova) is purported to have used litmus in the early 14th century. In general systematic use of indicators is traced to the latter half of the nineteenth century with the development of the three synthetic indicators described above. Many students will be familiar with the use of phenolphthalein to identify blood—often shown on the various forensic chemistry TV dramas by dropping some solution on a cotton swab that has been used to pick up some of the sample in question. If the swab turns red we frequently hear "It's blood". The reality of using phenolphthalein in this way is more complicated. The test is presumptive for the presence of blood, but not conclusive. It is not an acid–base reaction but rather, in the presence of hydrogen peroxide, relies on hemoglobin to catalyze the oxidation of phenolphthalein. An interesting assignment for students in a high-school or non-majors course would be to have them explore the details of this Kastle–Meyers test to see just what is involved in the correct application of the test, and what factors complicate the process. For example, would tomato juice infused with asparagus juice give a positive Kastle–Meyers test? Historically phenolphthalein was used in a variety of laxatives. Recently that usage has been discontinued due to concern about the carcinogenic nature of the substance. A review of the history of the controversy surrounding the use of phenolphthalein in laxatives would make a good research paper at the high-school level. Lastly, students with some practice building structures and performing calculations might wish to explore the structures of two other forms of phenolphthalein—one found in very acidic solutions, having an orange color, and one found in very basic solutions that is colorless.

  5. [Indications and results of kypho- and vertebroplasty].

    PubMed

    Kasperk, C; Nöldge, G; Grafe, I; Meeder, P; Huber, F; Nawroth, P

    2008-10-01

    The best currently available evidence based treatment reduces vertebral fracture risk but does not totally prevent osteoporotic and malignant follow-up fractures. Kyphoplasty and vertebroplasty are options of a causal treatment to reduce pain by internal stabilization of fractured vertebrae. The indication for these minimal invasive procedures requires an interdisciplinary discussion of the individual case to guarantee technical feasibility, to increase the likelihood that these procedures will indeed reduce pain and to embed these procedures into the long term therapeutic concept of every single patient. In addition to internal stabilization of a painfully fractured vertebra kyphoplasty also seeks to restore lost vertebral height which appears promising in acute vertebral fractures. Due to the procedure there are more cement leakages after vertebroplasty. Available controlled prospective studies demonstrate only for kyphoplasty a long-term benefit for the patient in terms of pain reduction, increased mobility and improved quality of life. PMID:18719874

  6. National Neighborhood Indicators Partnership

    NSDL National Science Digital Library

    The National Neighborhood Indicators Partnership works "to build local capacity" through a range of activities, including the creation of apps, outreach projects, and much more. Visitors can look over the Partnershipâ??s Featured area to get a sense of its recent initiatives which include the creation of integrated data systems and neighborhood centers. The Activities area includes Issue Areas which feature publications and presentations on matters that include absenteeism, affordable housing, children, and community development. The Library includes online guides on local data sharing, a user conference directory, and short stories from partners on their own work. The site is rounded out by the Data & Tech section with summary information on the local neighborhood-level data held by numerous community partners throughout the United States.

  7. The masticatory normative indicator.

    PubMed

    Woda, A; Nicolas, E; Mishellany-Dutour, A; Hennequin, M; Mazille, M-N; Veyrune, J-L; Peyron, M-A

    2010-03-01

    There is no established quantitative, objective method to differentiate individuals with good masticatory function from those lacking this attribute. The aim of this study was to specify a normal range of median particle size values for masticated raw carrots collected just before being swallowed. The masticatory normative indicator (MNI) value thus obtained was based on seven studies carried out by different investigators using different methods for measuring particle size in carrot boluses. A simple mathematical transformation of variables and the choice of an interval of +/-1.96 times the standard deviation gave 4.0 mm as the upper limit of normal median particle size for carrots in a population of young persons with good oral health. This value identifies boluses that may be considered as resulting from impaired mastication, as illustrated in healthy individuals with experimentally hampered mastication, denture wearers, and individuals presenting with obesity or Down syndrome. PMID:20118433

  8. Enhanced tamper indicator

    DOEpatents

    Garcia, Anthony R.; Johnston, Roger G.

    2003-07-08

    The present invention provides an apparatus and method whereby the reliability and tamper-resistance of tamper indicators can be improved. A flexible connector may be routed through a latch for an enclosure such as a door or container, and the free ends of the flexible connector may be passed through a first locking member and firmly attached to an insert through the use of one or more attachment members such as set screws. A second locking member may then be assembled in interlocking relation with the first locking member to form an interlocked assembly around the insert. The insert may have one or more sharp projections extending toward the first or second locking member so that any compressive force applied in an attempt to disassemble the interlocked assembly results in permanent, visible damage to the first or second locking member.

  9. International energy indicators

    NASA Astrophysics Data System (ADS)

    Rossi, E., Jr.

    1981-12-01

    Data on international energy indicators were tabulated and graphically represented. The following data are presented: world crude oil production, 1974 to October 1981; OPEC crude oil productive capacity; world crude oil and refined product inventory levels, 1975 to October, 1981; oil consumption in OECD countries, 1975 to October 1981; USSR crude oil production and exports, 1975 to October 1981; free world and US nuclear electricity generation, 1973 to December, 1981 and current capacity. Specific US data presented are: US domestic oil supply, 1977 to June, 1981; US gross imports of crude oil and products, 1973 to October, 1981; landed cost of Saudi crude current and 1974 dollars; US coal trade, 1975 to September, 1981; US natural gas trade, 1981; and energy/GNP ratio.

  10. Precipitation Indices Low Countries

    NASA Astrophysics Data System (ADS)

    van Engelen, A. F. V.; Ynsen, F.; Buisman, J.; van der Schrier, G.

    2009-09-01

    Since 1995, KNMI published a series of books(1), presenting an annual reconstruction of weather and climate in the Low Countries, covering the period AD 763-present, or roughly, the last millennium. The reconstructions are based on the interpretation of documentary sources predominantly and comparison with other proxies and instrumental observations. The series also comprises a number of classifications. Amongst them annual classifications for winter and summer temperature and for winter and summer dryness-wetness. The classification of temperature have been reworked into peer reviewed (2) series (AD 1000-present) of seasonal temperatures and temperature indices, the so called LCT (Low Countries Temperature) series, now incorporated in the Millennium databases. Recently we started a study to convert the dryness-wetness classifications into a series of precipitation; the so called LCP (Low Countries Precipitation) series. A brief outline is given here of the applied methodology and preliminary results. The WMO definition for meteorological drought has been followed being that a period is called wet respectively dry when the amount of precipitation is considerable more respectively less than usual (normal). To gain a more quantitative insight for four locations, geographically spread over the Low Countries area (De Bilt, Vlissingen, Maastricht and Uccle), we analysed the statistics of daily precipitation series, covering the period 1900-present. This brought us to the following definition, valid for the Low Countries: A period is considered as (very) dry respectively (very) wet if over a continuous period of at least 60 days (~two months) cq 90 days (~three months) on at least two out of the four locations 50% less resp. 50% more than the normal amount for the location (based on the 1961-1990 normal period) has been measured. This results into the following classification into five drought classes hat could be applied to non instrumental observations: Very wet period (+2): Wide scale river flooding, marshy acres and meadows.-Farmers cope with poor harvests of hay, grains, fruit etc. resulting in famines.-Late grape harvests, poor yield quantity and quality of wine. Wet period (+1): High water levels cq discharges of major rivers, tributaries and brooks, local river floodings, marshy acres and meadows in the low lying areas.-Wearisome and hampered agriculture. Normal (0) Dry period (-1): Low water levels cq discharges of major rivers, tributaries and brooks. Some brooks may dry up.-Summer half year: local short of yield of grass, hay and other forage.-Summer half year: moor-, peat- and forest fires. Very dry period (-2): Very low water levels cq discharges of major rivers and tributaries. Brooks and wells dry up. Serious shortage of drinking water; especially in summer.-Major agricultural damage, shortage of water, mortality stock of cattle. Shortage of grain. Flour can not be produced due to water mills running out of water, shortage of bread, bread riots, famines.-Large scale forest and peat areas, resulting in serious air pollution. Town fires. By verifying the historical evidence on these criterions, a series of 5 step indices ranging from very dry to very wet for summer and winter half year of the Low Countries was obtained. Subsequently these indices series were compared with the instrumentally observed seasonal precipitation sums for De Bilt (1735-2008), which is considered to be representative for the Central Netherlands. For winter (Oct-March) and summer half year (Apr.-Sept.) the accumulated precipitation amounts are calculated; these amounts are approximately normally distributed. Based on this distribution, the cumulative frequency distribution is calculated. By tabulating the number of summers in the pre-instrumental period 1201-1750 for each of the drought classes, a distribution is calculated which is then related to the modern accumulated precipitation distribution. Assuming that the accumulated precipitation amount has not been below (above) the mean precipitation minus (plus) three standard deviations for

  11. Technology and indications.

    PubMed

    Sunada, Keijiro; Yamamoto, Hironori

    2009-07-01

    Double-balloon endoscopy (DBE) was developed based on the principle of preventing stretching of the intestinal tract by anchoring the convoluted intestinal tract with an endoscope and overtube fitted with inflatable balloons. The DBE system includes the main body of the endoscope with a built-in air channel, a balloon attached to the tip of the endoscope, an overtube with a hydrophilic coating equipped with an inflatable balloon, and a balloon controller that safely inflates/deflates the two balloons. At present, there are three different types of endoscopes for DBE. The indications for DBE include the diagnosis or treatment of various small intestinal conditions such as obscure gastrointestinal bleeding, Crohn's disease, and benign and malignant tumors. In addition, DBE can be used to approach the surgically modified intestinal tract; conventional endoscopes have difficulty in that situation. DBE can be used for colonoscopy in cases in which it is difficult to insert a conventional colonoscope. In the future, DBE will have the potential for wider use in routine colonoscopy because the insertion technique is easy and reliable. PMID:19647642

  12. Ergodicity of financial indices

    NASA Astrophysics Data System (ADS)

    Kolesnikov, A. V.; Rühl, T.

    2010-05-01

    We introduce the concept of the ensemble averaging for financial markets. We address the question of equality of ensemble and time averaging in their sequence and investigate if these averagings are equivalent for large amount of equity indices and branches. We start with the model of Gaussian-distributed returns, equal-weighted stocks in each index and absence of correlations within a single day and show that even this oversimplified model captures already the run of the corresponding index reasonably well due to its self-averaging properties. We introduce the concept of the instant cross-sectional volatility and discuss its relation to the ordinary time-resolved counterpart. The role of the cross-sectional volatility for the description of the corresponding index as well as the role of correlations between the single stocks and the role of non-Gaussianity of stock distributions is briefly discussed. Our model reveals quickly and efficiently some anomalies or bubbles in a particular financial market and gives an estimate of how large these effects can be and how quickly they disappear.

  13. Cepheids as Distance Indicators

    E-print Network

    N. R. Tanvir

    1996-11-04

    We review the use of Cepheids as distance indicators with particular emphasis on the methods which have been applied to HST observations of Cepheids. The calibration of the period-luminosity relations is examined in detail and we identify possible problems with the existing calibrations. New V- and I-band period luminosity relations are presented based on a sample of 53 Cepheids in the LMC with photometry drawn from the literature. These revised PL relations result in a systematic decrease of approx 0.1 magnitudes in distance moduli derived using the standard method of extinction correction. Hence estimates of the Hubble constant based on such distances should be increased by $\\sim5%$. Other aspects of Cepheid distance determination, specifically incompleteness bias, metallicity dependence, the effects of crowding and contamination of samples by non-Cepheids are also discussed. We conclude that current HST distance estimates to individual galaxies are probably good to about 10%, but that much of this error is systematic. Efforts to reduce the systematics, therefore, for example by improving the photometric calibration, refining the distance to the LMC, and reobserving the Cepheid galaxies in the infrared with NICMOS, will give large returns.

  14. High Stability Engine Control (HISTEC)

    NASA Technical Reports Server (NTRS)

    DeLaat, John C.; Southwick, Robert D.; Gallops, George W.

    1996-01-01

    Future aircraft turbine engines, both commercial and military, must be able to successfully accommodate expected increased levels of steady-state and dynamic engine-face distortion. The current approach of incorporating a sufficient component design stall margin to tolerate these increased levels of distortion would significantly reduce performance. The objective of the High Stability Engine Control (HISTEC) program is to design, develop, and flight demonstrate an advanced, high-stability, integrated engine control system that uses measurement-based, real-time estimates of distortion to enhance engine stability. The resulting distortion tolerant control reduces the required design stall margin, with a corresponding increase in performance and decrease in fuel burn. The HISTEC concept, consisting of a Distortion Estimation System and a Stability Management Control, has been designed and developed. The Distortion Estimation System uses a small number of high-response pressure sensors at the engine face to calculate indicators of the type and extent of distortion in real time. The Stability Management Control, through direct control of the fan and compressor pressure ratio, accommodates the distortion by transiently increasing the amount of stall margin available based on information from the Distortion Estimation System. Simulation studies have shown the HISTEC distortion tolerant control is able to successfully estimate and accommodate time-varying distortion. Currently, hardware and software systems necessary for flight demonstration of the HISTEC concept are being designed and developed. The HISTEC concept will be flight tested in early 1997.

  15. Chromatographic behavior of peptides containing oxidized methionine residues in proteomic LC-MS experiments: Complex tale of a simple modification.

    PubMed

    Lao, Ying W; Gungormusler-Yilmaz, Mine; Shuvo, Sabbir; Verbeke, Tobin; Spicer, Vic; Krokhin, Oleg V

    2015-07-01

    On average, the oxidation of a single Met residue to Mso (methionine S-oxide, methionine sulfoxide) and Msn (methionine S,S-dioxide, methionine sulfone) decreases peptide retention in RP HPLC by 2.37 and 1.95 Hydrophobicity Index units (% acetonitrile), respectively. At the same time, the magnitude of the retention shift varies greatly (-9.1 to +0.4% acetonitrile for Mso) depending on peptide sequence. The latter effects are mostly associated with the stabilization of secondary structures upon peptide interaction with the hydrophobic stationary phase: when an oxidized residue is located in the hydrophobic face of an amphipathic helix, the decrease in retention is profound. The same amino acid positioning leads to complete or partial resolution of pairs of peptides containing diastereomeric Mso residues. Contrary to all previously reported observations, and the nature of this modification, we also demonstrate for the first time that methionine oxidation may increase peptide hydrophobicity. This behavior is characteristic for Met residues in the N3 position of an N-capping box stabilization motif prior to the amphipathic helix. All these findings indicate that the prediction of peptide secondary structures upon interaction with hydrophobic surfaces must become an integral part of peptide retention modeling in proteomic applications going forward. PMID:26025879

  16. Indications and limitations of splints and casts.

    PubMed

    Mulon, Pierre-Yves; Desrochers, André

    2014-03-01

    Long bone fractures are relatively common in cattle, whether they result from a self-inflicted trauma or from external actors (herd mate or farm machinery). Various advanced orthopedic techniques have been described to stabilize and treat fractures in cattle with success. Unfortunately the use of most of those techniques remains unrealistic in a field setting, rendering the realization of splints and casts still accurate for the treatment of long bone fracture in cattle. This article refers to the use of all external coaptation and their specific indications as well as their limitations. PMID:24534659

  17. Viscosupplementation: techniques, indications, results.

    PubMed

    Legré-Boyer, V

    2015-02-01

    Viscosupplementation by hyaluronic acid (HA) injections is frequently used for local treatment of osteoarthritis (OA), due to ease of use and good tolerance. A profusion of linear or reticulated HA derivates are marketed, with varied characters and levels of evidence. Viscosupplementation has demonstrated moderate but significant efficacy (20%) versus placebo in terms of pain and function, with a high rate of responders (60-70%) in knee osteoarthritis. It allows reduced administration of opioid analgesics and NSAIDs, with improved risk/benefit ratio, and may delay joint replacement. Cartilage protection remains to be proven. Clinical efficacy shows 1-4 weeks' later onset than corticosteroids, but is maintained for 6 or even 12 months. Systematic association of corticosteroid and HA injection is not justified, and an interval has to be left before undertaking arthroplasty. Intra-articular injection of HA requires a skilled specialist, and may be difficult in a non-swollen joint; some tips and tricks may be helpful. In other joints than the knee, radiologic or ultrasound guidance is recommended. The efficacy of viscosupplementation is a matter of ongoing debate, after discordant findings in some meta-analyses. Some poor results may be due to inappropriate use of HA injections, poorly adapted to the patient's OA phenotype. Viscosupplementation is a treatment for chronic moderate symptomatic OA, and not for flares with joint swelling. Application in sport-related chondropathy has yet to be properly assessed. The optimal response profile remains to be determined. The ideal indication in the knee seems to be moderate femorotibial OA without swelling. Results have been generally disappointing in hip osteoarthritis but promising in OA of the ankle and shoulder (with and without rotator cuff tear). Further studies are needed to determine response profile and optimal treatment schedule, according to the joint. PMID:25596987

  18. Selection indices to identify drought-tolerant grain sorghum cultivars.

    PubMed

    Menezes, C B; Ticona-Benavente, C A; Tardin, F D; Cardoso, M J; Bastos, E A; Nogueira, D W; Portugal, A F; Santos, C V; Schaffert, R E

    2014-01-01

    Twenty-five cultivars of grain sorghum [Sorghum bicolor (L.) Moench] were examined under both drought stress and normal conditions in 4 experiments. In each condition, genotypes were evaluated in a factorial experiment using a randomized complete block design with 3 replications. Eight drought tolerance indices including stability tolerance index, mean productivity (MP), geometric MP, harmonic mean, stress susceptibility index, tolerance index, yield index, and yield stability index were estimated for each genotype based on grain yield under drought (Ys) and irrigated conditions (Yp). The results indicated that there were positive and significant correlations among Yp and Ys with geometric MP, MP, harmonic mean, and stability tolerance index, indicating that these factors are better predictors of Yp and Ys than tolerance index, stress susceptibility index, yield stability index, and yield index. Based on adjusted means at Yp and Ys, indices geometric MP, MP, harmonic mean, and stability tolerance index, unweighted pair group method with arithmetic mean cluster and biplot analysis, the most tolerant cultivars were '9929020', '9929034', and 'N 95B'. PMID:25501191

  19. Relationship Stability through Lenses of Complexity.

    PubMed

    Karakurt, Gunnur

    2012-03-01

    Research on relationship stability usually considers the effect of couple outcomes and individual differences on relationship stability in isolation from each other. These separate bodies of research often lead to inconsistent results. In order to better understand relationship stability and explain inconsistencies in the literature, it is important to investigate more complex models that integrate couple outcomes and behaviors with individual differences. Motivated by these considerations, we examined the complex interplay between personal characteristics, couple interactions, and relationship stability. In particular, we investigated the relationships among investment model, big five personality traits, attachment dimensions, relationship factors and relationship stability. Participants of this study included 162 individuals (Female N=117) who are currently in a relationship from a large Midwestern university campus. Analyses were conducted using Structural Equation Modeling. Examination of the structural path parameters indicated that attachment had significant direct effect on personality, relationship factors, and relationship stability. Personality also had a significant direct effect on relationship stability. Finally personality had no direct effect on relationship factors and relationship factors had no direct effect on relationship stability. These results suggest that the effect of personality on relationship stability is direct, rather than being mediated by relationship factors. PMID:23124824

  20. Application of reversed-phase high-performance liquid chromatography to the separation of apolipoproteins A-IV, A-I and E from rat high-density lipoprotein.

    PubMed

    Meyer, B; Kecorius, E; Barter, P; Fidge, N; Tetaz, T

    1991-03-01

    Apolipoproteins A-IV, A-I and E from rat high-density lipoprotein (HDL) were successfully purified by reversed-phase high-performance liquid chromatography (RP-HPLC), using a method which we have previously developed for the separation of apolipoproteins A-IV, A-I and E from human lymph chylomicrons [T. Tetaz, E. Kecorius, B. Grego and N. Fidge, J. Chromatogr., 511 (1990) 147]. Since analytical-scale RP-HPLC indicated that the C apolipoproteins from rat HDL coeluted with both apo A-IV and apo A-I, delipidated rat HDL was first subjected to preparative-scale size-exclusion HPLC (HPSEC) on a Serva Si300 column, which effectively separated the C apolipoproteins from all but apolipoprotein E. Fractions from HPSEC which were enriched for apolipoproteins A-IV, A-I or E were directly applied to RP-HPLC on a TSK Phenyl-5PW column. This procedure yielded fractions containing apolipoproteins A-IV, A-I or E which were pure as assessed by N-terminal sequencing and silver staining of sodium dodecyl sulphate-polyacrylamide gels. PMID:1906476

  1. Should researchers use single indicators, best indicators, or multiple indicators in structural equation models?

    PubMed Central

    2012-01-01

    Background Structural equation modeling developed as a statistical melding of path analysis and factor analysis that obscured a fundamental tension between a factor preference for multiple indicators and path modeling’s openness to fewer indicators. Discussion Multiple indicators hamper theory by unnecessarily restricting the number of modeled latents. Using the few best indicators – possibly even the single best indicator of each latent – encourages development of theoretically sophisticated models. Additional latent variables permit stronger statistical control of potential confounders, and encourage detailed investigation of mediating causal mechanisms. Summary We recommend the use of the few best indicators. One or two indicators are often sufficient, but three indicators may occasionally be helpful. More than three indicators are rarely warranted because additional redundant indicators provide less research benefit than single indicators of additional latent variables. Scales created from multiple indicators can introduce additional problems, and are prone to being less desirable than either single or multiple indicators. PMID:23088287

  2. Illustrating Chemiluminescence with Siloxene Indicator.

    ERIC Educational Resources Information Center

    Hoff, Ray

    1981-01-01

    Discusses the nature of light-producing reactions and provides a procedure for demonstrating chemical luminescence using siloxene indicator. Indicates source of this chemical and safety precautions. (SK)

  3. GMM Repeat Sales Price Indices

    Microsoft Academic Search

    Liang Peng

    2002-01-01

    Illiquid assets are widely spread within the economy but their indices are difficult to measure. This paper proposes a Generalized Method of Moment (GMM) repeat sales regression for estimating illiquid asset price indices. This method has estimators that are arithmetic averages of individual asset returns. This method is able to estimate custom-weighted indices, including equal- and value-weighted indices. It can

  4. Station stability measurement

    NASA Technical Reports Server (NTRS)

    Sosa, E. N.

    1981-01-01

    Methods and instrumentation are being developed to determine the frequency stability of Deep Space Stations. The efforts are presently focused on the verification of the stability of the X-band uplink and other RF and microwave subsystems which contribute to the overall stability of the system. The measurement methodology is presented as well as frequency stability data generated with the development measurement system. The system characteristics are highlighted and the potential areas where improvements could be made are discussed.

  5. Food Fortification Stability Study

    NASA Technical Reports Server (NTRS)

    Abdulmalik, T. O.; Cooper, M. R.; Douglas, G. L.

    2015-01-01

    NASA has established the goal of traveling beyond low-Earth orbit and extending manned exploration to Mars. The extended length of a Mars mission, along with the lack of resupply missions increases the importance of nutritional content in the food system. The purpose of this research is to assess the stability of vitamin supplementation in traditionally processed spaceflight foods. It is expected that commercially available fortificants will remain stable through long-duration missions if proper formulation, processing, and storage temperatures are all achieved. Five vitamins (vitamin E, vitamin K, pantothenic acid, folic acid, and thiamin) were blended into a vitamin premix (DSM, Freeport, TX); premixes were formulated to be compatible with current processing techniques (retort or freeze-dried), varied water activities (high or low), and packaging material. The overall goal of this process is to provide 25% of the recommended daily intake of each vitamin (per serving), following processing and two years of ambient storage. Four freeze-dried foods (Scrambled Eggs, Italian Vegetables, Potatoes Au Gratin, Noodles and Chicken) and four thermostabilized foods (Curry Sauce with Vegetables, Chicken Noodle Soup, Grilled Pork Chop, Rice with Butter) were produced (with and without the vitamin premix), to assess the impact of the added fortificant on color and taste, and to determine the stability of supplemental vitamins in spaceflight foods. The use of fortification in spaceflight foods appears to be a plausible mitigation step to inadequate nutrition. This is due to the ease of vitamin addition as well as the sustainability of the premixes through initial processing steps. Postprocessing analysis indicated that vitamin fortification with this premix did not immediately impact organoleptic properties of the food. At this stage, the largest hurdle to fortification is the preciseness to which vitamins can be added; the total amount of vitamins required for production is 10 - 20 grams, a minor percentage of the formulation. As demonstrated by the over-fortification measured in Italian Vegetables and Grilled Pork Chop, homogeneity may be difficult to achieve with such small amounts. Thus, pouch-to-pouch variability, over-fortification, and underfortification may ensue if a method for precise addition is not identified. Stability will continue to be evaluated over two years of storage at three temperatures, and future analysis should reveal the extent to which this issue should be a concern

  6. Frontogenetical Circulations and Stability

    NSDL National Science Digital Library

    COMET

    2007-10-24

    “Frontogenetical Circulations and Stability” is a Webcast by Dr. James T. Moore that focuses on an overview of different stability types, including convective, potential, inertial, conditional and symmetric, the concept of frontogenesis and associated circulations. The webcast concludes with a discussion of the role of stability in determining the character of frontogenetical circulations.

  7. Longitudinal Stability Calculations

    SciTech Connect

    Blaskiewicz,M.

    2009-01-02

    Coupled bunch longitudinal stability in the presence of high frequency impedances is considered. A frequency domain technique is developed and compared with simulations. The frequency domain technique allows for absolute stability tests and is applied to the problem of longitudinal stability in RHIC with the new 56 MHz RF system.

  8. Automatic Stability of Airplanes

    NASA Technical Reports Server (NTRS)

    Haus, FR

    1932-01-01

    It is endeavored in this report to give a full outline of the problem of airplane stability and to classify the proposed solutions systematically. Longitudinal stability, which can be studied separately, is considered first. The combination of lateral and directional stabilities, which cannot be separated, will be dealt with later.

  9. Statistical Indicators for Religious Studies: Indicators of Level and Structure

    ERIC Educational Resources Information Center

    Herteliu, Claudiu; Isaic-Maniu, Alexandru

    2009-01-01

    Using statistic indicators as vectors of information relative to the operational status of a phenomenon, including a religious one, is unanimously accepted. By introducing a system of statistic indicators we can also analyze the interfacing areas of a phenomenon. In this context, we have elaborated a system of statistic indicators specific to the…

  10. CONFIDENTIAL INDICATOR/NO PRINT INDICATOR Georgia Institute of Technology

    E-print Network

    Weber, Rodney

    CONFIDENTIAL INDICATOR/NO PRINT INDICATOR Georgia Institute of Technology Registrar's Office, Atlanta GA 30332-0315 Fax 404-894-0167 "CONFIDENTIAL" INDICATOR ­ (Option A) Checking the "Confidential records are "confidential" each time your record is viewed. Your name and associated information

  11. Synthetic fibers as an indicator of land application of sludge

    Microsoft Academic Search

    Kimberly Ann V. Zubris; Brian K. Richards

    2005-01-01

    Synthetic fabric fibers have been proposed as indicators of past spreading of wastewater sludge. Synthetic fiber detectability was examined in sludges (dewatered, pelletized, composted, alkaline-stabilized) and in soils from experimental columns and field sites applied with those sludge products. Fibers (isolated by water extraction and examined using polarized light microscopy) were detectable in sludge products and in soil columns over

  12. RANGELAND HEALTH ATTRIBUTES AND INDICATORS FOR QUALITATIVE ASSESSMENT

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Panels of experts from the Society for Range Management and the National Research Council proposed that status of rangeland ecosystems could be ascertained by evaluating an ecological site¿s potential to conserve soil resources and by a series of indicators for ecosystem processes and site stability...

  13. Gas turbine combustor stabilization by heat recirculation

    NASA Technical Reports Server (NTRS)

    Ganji, A.; Short, J.; Branch, M. C.; Oppenheim, A. K.

    1975-01-01

    The feasibility of heat recirculation for stabilization of lean mixtures and emission reduction has been studied in detail for a typical aircraft gas turbine combustor. Thermodynamic calculations have indicated temperature and heat recirculation rates for operation of the combustor over a range of combustion zone equivalence ratios and for varying modes of desired engine operation. Calculations indicate the feasibility of stabilizing the combustion zone at equivalence ratios as low as 0.2 with achievable heat recirculation rates. Detailed chemical kinetic calculations suggest that combustor heat release is maintained with reaction completion substantially before the NO forming reactions, even though CO is rapidly oxidized in this same region.

  14. Parafermion stabilizer codes

    E-print Network

    Utkan Güngördü; Rabindra Nepal; Alexey A. Kovalev

    2014-10-29

    We define and study parafermion stabilizer codes which can be viewed as generalizations of Kitaev's one dimensional model of unpaired Majorana fermions. Parafermion stabilizer codes can protect against low-weight errors acting on a small subset of parafermion modes in analogy to qudit stabilizer codes. Examples of several smallest parafermion stabilizer codes are given. A locality preserving embedding of qudit operators into parafermion operators is established which allows one to map known qudit stabilizer codes to parafermion codes. We also present a local 2D parafermion construction that combines topological protection of Kitaev's toric code with additional protection relying on parity conservation.

  15. Study on degradation kinetics of 2-(2-hydroxypropanamido) benzoic acid in aqueous solutions and identification of its major degradation product by UHPLC/TOF-MS/MS.

    PubMed

    Zhang, Qili; Guan, Jiao; Rong, Rong; Zhao, Yunli; Yu, Zhiguo

    2015-08-10

    A RP-HPLC method was developed and validated for the degradation kinetic study of 2-(2-hydroxypropanamido) benzoic acid (HPABA), a promising anti-inflammatory drug, which would provide a basis for further studies on HPABA. The effects of pH, temperature, buffer concentration and ionic strength on the degradation kinetics of HPABA were discussed. Experimental parameters such as degradation rate constants (k), activation energy (Ea), acid and alkali catalytic constants (kac, kal), shelf life (t1/2) and temperature coefficient (Q10) were calculated. The results indicated that degradation kinetics of HPABA followed zero-order reaction kinetics; degradation rate constants (k) of HPABA at different pH values demonstrated that HPABA was more stable in neutral and near-neutral conditions; the function of temperature on k obeyed the Arrhenius equation (r=0.9933) and HPABA was more stable at lower temperature; with the increase of ionic strength and buffer concentration, the stability of HPABA was decreased. The major unknown degradation product of HPABA was identified by UHPLC/TOF-MS/MS with positive electrospray ionization. Results demonstrated that the hydrolysis product was the primary degradation product of HPABA and it was deduced as anthranilic acid. PMID:25935790

  16. Methionine oxidation accelerates the aggregation and enhances the neurotoxicity of the D178N variant of the human prion protein.

    PubMed

    Feng, Boya; Wang, Zonglin; Liu, Ting; Jin, Rui; Wang, Shaobo; Wang, Wei; Xiao, Gengfu; Zhou, Zheng

    2014-12-01

    The D178N mutation of the prion protein (PrP) results in the hereditary prion disease fatal familial insomnia (FFI). Little is known regarding the effects of methionine oxidation on the pathogenesis of D178N-associated FFI. In the present study, we found that the D178N variant was more susceptible to oxidation than wild-type PrP, as indicated by reverse-phase high performance liquid chromatography (RP-HPLC) and mass spectrometry (MS) analysis. Circular dichroism (CD), differential scanning calorimetry (DSC), thioflavin T (ThT) binding assay studies demonstrated that methionine oxidation decreased the structural stability of the D178N variant, and the oxidized D178N variant exhibited a greater propensity to form ?-sheet-rich oligomers and aggregates. Moreover, these aggregates of oxidized D178N PrP were more resistant to proteinase K (PK) digestion. Additionally, using fluorescence confocal microscopy, we detected a high degree of aggregation in D178N-transfected Neuro-2a (N2a) cells after treatment with hydrogen peroxide (H2O2). Furthermore, the oxidation and consequent aggregation of the D178N variant induced greater apoptosis of N2a cells, as monitored using flow cytometry. Collectively, these observations suggest that methionine oxidation accelerates the aggregation and enhances the neurotoxicity of the D178N variant, possibly providing direct evidence to link the pathogenesis of D178N-associated FFI with methionine oxidation. PMID:25281825

  17. Purification and characterisation of plantaricin ZJ008, a novel bacteriocin against Staphylococcus spp. from Lactobacillus plantarum ZJ008.

    PubMed

    Zhu, Xuan; Zhao, Yizhen; Sun, Yalian; Gu, Qing

    2014-12-15

    A novel bacteriocin, plantaricin ZJ008 produced by Lactobacillus plantarum ZJ008 isolated from fresh milk, was purified by XAD 2, cation exchange chromatograph, gel chromatograph, and RP-HPLC. Mass spectrometry based on MALDI-TOF indicated that the bacteriocin had a molecular of 1334.77 Da. Only five of twenty amino acids could be identified by Edman degradation. This bacteriocin was highly thermostable (121°C, 30 min) and exhibited narrow pH stability (pH 4.0-5.0). It was sensitive to ?-Chymotrypsin, trypsin, papain, and pepsin. However it still had 80% of activity after treatment by proteinase K. The action mode of this peptide functioned as bactericidal, but it did not lead to lysis of cells. This bacteriocin exhibited broad-spectrum antimicrobial activity against tested Gram-positive and Gram-negative bacteria, especially Staphylococcus spp. These results suggested that this bacteriocin appears potentially very useful to control and inhibit Staphylococcus spp. in the food industry. PMID:25038669

  18. Smart Indicators on Learning Interactions

    Microsoft Academic Search

    Christian Glahn; Marcus Specht; Rob Koper

    2007-01-01

    Indicators help actors to organise, orientate and navigate through complex environments by providing contextual information relevant for the performance of learning tasks. In this article we analyse the requirements, present a model and an initial prototype of a software system that uses smart indicators to support learners to be more engaged in the learning process. We argue that indicators need

  19. Hydrologic indices for nontidal wetlands

    USGS Publications Warehouse

    Lent, R.M.; Weiskel, P.K.; Lyford, F.P.; Armstrong, D.S.

    1997-01-01

    Two sets of hydrologic indices were developed to characterize the water-budget components of nontidal wetlands. The first set consisted of six water-budget indices for input and output variables, and the second set consisted of two hydrologic interaction indices derived from the water-budget indices. The indices then were applied to 19 wetlands with previously published water-budget data. Two trilinear diagrams for each wetland were constructed, one for the three input indices and another for the three output indices. These two trilinear diagrams then were combined with a central quadrangle to form a Piper-type diagram, with data points from the trilinear diagrams projected onto the quadrangle. The quadrangle then was divided into nine fields that summarized the water-budget information. Two quantitative "interaction indices" were calculated from two of the six water-budget indices (precipitation and evapotranspiration). They also were obtained graphically from the water-budget indices, which were first projected to the central quadrangle of a Piper-type diagram from the flanking trilinear plots. The first interaction index (l) defines the strength of interaction between a wetland and the surrounding ground- and surface-water system. The second interaction index (S) defines the nature of the interaction between the wetland and the surrounding ground- and surface-water system (source versus sink). Evaluation of these indices using published wetland water-budget data illustrates the usefulness of the technique.

  20. Biological Indicators of Watershed Health

    NSDL National Science Digital Library

    This recently launched site on biological indicators, from the Environmental Protection Agency, is a gem, offering basic yet critical information on the what, where, why, and how of biological indicators. Presented in straightforward language, the site sets out to educate viewers about the importance of biological indicators -- those organisms that, because of their sensitivity to changes in the environment, "can provide accurate information about the health of a specific river, stream, lake, wetland, or estuary." The site is organized into seven main sections: Why use Indicators?, Key Concepts, Learn About State Programs, Biocriteria Resources, Fish as Indicators, Invertebrates as Indicators, and Periphyton as Indicators. In each section, a series of brief statements (with accompanying color photographs) leads the viewer through the logic, techniques, and methods used to assess watershed health. A collection of links rounds out the site.

  1. Process for stabilization of coal liquid fractions

    DOEpatents

    Davies, Geoffrey (Boston, MA); El-Toukhy, Ahmed (Alexandria, EG)

    1987-01-01

    Coal liquid fractions to be used as fuels are stabilized against gum formation and viscosity increases during storage, permitting the fuel to be burned as is, without further expensive treatments to remove gums or gum-forming materials. Stabilization is accomplished by addition of cyclohexanol or other simple inexpensive secondary and tertiary alcohols, secondary and tertiary amines, and ketones to such coal liquids at levels of 5-25% by weight with respect to the coal liquid being treated. Cyclohexanol is a particularly effective and cost-efficient stabilizer. Other stabilizers are isopropanol, diphenylmethanol, tertiary butanol, dipropylamine, triethylamine, diphenylamine, ethylmethylketone, cyclohexanone, methylphenylketone, and benzophenone. Experimental data indicate that stabilization is achieved by breaking hydrogen bonds between phenols in the coal liquid, thereby preventing or retarding oxidative coupling. In addition, it has been found that coal liquid fractions stabilized according to the invention can be mixed with petroleum-derived liquid fuels to produce mixtures in which gum deposition is prevented or reduced relative to similar mixtures not containing stabilizer.

  2. Stability of holographic superconductors

    SciTech Connect

    Kanno, Sugumi [Centre for Particle Theory, Department of Mathematical Sciences, Durham University, Science Laboratories, South Road, Durham, DH1 3LE (United Kingdom); Soda, Jiro [Department of Physics, Kyoto University, Kyoto, 606-8501 (Japan)

    2010-10-15

    We study the dynamical stability of holographic superconductors. We first classify perturbations around black hole background solutions into vector and scalar sectors by means of a 2-dimensional rotational symmetry. We prove the stability of the vector sector by explicitly constructing the positive definite Hamiltonian. To reveal a mechanism for the stabilization of a superconducting phase, we construct a quadratic action for the scalar sector. From the action, we see the stability of black holes near a critical point is determined by the equation of motion for a charged scalar field. We show the effective mass of the charged scalar field in hairy black holes is always above the Breitenlohner-Freedman bound near the critical point due to the backreaction of a gauge field. It implies the stability of the superconducting phase. We also argue that the stability continues away from the critical point.

  3. Indicators for Transboundary River Management

    Microsoft Academic Search

    CAROLIN M. LORENZ; ALISON J. GILBERT; WIM P. COFINO

    2001-01-01

    The aim of this paper is to analyze the potential of indicators for integrated river basin management and to develop a set\\u000a of indicators for the management of transboundary river basins. An indicator, comprising a variable or some aggregation of\\u000a variables, describes a system or process such that it has significance beyond the face value of its components. Integrated\\u000a river

  4. Stability of Colloidal Quasicrystals

    E-print Network

    A. R. Denton; H. Lowen

    1998-03-06

    Freezing of charge-stabilized colloidal suspensions and relative stabilities of crystals and quasicrystals are studied using thermodynamic perturbation theory. Macroion interactions are modelled by effective pair potentials combining electrostatic repulsion with polymer-depletion or van der Waals attraction. Comparing free energies -- counterion terms included -- for elementary crystals and rational approximants to icosahedral quasicrystals, parameters are identified for which one-component quasicrystals are stabilized by a compromise between packing entropy and cohesive energy.

  5. Stabilizing Grout Compatibility Study

    SciTech Connect

    HARBOUR, JOHNR.

    2004-05-19

    This report provides data that will be used to formulate the stabilizing grout and includes experimental results for Tc-99 stabilization by two reagents, (1) ground granulated blast furnace slag (GGBFS) and (2) surface treated hydroxyapatite (HA). One or both of these reagents are being considered by CH2M HILL for incorporation in the binder portion (matrix portion without sand) of the stabilizing grout. The technical basis for identifying the grout ingredient(s) for stabilizing technetium (Tc-99) will be provided by researchers at the Savannah River Technology Center (SRTC) in a subsequent report.

  6. Determination of stabilizer states

    E-print Network

    Xia Wu; Ying-hui Yang; Yu-kun Wang; Qiao-yan Wen; Su-juan Qin; Fei Gao

    2015-03-18

    The determination of many special types of quantum states has been studied thoroughly, such as the generalized |GHZ> states, |W> states equivalent under stochastic local operations and classical communication and Dicke states. In this paper, we are going to study another special entanglement states which is stabilizer states. The stabilizer states and their subset graph states play an important role in quantum error correcting codes, multipartite purification and so on. We show that all n- qubit stabilizer states are uniquely determined (among arbitrary states, pure or mixed) by their reduced density matrices for systems which are the supports of n independent generators of the corresponding stabilizer formalisms.

  7. Some Stability Measures for Software Maintenance

    Microsoft Academic Search

    Stephen S. Yau; James S. Collofello

    1980-01-01

    Software maintenance is the dominant factor contributing to the high cost of software. In this paper, the software maintenance process and the important software quality attributes that affect the maintenance effort are discussed. One of the most important quality attributes of software maintainability is the stability of a program, which indicates the resistance to the potential ripple effect that the

  8. Methods for obtaining desired helicopter stability characteristics

    NASA Technical Reports Server (NTRS)

    Gustafson, F B; Tapscott, Robert J

    1954-01-01

    A brief summary is made of methods available to the helicopter designer for obtaining desired stability characteristics by modifications to the airframe design. The discussion is based on modifications made during the establishment of flying-qualities criteria and includes sample indications of theoretical studies of additional methods.

  9. Agent Based Power System Transient Stability Enhancement

    E-print Network

    Pota, Himanshu Roy

    . Hossain and H. R. Pota Abstract--This paper describes an intelligent agent approach to power system fault, various tie lines, large number of electrical devices, etc. So the recent researches indicate a more-agent technology. Index Terms--Multi-agent system, electric power system, fault diagnosis, transient stability

  10. Voltage stability in distribution networks with DG

    Microsoft Academic Search

    M. Alonso; H. Amaris

    2009-01-01

    This paper presents a methodology for optimal placement of DG units in power networks to guarantee the voltage profile, maximize loadability conditions in normal and in contingencies situations. The methodology aims in finding the configuration, among a set of system components, which meets the desired system reliability requirements taking into account stability limits. Results shown in the paper indicate that

  11. Predicting Premarital Relationship Stability: A Methodological Refinement.

    ERIC Educational Resources Information Center

    Lloyd, Sally A.; And Others

    1984-01-01

    Attempted to predict relationship satisfaction in students (N=131) while controlling for the length of the relationship through an initial data collection and two subsequent follow-ups. Results indicated that involvement, reward level, and chance of marriage were all significant predictors of stability both at the three-month and the seven-month…

  12. Thermal stability of sulfonated polymers

    SciTech Connect

    Audibert, A.; Argillier, J.F. [Inst. Francais du Petrole, Rueil-Malmaison (France)

    1995-11-01

    Polyacrylamides which are used in oil applications i.e. polymer flooding and water based muds, are hydrolyzed versus time and temperature. This leads to a lack of tolerance towards electrolyte contamination and to a rapid degradation inducing a loss of their properties. Modifications of polyacrylamide structure have been proposed to postpone their thermal stability to higher temperatures. Monomers such as acrylamido methylpropane sulfonate (AMPS) or sulfonated styrene/maleic anhydride can be used to prevent acrylamide comonomer from hydrolysis. The aim of this work is to study under controlled conditions, i.e. anaerobic atmosphere, neutral pH, the stability of sulfonated polymers in order to distinguish between hydrolysis and radical degradation reactions. It has been observed that up to 100 C, the AMPS group is stable and protects the acrylamide function from hydrolysis up to 80%. At higher temperature, even the hydrolysis of the AMPS group occurs, giving acrylate and {beta},{beta} dimethyl taurine, with a kinetics that depends on temperature and time. Degradation in terms of molecular weight then occurs indicating that it follows a radical decarboxylation reaction. It can be limited either by the use of free radical scavenger or when the polymer is in the presence of a mineral phase such as bentonite. These results provide valuable data for the determination of the limits of use of sulfonated copolymers and guidelines for optimizing chemical structure of sulfonated polymers used in water based formulation, in particular to enhance their thermal stability.

  13. Dimensional stability of natural fibers

    SciTech Connect

    Driscoll, Mark S. [Ultraviolet Light/Electron Beam (UV/EB) Technology Center, State University of New York College of Environmental Science and Forestry (SUNY-ESF), 1 Forestry Drive, Syracuse, NY 13210 (United States); Smith, Jennifer L.; Woods, Sean; Tiss, Kenneth J. [Ultraviolet Light/Electron Beam (UV/EB) Technology Center, State University of New York College of Environmental Science and Forestry (SUNY-ESF), 1 Forestry Drive, Syracuse, NY 13210 and Sustainable Construction Management and Engineering, SUNY-ESF (United States); Larsen, L. Scott [New York State Energy Research and Development Authority (NYSERDA), 17 Columbia Circle, Albany, NY 12203 (United States)

    2013-04-19

    One of the main problems associated with the use of natural fibers as reinforcing agents in composites is their uptake of moisture. Many natural fibers are lignocellulosic, which causes them to swell and shrink as the amount of available moisture changes. Swelling and shrinking can cause composites to prematurely fail. This paper presents the results of a preliminary study that considers the use of two different low molecular weight monomers, hydroxyethyl methacrylate (HEMA) and hydroxyethyl acrylate (HEA), polymerized by electron beam ionizing radiation, to dimensionally stabilize natural fibers. Eight different treatments consisting of varying amounts of monomer, encapsulating agent, and cross-linkers, were evaluated for their ability to dimensionally stabilize sisal fiber. Results indicate that both polymerized HEA and HEMA can reduce the swelling of sisal fiber. The effectiveness of HEA and HEMA can be further enhanced with the use of a cross-linker (SR 454). The use of hydroxylated monomers to dimensionally stabilize natural fibers may play an important role in reducing delamination and improving fiber-resin adhesion in composites.

  14. Validation of the Goal Attainment Scale of Stabilization

    ERIC Educational Resources Information Center

    Balkin, Richard S.

    2013-01-01

    Factor structure for the Goal Attainment Scale of Stabilization was evaluated using separate samples for exploratory factor analysis and confirmatory factor analysis. Results indicated a 25-item two-factor solution. The Goal Attainment Scale of Stabilization may be useful in identifying the extent to which adolescents in crisis meet therapeutic…

  15. Chemochromic Indicators for the Detection of Hypergolic Fuels

    NASA Technical Reports Server (NTRS)

    Santiago-Maldonado, E.; Captian, J.; Devor, R.

    2010-01-01

    The toxicity and hazard level associated with the use of hypergolic fuels necessitates the development of technology capable of detecting the presence of such fuels in a variety of different environments and conditions. The most commonly used sensors for the detection of hypergolic fuels are electrochemical in nature, which have serious limitations when used as area monitoring devices. Recent collaborative work between Kennedy Space Center and ASRC Aerospace has led to the development of indicators which exhibit a color change upon exposure to hydrazine under different conditions. The indicators under investigation on this developmental effort are para-dimethylaminobenzaldehyde (PDAB), various formulations of universal pH indicators, and potassium tetrachloroaurate (KAuCl4). These chemochromic indicators have been tested for the detection of hydrazine under various conditions: pure liquid fuel, aqueous fuel solution, saline aqueous fuel solutions, vapor fuel, and 3-month shelf life study, which included UV protection, thermal extremes, and normal storage conditions. The hypergolic fuel indicator test was conducted with the indicator impregnated into a wipe material to test the applicability of the indicator to be used to capture (absorb) and indicate the presence of hypergolic fuels. Each of the indicators performed well, with the universal pH indicator being the best candidate because of the visible response color change and the indicator stability after the shelf life study.

  16. Quality Indicators for Learning Analytics

    ERIC Educational Resources Information Center

    Scheffel, Maren; Drachsler, Hendrik; Stoyanov, Slavi; Specht, Marcus

    2014-01-01

    This article proposes a framework of quality indicators for learning analytics that aims to standardise the evaluation of learning analytics tools and to provide a mean to capture evidence for the impact of learning analytics on educational practices in a standardised manner. The criteria of the framework and its quality indicators are based on…

  17. Quality Indicators of Online Programs

    Microsoft Academic Search

    Leo Hirner; Thomas Kochtanek

    2012-01-01

    The continued growth of online programs in higher education has resulted in concerns about how institutions monitor the quality of their online programs. These concerns indicate a need for a process by which online programs may be evaluated and compared. They provided the impetus for this study, the goals of which were to identify quality indicators specific to community college

  18. Fit Indices Versus Test Statistics

    ERIC Educational Resources Information Center

    Yuan, Ke-Hai

    2005-01-01

    Model evaluation is one of the most important aspects of structural equation modeling (SEM). Many model fit indices have been developed. It is not an exaggeration to say that nearly every publication using the SEM methodology has reported at least one fit index. Most fit indices are defined through test statistics. Studies and interpretation of…

  19. Indicator Variables for Optimal Policy

    Microsoft Academic Search

    Lars E. O. Svensson; Michael Woodford

    1999-01-01

    The optimal weights on indicators in models with partial information about the state of the economy and forward-looking variables are derived and interpreted, both for equilibria under discretion and under commitment. An example of optimal monetary policy with a partially observable potential output and a forward-looking indicator is examined. The optimal response to the optimal estimate of potential output displays

  20. Deriving indicators of sustainable development

    Microsoft Academic Search

    Hartmut Bossel

    1996-01-01

    Assessments of current and future development paths require comprehensive sets of indicators covering all essential aspects. From a holistic systems point of view, most currently proposed indicator sets are incomplete and deficient. Assessments of sustainable development require a full representation of the satisfaction states of the “basic orientors” (=fundamental interests) of constituent sector systems, and of their contribution to basic

  1. Some Indices of Lake Productivity

    Microsoft Academic Search

    John B. Moyle

    1949-01-01

    In an attempt to evaluate lake-survey procedures some of the chemical, physical, and biological measurements that have been considered possible indices of lake productivity have been examined in the light of 11 years of lake surveys and 6 years of pond rearing of yellow pikeperch. In Minnesota waters total alkalinity and total phosphorus appear to be the most valuable indices.

  2. Stability of the pumpkin balloon

    NASA Astrophysics Data System (ADS)

    Baginski, Frank

    A large axisymmetric balloon with positive differential pressure, e.g., a sphere, leads to high film stresses. These can be significantly reduced by using a lobed pumpkin-like shape re-enforced with tendons. A number of schemes have been proposed to achieve a cyclically symmetric pumpkin-shape at full inflation, including the constant bulge angle (CBA) design and the constant bulge radius (CBR) design. The authors and others have carried out stability studies of CBA and CBR designs and found instabilities under various conditions. While stability seems to be a good indicator of deployment problems for large balloons under normal ascent conditions, one cannot conclude that a stable design will deploy reliably. Nevertheless, stability analysis allows one to quantify certain deployment characteristics. Ongoing research by NASA's Balloon Program Office utilizes a new design approach developed by Rodger Farley, NASA/GSFC, that takes into account film and tendon strain. We refer to such a balloon as a constant stress (CS) pumpkin design. In June 2006, the Flight 555-NT balloon (based on a hybrid CBR/CBA design) developed an S-cleft and did not deploy. In order to understand the S-cleft phenomena and study a number of aspects related to the CS-design, a series of inflation tests were conducted at TCOM, Elizabeth City, NC in 2007. The test vehicles were 27 meter diameter pumpkins distinguished by their respective equatorial bulge angles (BA). For example, BA98 indicates an equatorial bulge angle of 98° . BA90, BA55, and BA00 are similarly defined. BA98 was essentially a one-third scale version of of the Flight 555 balloon (i.e., 12 micron film instead of 38.1 micron, mini-tendons, etc.). BA90 and BA55 were Farley CS-designs. BA00 was derived from the BA55 design so that a flat chord spanned adjacent tendons. In this paper, we will carry out stability studies of BA98, BA90, BA55, and BA00. We discuss the deployment problem of pumpkin balloons in light of 2007 inflation test results and flight data. In previous stability work, we added constant uniform perturbations to the design in our sensitivity studies. Here, we consider non-uniform perturbation as well. For example, a tendon may have a certain average slack strain s when measured over its entire length. However, there will be local variations ˆ about s. We explore such sensitivities via case studies. ˆ

  3. VizieR Online Data Catalog: Refractive indices of grain materials (Cuzzi+, 2014)

    NASA Astrophysics Data System (ADS)

    Cuzzi, J. N.; Estrada, P. R.; Davis, S. S.

    2014-04-01

    For ease of comparison with previously published results, we adopt refractive indices, material abundances, and stability regimes for the condensible constituents as published by Pollack et al. (1994ApJ...421..615P). (1 data file).

  4. Charts for checking the stability of plane systems of rods

    NASA Technical Reports Server (NTRS)

    Borkmann, K

    1937-01-01

    Charts are presented for checking the stability of plane systems of rods, the use of the charts being illustrated by examples. It is also indicated how best to combine the individual members to form stable structures.

  5. Stabilized radio frequency quadrupole

    DOEpatents

    Lancaster, Henry D. (Orinda, CA); Fugitt, Jock A. (Berkeley, CA); Howard, Donald R. (Danville, CA)

    1984-01-01

    A long-vane stabilized radio frequency resonator for accelerating charged particles and including means defining a radio frequency resonator cavity, a plurality of long vanes mounted in the defining means for dividing the cavity into sections, and means interconnecting opposing ones of the plurality of vanes for stabilizing the resonator.

  6. Stability of Coupling Algorithms

    E-print Network

    Akkasale, Abhineeth

    2012-07-16

    INTRODUCTION AND MOTIVATION : : : : : : : : : : : : : 1 A. Approaches to solving a coupled system . . . . . . . . . . . 3 B. Common terminology . . . . . . . . . . . . . . . . . . . . . 5 C. Classi cation of coupling algorithms . . . . . . . . . . . . . 7 1.... Stability criterion . . . . . . . . . . . . . . . . . . . . . . . 14 III REPRESENTATIVE NUMERICAL EXAMPLES : : : : : : : : 16 A. Split SDOF: rst order system . . . . . . . . . . . . . . . . 16 1. CSS implementation and stability of a rst order system 18...

  7. Stabilization of Kepler's problem

    NASA Technical Reports Server (NTRS)

    Stokes, A.

    1977-01-01

    A regularization of Kepler's problem due to Moser (1970) is used to stabilize the equations of motion. In other words, a particular solution of Kepler's problem is imbedded in a Liapunov stable system. Perturbations can be introduced into the stabilized equations.

  8. Head stabilization in herons

    Microsoft Academic Search

    G. Katzir; E. Schechtman; N. Carmi; D. Weihs

    2001-01-01

    We examined head stabilization in relation to body mass and length of legs in four heron species (little egrets, Egretta garzetta; night herons, Nycticorax nycticorax; squacco herons, Ardeola ralloides; and cattle egrets, Bubulcus ibis: Aves: Ardeidae). Head stabilization, under controlled, sinusoidal, perch perturbations was mostly elicited at frequencies lower than 1 Hz. Maximal perturbation amplitudes sustained were positively correlated with

  9. Forces Stabilizing Proteins

    PubMed Central

    Pace, C. Nick; Scholtz, J. Martin; Grimsley, Gerald R.

    2014-01-01

    The goal of this article is to summarize what has been learned about the major forces stabilizing proteins since the late 1980s when site-directed mutagenesis became possible. The following conclusions are derived from experimental studies of hydrophobic and hydrogen bonding variants. 1. Based on studies of 138 hydrophobic interaction variants in 11 proteins, burying a –CH2– group on folding contributes 1.1 ± 0.5 kcal/mol to protein stability. 2. The burial of nonpolar side chains contributes to protein stability in two ways: first, a term that depends on the removal of the side chains from water and, more importantly, the enhanced London dispersion forces that result from the tight packing in the protein interior. 3. Based on studies of 151 hydrogen bonding variants in 15 proteins, forming a hydrogen bond on folding contributes 1.1 ± 0.8 kcal/mol to protein stability. 4. The contribution of hydrogen bonds to protein stability is strongly context dependent. 5. Hydrogen bonds by side chains and peptide groups make similar contributions to protein stability. 6. Polar group burial can make a favorable contribution to protein stability even if the polar group is not hydrogen bonded. 7. Hydrophobic interactions and hydrogen bonds both make large contributions to protein stability. PMID:24846139

  10. SRED: Stabilized RED

    Microsoft Academic Search

    Teunis J. Ott; T. V. Lakshman; Larry H. Wong

    1999-01-01

    This paper describes a mechanism we call "SRED" (Stabilized Random Early Drop). Like RED (Random Early Detection) SRED pre-emptively discards packets with a load-dependent probability when a buffer in a router in the Internet or an Intranet seems congested. SRED has an additional feature that over a wide range of load levels helps it stabilize its buffer occupation at a

  11. Stabilized radio frequency quadrupole

    DOEpatents

    Lancaster, H.D.; Fugitt, J.A.; Howard, D.R.

    1984-12-25

    Disclosed is a long-vane stabilized radio frequency resonator for accelerating charged particles and including means defining a radio frequency resonator cavity, a plurality of long vanes mounted in the defining means for dividing the cavity into sections, and means interconnecting opposing ones of the plurality of vanes for stabilizing the resonator. 5 figs.

  12. Developing indicators for European birds

    PubMed Central

    Gregory, Richard D; van Strien, Arco; Vorisek, Petr; Gmelig Meyling, Adriaan W; Noble, David G; Foppen, Ruud P.B; Gibbons, David W

    2005-01-01

    The global pledge to deliver ‘a significant reduction in the current rate of biodiversity loss by 2010’ is echoed in a number of regional and national level targets. There is broad consensus, however, that in the absence of conservation action, biodiversity will continue to be lost at a rate unprecedented in the recent era. Remarkably, we lack a basic system to measure progress towards these targets and, in particular, we lack standard measures of biodiversity and procedures to construct and assess summary statistics. Here, we develop a simple classification of biodiversity indicators to assist their development and clarify purpose. We use European birds, as example taxa, to show how robust indicators can be constructed and how they can be interpreted. We have developed statistical methods to calculate supranational, multi-species indices using population data from national annual breeding bird surveys in Europe. Skilled volunteers using standardized field methods undertake data collection where methods and survey designs differ slightly across countries. Survey plots tend to be widely distributed at a national level, covering many bird species and habitats with reasonable representation. National species' indices are calculated using log-linear regression, which allows for plot turnover. Supranational species' indices are constructed by combining the national species' indices weighted by national population sizes of each species. Supranational, multi-species indicators are calculated by averaging the resulting indices. We show that common farmland birds in Europe have declined steeply over the last two decades, whereas woodland birds have not. Evidence elsewhere shows that the main driver of farmland bird declines is increased agricultural intensification. We argue that the farmland bird indicator is a useful surrogate for trends in other elements of biodiversity in this habitat. PMID:15814345

  13. Communication Indicators. I. Communication Indicators and Indicators of Socio-Economic Development. Communication and Society 3.

    ERIC Educational Resources Information Center

    O'Brien, Rita Cruise; And Others

    This report summarizes a Unesco-sponsored study of indicators of international communication and socioeconomic development. Following a brief description of the background, purpose, and methodology of the study, the report discusses its findings in the following areas: (1) communication and social indicators; (2) communications and the growth of…

  14. Refinement of microwave vegetation indices

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Previous investigations have established the basis for a new type of vegetation index based on passive microwave satellite observations. These microwave vegetation indices (MVIs) have been qualitatively evaluated by examining global spatial and seasonal temporal features. Limited quantitative studie...

  15. Global Climate Change Key Indicators

    NSDL National Science Digital Library

    This website charts measurement of key indicators of global climate change. Simple explanations and "What Does This Mean?" sections accompany each area of sea level, carbon dioxide concentration, global surface temperature, Arctic sea ice and land ice.

  16. Community Health Status Indicators Project

    E-print Network

    conditions for health in order to eliminate health disparities #12;Challenges · Acquire resources to addCommunity Health Status Indicators Project National Center for Environmental Health Environmental Health Tracking Branch Marilyn Metzler National Center for Chronic Disease Prevention and Health

  17. EVALUATION GUIDELINES FOR ECOLOGICAL INDICATORS

    EPA Science Inventory

    This document presents fifteen technical guidelines to evaluate the suitability of an ecological indicator for a particular monitoring program. The guidelines are organized within four evaluation phrases: conceptual relevance, feasibility of implementation, response variability...

  18. Environmental indices in irrigation management.

    PubMed

    Manoliadis, O G

    2001-10-01

    Irrigation management calls for objective criteria capable of representing the economy, reliability, and productivity of irrigation systems. These criteria must be compatible with long-term sustainability and conservation goals. The criteria representing the above goals are the economic effect of management on yield reduction, economic effect, and reliability referring to plant growth and operation of the network. In this study environmental indices are introduced to express the above criteria in quantitative terms. The inclusion of these indices at the farm and network level create a multicriteria framework for decision-making based on composite programming. An experimental study was conducted during the irrigation periods of 1989 and 1990 in Chania, Greece, concerning water delivered to 40 experimental plots, soil moisture content at the rootzone, and irrigation system operational failures. The data collected in real time were used for the calculation of the corresponding environmental indices. The variation in time and space is high and resulted in up to 62% of yield loss and low system performance (up to 7% of system temporal reliability). The study indicated that environmental indices could be incorporated to select alternatives and also to develop policies on water delivery. The final decision involves a trade-off analysis between cost of application and desired system performance. Measures of both primary objectives can be obtained using environmental indices that represent system operation aggregation at its basic levels (on farm and network). PMID:11494068

  19. Specificity versus stability in computational protein design

    PubMed Central

    Bolon, Daniel N.; Grant, Robert A.; Baker, Tania A.; Sauer, Robert T.

    2005-01-01

    Protein–protein interactions can be designed computationally by using positive strategies that maximize the stability of the desired structure and/or by negative strategies that seek to destabilize competing states. Here, we compare the efficacy of these methods in reengineering a protein homodimer into a heterodimer. The stability-design protein (positive design only) was experimentally more stable than the specificity-design heterodimer (positive and negative design). By contrast, only the specificity-design protein assembled as a homogenous heterodimer in solution, whereas the stability-design protein formed a mixture of homodimer and heterodimer species. The experimental stabilities of the engineered proteins correlated roughly with their calculated stabilities, and the crystal structure of the specificity-design heterodimer showed most of the predicted side-chain packing interactions and a main-chain conformation indistinguishable from the wild-type structure. These results indicate that the design simulations capture important features of both stability and structure and demonstrate that negative design can be critical for attaining specificity when competing states are close in structure space. PMID:16129838

  20. 46 CFR 28.530 - Stability instructions.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ...VESSELS REQUIREMENTS FOR COMMERCIAL FISHING INDUSTRY VESSELS Stability § 28.530 Stability...operating personnel in the commercial fishing industry have had specialized training in stability. Therefore, stability...

  1. 46 CFR 28.530 - Stability instructions.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ...VESSELS REQUIREMENTS FOR COMMERCIAL FISHING INDUSTRY VESSELS Stability § 28.530 Stability...operating personnel in the commercial fishing industry have had specialized training in stability. Therefore, stability...

  2. 46 CFR 28.530 - Stability instructions.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ...VESSELS REQUIREMENTS FOR COMMERCIAL FISHING INDUSTRY VESSELS Stability § 28.530 Stability...operating personnel in the commercial fishing industry have had specialized training in stability. Therefore, stability...

  3. 46 CFR 28.530 - Stability instructions.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ...VESSELS REQUIREMENTS FOR COMMERCIAL FISHING INDUSTRY VESSELS Stability § 28.530 Stability...operating personnel in the commercial fishing industry have had specialized training in stability. Therefore, stability...

  4. 46 CFR 28.530 - Stability instructions.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ...VESSELS REQUIREMENTS FOR COMMERCIAL FISHING INDUSTRY VESSELS Stability § 28.530 Stability...operating personnel in the commercial fishing industry have had specialized training in stability. Therefore, stability...

  5. Fluid sphere: Stability problem and dimensional constraint

    NASA Astrophysics Data System (ADS)

    Rahaman, Farook; Pradhan, Anirudh; Ahmed, Nasr; Ray, Saibal; Saha, Bijan; Rahaman, Mosiur

    2015-04-01

    We study different dimensional fluids inspired by noncommutative geometry which admit conformal Killing vector (CKV). The solutions of the Einstein field equations were examined specifically for five different set of spacetime. We calculate the active gravitational mass and impose stability conditions of the fluid sphere. The analysis thus carried out immediately indicates that at four dimension only one can get a stable configuration for any spherically symmetric stellar system and any other dimension, lower or higher, becomes untenable as far as the stability of a system is concerned.

  6. Fluid sphere: stability problem and dimensional constraint

    E-print Network

    Farook Rahaman; Anirudh Pradhan; Nasr Ahmed; Saibal Ray; Bijan Saha; Mosiur Rahaman

    2015-04-14

    We study different dimensional fluids inspired by noncommutative geometry which admit conformal Killing vectors. The solutions of the Einstein field equations examined specifically for five different set of spacetime. We calculate the active gravitational mass and impose stability conditions of the fluid sphere. The analysis thus carried out immediately indicates that at $4$-dimension only one can get a stable configuration for any spherically symmetric stellar system and any other dimensions, lower or higher, becomes untenable as far as the stability of a system is concerned.

  7. Surface controlled blade stabilizer

    DOEpatents

    Russell, Larry R. (6025 Edgemor, Suite C, Houston, TX 77081)

    1983-01-01

    Drill string stabilizer apparatus, controllable to expand and retract entirely from the surface by control of drill string pressure, wherein increase of drill string pressure from the surface closes a valve to create a piston means which is moved down by drill string pressure to expand the stabilizer blades, said valve being opened and the piston moving upward upon reduction of drill string pressure to retract the stabilizer blades. Upward and downward movements of the piston and an actuator sleeve therebelow are controlled by a barrel cam acting between the housing and the actuator sleeve.

  8. Leading indicators of trophic cascades.

    PubMed

    Carpenter, S R; Brock, W A; Cole, J J; Kitchell, J F; Pace, M L

    2008-02-01

    Regime shifts are large, long-lasting changes in ecosystems. They are often hard to predict but may have leading indicators which are detectable in advance. Potential leading indicators include wider swings in dynamics of key ecosystem variables, slower return rates after perturbation and shift of variance towards lower frequencies. We evaluated these indicators using a food web model calibrated to long-term whole-lake experiments. We investigated whether impending regime shifts driven by gradual increase in exploitation of the top predator can create signals that cascade through food webs and be discerned in phytoplankton. Substantial changes in standard deviations, return rates and spectra occurred near the switch point, even two trophic levels removed from the regime shift in fishes. Signals of regime shift can be detected well in advance, if the driver of the regime shift changes much more slowly than the dynamics of key ecosystem variables which can be sampled frequently enough to measure the indicators. However, the regime shift may occur long after the driver has passed the critical point, because of very slow transient dynamics near the critical point. Thus, the ecosystem can be poised for regime shift by the time the signal is discernible. Field tests are needed to evaluate these indicators. PMID:18021242

  9. Stabilization precision control methods of photoelectric aim-stabilized system

    NASA Astrophysics Data System (ADS)

    Song, Xiaoru; Chen, Hua; Xue, Yonggang

    2015-09-01

    To solve the question that photoelectric aim-stabilized system can be controlled with high precision and stability, this paper researches a new photoelectric aim-stabilized control algorithm, analyzes the photoelectric aim-stabilized system architecture, sets up stability control system mathematical model, designs the stability of the photoelectric aim-stabilized LSSVM identification and control system, discusses uncertain factors and calculates the LSSVM parameters by the Chaos theory, gives the predictive controller model by the LSSVM and designs new photoelectric aim-stabilized system. Through the simulation calculation and experimental analysis, new photoelectric aim-stabilized control algorithm was verified; the results show the new photoelectric aim-stabilized control method can meet the demand of high precision control in photoelectric aim-stabilized system.

  10. Oxygen respirometry to assess stability and maturity of composted municipal solid waste

    Microsoft Academic Search

    D. A. Iannotti; M. E. Grebus; B. L. Toth; L. V. Madden; A. J. Hoitink

    1994-01-01

    The stability and maturity of compost prepared from municipal solid waste (MSW) at a full-scale composting plant was assessed through chemical, physical, and biological assays. Respiration bioassays used to determine stability (Oâ and COâ respirometry) were sensitive to process control problems at the composting plant and indicated increasing stability with time. Radish (Raphanus sativus L.) and ryegrass (Lolium perenne L.)

  11. The Relationship between Anxiety-Stability, Working Memory and Cognitive Style

    ERIC Educational Resources Information Center

    Grimley, Michael; Dahraei, Hassan; Riding, Richard J.

    2008-01-01

    While prior research indicates that relationships exist between anxiety-stability and working memory, and cognitive style and anxiety-stability, they have not been considered together. The aim of this study was to consider how anxiety-stability is related to working memory, gender and style in interaction. The sample consisted of 179…

  12. Cold plasma stabilization of a mirror-confined, hot-electron plasma

    Microsoft Academic Search

    I. G. Brown; A. J. Lichtenberg; M. A. Lieberman; N. C. Wyeth

    1976-01-01

    The stabilization of a hot-electron plasma in a simple mirror geometry is investigated. Controlled quantities of neutral gas generate a cold plasma through hot-electron ionization. Increasing stability is found with increasing gas pressure. The pressure required for stabilization is found to be inversely proportional to the ionization cross section of the type of neutral gas, indicating that the number of

  13. Autographic Indicator for Tension Tests

    E-print Network

    Hood, George J.

    1902-01-01

    by Adolf Martens, two volumes* In the second class, the indicators, being fastened securely to the test piece9 show more accurate res Its. One of the best of this type is the Henning Pocket Indicator, described in A*S*M*E* Records Vol* XX, Page... into the threads of lead screw L* When one pen has traveled across the drum the next pen is fed into the lead screw by the feeders P^and sliding rod J . The lead serew L has 80 threads per inch and hence must make one revolution per 250 pounds increase...

  14. Development and validation of a chromatographic method for determining Clematichinenoside AR and related impurities

    PubMed Central

    2012-01-01

    Background Clematichinenoside AR is a promising lead compound for the treatment of rheumatoid arthritis. A systematic research for the related impurities in AR bulk samples is still lacking. For the safe use of this natural product in future clinical practice, the structure and content of each constituent, including the main ingredient as well as the impurities in AR bulk sample must be characterized in detail. Results A simple and stability indicating RP-HPLC method was developed and validated for determining the purity of clematichinenoside AR (AR), a natural product from the roots of Clematis manshurica Rupr. (Ranunculaceae) with the potential of treating rheumatoid arthritis. Five impurities were characterized, and impurity 2 (Clematomandshurica saponin F) is a new triterpenoid saponin isolated from this product. Optimum separation for clematichinenoside AR and five related impurities was carried out on an Agilent octadecylsilane bonded silica gel column (TC-C18, 4.6 mm ×150 mm, 5 ?m) using a gradient HPLC method. The validation results showed good sensitivity, specificity, linearity(r2>0.9992) precision(RSD<1.63%), accuracy(recoveries in the range of 95.60%-104.76%) and robustness. Three AR bulk samples containing all the impurities were examined by two methods, and the stability of correction factors for the determination of related impurities was discussed. The proposed stability-indicating method was suitable for the quality control of this natural product. Conclusion Five related impurities of clematichinenoside AR were characterized, including a new triterpenoid saponins firstly found in clematichinenoside AR bulk samples. In the simple chromatographic method for determining clematichinenoside AR and its related impurities in bulk samples, the correction factor was better for the quality control in the relative stable concentrations. PMID:23216920

  15. Frequency stability review

    NASA Technical Reports Server (NTRS)

    Greenhall, C. A.

    1987-01-01

    Certain aspects of the description and measurement of oscillator stability are treated. Topics covered are time and frequency deviations, Allan variance, the zero-crossing counter measurement technique, frequency drift removal, and the three-cornered hat.

  16. Stability of streamwise vortices

    NASA Astrophysics Data System (ADS)

    Khorrami, M. K.; Grosch, C. E.; Ash, R. L.

    1987-04-01

    A brief overview of some theoretical and computational studies of the stability of streamwise vortices is given. The local induction model and classical hydrodynamic vortex stability theories are discussed in some detail. The importance of the three-dimensionality of the mean velocity profile to the results of stability calculations is discussed briefly. The mean velocity profile is provided by employing the similarity solution of Donaldson and Sullivan. The global method of Bridges and Morris was chosen for the spatial stability calculations for the nonlinear eigenvalue problem. In order to test the numerical method, a second order accurate central difference scheme was used to obtain the coefficient matrices. It was shown that a second order finite difference method lacks the required accuracy for global eigenvalue calculations. Finally the problem was formulated using spectral methods and a truncated Chebyshev series.

  17. Achieving placement stability.

    PubMed

    Carnochan, Sarah; Moore, Megan; Austin, Michael J

    2013-01-01

    Placement stability as an outcome goal in child welfare performance measurement is grounded in the importance of providing stability for children as they are developing attachments and relationships to caregivers. Research shows that many children are vulnerable to placement instability, especially those who have been in long term foster care. This literature review provides an overview of the federal placement stability measure. It then summarizes the diverse set of factors has been found to be associated with placement instability, including characteristics of the child and family of origin, placement type and quality, and the child welfare system and services. Promising practices aimed at promoting placement stability are summarized, followed by questions designed to foster discussion about the relationship of the evidence to child welfare practice. PMID:23705653

  18. Stabilizer state breeding

    E-print Network

    Erik Hostens; Jeroen Dehaene; Bart De Moor

    2006-08-18

    We present a breeding protocol that distills pure copies of any stabilizer state from noisy copies and a pool of predistilled pure copies of the same state, by means of local Clifford operations, Pauli measurements and classical communication.

  19. Stabilizer state breeding

    SciTech Connect

    Hostens, Erik; Dehaene, Jeroen; Moor, Bart de [ESAT-SCD, K.U. Leuven, Kasteelpark Arenberg 10, B-3001 Leuven (Belgium)

    2006-12-15

    We present a breeding protocol that distills pure copies of any stabilizer state from noisy copies and a pool of predistilled pure copies of the same state, by means of local Clifford operations, Pauli measurements, and classical communication.

  20. Tetraphenylborate Solids Stability Tests

    SciTech Connect

    Walker, D.D. [Westinghouse Savannah River Company, AIKEN, SC (United States)

    1997-06-25

    Tetraphenylborate solids are a potentially large source of benzene in the slurries produced in the In-Tank Precipitation (ITP) process. The stability of the solids is an important consideration in the safety analysis of the process and we desire an understanding of the factors that influence the rate of conversion of the solids to benzene. This report discusses current testing of the stability of tetraphenylborate solids.

  1. Inhibition of Peptide Acylation in PLGA Microspheres with Water-soluble Divalent Cationic Salts

    Microsoft Academic Search

    Ying Zhang; Andreas M. Sophocleous; Steven P. Schwendeman

    2009-01-01

    Purpose  To test the potential of water-soluble divalent cationic salts to inhibit acylation of octreotide encapsulated in poly(D,L-lactic-co-glycolic\\u000a acid)-star (PLGA) microspheres.\\u000a \\u000a \\u000a \\u000a Methods  The divalent cationic salts, calcium chloride and manganese chloride, previously shown to disrupt peptide sorption, were introduced\\u000a in PLGA microspheres prepared by the double emulsion-solvent evaporation method. Peptide stability was monitored by reversed-phase\\u000a high performance liquid chromatography (RP-HPLC) and identified

  2. Stability in dynamical astronomy.

    PubMed

    Szebehely, V

    1978-12-01

    Hill's concept of stability is generalized and its relation to bifurcation theory is shown. A quantitative measure of stability is introduced that allows the comparison of the stability of different astronomical systems. Theoretical stability limits for triple stellar systems, for planetary systems, and for satellite systems are established. The measure of stability is evaluated for several known triple stellar systems as well as for the planets and for the natural satellites of the solar system. The model of the restricted problem of three bodies and values of the Jacobian constant are used to study planetary and satellite systems. The model of the general problem of three bodies is used to establish criteria for triple stellar systems.IN GENERAL, THE RESULTS SHOW A HIERARCHY OF STABILITY: the existing triple systems are more stable than the planetary orbits of the solar system. The satellites of the solar system are least stable; in fact, some of the satellites are close to the line of instability (the Earth's Moon) and some are actually unstable (the four outermost satellites of Jupiter). PMID:16592589

  3. Aircraft Control-Position Indicator

    NASA Technical Reports Server (NTRS)

    Dennis, D. V.

    1985-01-01

    Aircraft control-position indicator cockpit-mounted instrument that displays positions of elevator and ailerons to pilot. Display is cruciform array of lights: horizontal row of amber lights and vertical row of green lights representing aileron and elevator positions, respectively. Display used extensively in spin testing and has been trouble-free, with no maintenance required after about 30 hours of operation.

  4. Gain function and hydrocarbon indicators

    Microsoft Academic Search

    De-hua Han; Michael Batzle

    1999-01-01

    Summary We have derived the gain function for porous rock based on the Gassmann's equation. We study property of the gain function for consolidated sandstone and poor consolidated sands from deep-water, Gulf of Mexico. We apply the gain function to derive pore fluid modulus as a hydrocarbon indicator from log data.

  5. Curiethérapie endobronchique : technique et indications

    Microsoft Academic Search

    C Hennequin; O Bleichner; J Trédaniel; C Maylin

    2003-01-01

    The endobronchial brachytherapy procedure involves the insertion of an afterloading catheter into bronchus in close proximity to an endoluminal lesion, and to perform limited irradiation sparing as much as possible normal health tissues. The catheter is inserted during a classical flexible bronchoscopy. Three types of indications have been discussed: (i) palliative treatment of lung carcinoma, with or without laser desobstruction:

  6. Geochemical indicators of intrinsic bioremediation

    Microsoft Academic Search

    Robert C. Borden; Carlos A. Gomez; Mark T. Becker

    1995-01-01

    A detailed field investigation has been completed at a gasoline-contaminated aquifer near Rocky Point, NC, to examine possible indicators of intrinsic bioremediation and identify factors that may significantly influence the rae and extent of bioremediation. The dissolved plume of benzene, toluene, ethylbenzene, and xylene (BTEX) in ground water is naturally degrading. Toluene and o-xylene are most rapidly degraded followed by

  7. Quality Indicators of Online Programs

    ERIC Educational Resources Information Center

    Hirner, Leo; Kochtanek, Thomas

    2012-01-01

    The continued growth of online programs in higher education has resulted in concerns about how institutions monitor the quality of their online programs. These concerns indicate a need for a process by which online programs may be evaluated and compared. They provided the impetus for this study, the goals of which were to identify quality…

  8. International Comparisons of Unemployment Indicators.

    ERIC Educational Resources Information Center

    Sorrentino, Constance

    1993-01-01

    Comparison of seven indicators (long-term unemployment, job losers, adult unemployment, full-time unemployment, conventional unemployment, part-time work for economic reasons, and discouraged workers) in North America, Europe, and Japan show that Sweden and Japan have the largest unemployment increase. Long-term joblessness prevailed in Europe;…

  9. Graph Theoretical Indicators and Refactoring

    Microsoft Academic Search

    J. Adrian Zimmer

    2003-01-01

    \\u000a Metrics of software quality grow stale after a while and there is always a need for new ones. Graph theory can be a fruitful\\u000a source. We discuss how. Before that we discuss what metrics do and we suggest the word “indicator” better describes that function\\u000a than the word “metric”.

  10. The Deep Space Network stability analyzer

    NASA Technical Reports Server (NTRS)

    Breidenthal, Julian C.; Greenhall, Charles A.; Hamell, Robert L.; Kuhnle, Paul F.

    1995-01-01

    A stability analyzer for testing NASA Deep Space Network installations during flight radio science experiments is described. The stability analyzer provides realtime measurements of signal properties of general experimental interest: power, phase, and amplitude spectra; Allan deviation; and time series of amplitude, phase shift, and differential phase shift. Input ports are provided for up to four 100 MHz frequency standards and eight baseband analog (greater than 100 kHz bandwidth) signals. Test results indicate the following upper bounds to noise floors when operating on 100 MHz signals: -145 dBc/Hz for phase noise spectrum further than 200 Hz from carrier, 2.5 x 10(exp -15) (tau =1 second) and 1.5 x 10(exp -17) (tau =1000 seconds) for Allan deviation, and 1 x 10(exp -4) degrees for 1-second averages of phase deviation. Four copies of the stability analyzer have been produced, plus one transportable unit for use at non-NASA observatories.

  11. Moving toward Ylide-Stabilized Carbenes.

    PubMed

    Borthakur, Bitupon; Phukan, Ashwini K

    2015-08-01

    The effect of ylide substitution at the ? position to the carbene carbon (Cc ) atom on the stability and ?-donating ability of a number of cyclic carbenes has been studied theoretically. The stabilities of all of the carbenes were investigated from an evaluation of their singlet-triplet energy gaps and stabilization energies. All carbenes were found to have a stable singlet state. The energy of the ?-symmetric lone-pair orbital at the Cc atom increases as a result of the introduction of ylide centers near to the Cc atom. This indicates an enhanced ?-donating ability of the ylide-containing carbenes. The calculated carbonyl-stretching frequencies of the corresponding rhodium complexes, proton affinities, and nucleophilicity index values correlate well with the ? basicity of the carbenes. PMID:26119685

  12. EVALUATION USING AN ORGANOPHILIC CLAY TO CHEMICALLY STABILIZE WASTE CONTAINING ORGANIC COMPOUNDS

    EPA Science Inventory

    A modified clay (organophilic) was utilized to evaluate the potential for chemically stabilizing a waste containing organic compounds. hemical bonding between the binder and the contaminants was indicated. eachate testing also indicated strong binding. Copy available at NTIS as ...

  13. The significance of froth stability in mineral flotation--a review.

    PubMed

    Farrokhpay, Saeed

    2011-08-10

    This paper presents a review of the published articles related to froth stability and its importance in mineral flotation. Froth structure and froth stability are known to play a significant role in determining the mineral grade and recovery achieved in a flotation operation. Froth stability is depending not only on the type and concentration of the frother but also on the nature and amount of the particles present in the system. To date, there is no specific criterion to quantify froth stability although a number of parameters are used as indicators of froth stability. Linking froth stability to the metallurgical performance is also challenged. PMID:21470589

  14. [Indications for catheter ablation of ventricular tachycardia].

    PubMed

    Deneke, T; Israel, C W; Krug, J; Nentwich, K; Müller, P; Mügge, A; Schade, A

    2013-09-01

    Ventricular tachyarrhythmias (VT) can cause sudden cardiac death. This can be prevented by an implantable cardioverter-defibrillator (ICD) but approximately 25% of patients with an ICD develop electrical storm (? 3 VTs within 24 hours) during the course of 4-5 years. This is a life-threatening event even in the presence of an ICD, particularly if incessant VT is present, and may significantly deteriorate the patient's psychological state if multiple shocks are discharged. Catheter ablation of VT has developed into a standard procedure in many specialized electrophysiology centers. Patients with hemodynamically stable and unstable VT are amendable to substrate-based ablation strategies. Catheter ablation can be performed as emergency procedure in patients with electrical storm as well as electively in patients with monomorphic VT stored in ICD memory. In patients with ischemic or non-ischemic cardiomyopathy, VT ablation is complementary to ICD implantation and can reduce the number of ventricular arrhythmia episodes and shocks and should be performed early. In patients with electrical storm, catheter ablation can acutely achieve rhythm stabilization and may improve prognosis in the long term. Further indications for catheter ablation exist in patients with idiopathic VT where catheter ablation represents a curative therapy, and in patients with symptomatic or asymptomatic frequent premature ventricular beats which may improve prognosis in patients with heart failure and cardiac resynchronization therapy. PMID:24046136

  15. Embryonic subcellular distribution of 13-cis- and all-trans-retinoic acid indicates differential cytosolic/nuclear localization.

    PubMed

    Rühl, R; Plum, C; Elmazar, M M; Nau, H

    2001-09-01

    Isotretinoin (13-cis-retinoic acid [13CRA], Accutane) is used for the treatment of dermatological diseases. Isotretinoin is, however, teratogenic in animals and humans. The mechanism of action of its teratogenicity is still not clearly identified. It has little or no binding properties to cytosolic retinoid-binding proteins or nuclear retinoid receptors (RAR, RXR). One hypothesis is that the teratogenicity of 2 approximately equipotent teratogenic doses of 13CRA and all-trans-retinoic acids (ATRA) could mainly be correlated to ATRA in the nuclei, where the retinoic acid receptors (RARs) are located. To test this hypothesis, female mice at gestational day 11 were treated with approximately equipotent teratogenic doses of 13-cis-retinoic acid (100 mg/kg orally) or all-trans-retinoic acid (10 mg/kg orally) and sacrificed 1 h and 4 h after administration. Embryos were homogenized and centrifuged into 4 fractions, and the purity of the fractions was tested by quantification of marker constituents for various cell compartments. We analyzed, by RP-HPLC, nuclear, mitochondrial, microsomal, and cytosolic fractions, as well as embryo homogenate and maternal plasma. After treatment with 13-cis-retinoic acid, this substance was mainly located in the nuclear fraction of the embryo (approximately 82%), whereas all-trans-retinoic acid, after ATRA treatment, was mainly located in the cytosolic supernatant (approximately 64%). The binding to cellular retinoid-binding protein (CRABP) may limit the access of ATRA to the nucleus, in contrast to 13CRA, which does not bind to CRABP. The concentration of ATRA in the nuclear fraction was similar after administration of either 13CRA or ATRA. The teratogenic activity of 13-cis-retinoic acid could therefore be explained by its access to the nucleus and its possible conversion to all-trans-retinoic acids, which will interact with the nuclear retinoid receptors. PMID:11509747

  16. Uncertainties in climate stabilization

    SciTech Connect

    Wigley, T. M.; Clarke, Leon E.; Edmonds, James A.; Jacoby, H. D.; Paltsev, S.; Pitcher, Hugh M.; Reilly, J. M.; Richels, Richard G.; Sarofim, M. C.; Smith, Steven J.

    2009-11-01

    We explore the atmospheric composition, temperature and sea level implications of new reference and cost-optimized stabilization emissions scenarios produced using three different Integrated Assessment (IA) models for U.S. Climate Change Science Program (CCSP) Synthesis and Assessment Product 2.1a. We also consider an extension of one of these sets of scenarios out to 2300. Stabilization is defined in terms of radiative forcing targets for the sum of gases potentially controlled under the Kyoto Protocol. For the most stringent stabilization case (“Level 1” with CO2 concentration stabilizing at about 450 ppm), peak CO2 emissions occur close to today, implying a need for immediate CO2 emissions abatement if we wish to stabilize at this level. In the extended reference case, CO2 stabilizes at 1000 ppm in 2200 – but even to achieve this target requires large and rapid CO2 emissions reductions over the 22nd century. Future temperature changes for the Level 1 stabilization case show considerable uncertainty even when a common set of climate model parameters is used (a result of different assumptions for non-Kyoto gases). Uncertainties are about a factor of three when climate sensitivity uncertainties are accounted for. We estimate the probability that warming from pre-industrial times will be less than 2oC to be about 50%. For one of the IA models, warming in the Level 1 case is greater out to 2050 than in the reference case, due to the effect of decreasing SO2 emissions that occur as a side effect of the policy-driven reduction in CO2 emissions. Sea level rise uncertainties for the Level 1 case are very large, with increases ranging from 12 to 100 cm over 2000 to 2300.

  17. Chapter A7. Biological Indicators

    USGS Publications Warehouse

    Myers, Donna N.; Wilde, Franceska D.

    2003-01-01

    The National Field Manual for the Collection of Water-Quality Data (National Field Manual) provides guidelines and standard procedures for U.S. Geological Survey (USGS) personnel who collect data used to assess the quality of the Nation's surface-water and ground-water resources. This chapter of the manual includes procedures for the (1) determination of biochemical oxygen demand using a 5-day bioassay test; (2) collection, identification, and enumeration of fecal indicator bacteria; (3) collection of samples and information on two laboratory methods for fecal indicator viruses (coliphages); and (4) collection of samples for protozoan pathogens. Each chapter of the National Field Manual is published separately and revised periodically. Newly published and revised chapters are posted on the World Wide Web on the USGS page 'National Field Manual for the Collection of Water-Quality Data.' The URL for this page is http://pubs.water.usgs.gov/twri9A/ (accessed November 25, 2003).

  18. Microbial indicators of soil quality

    SciTech Connect

    Turco, R.F.; Kennedy, A.C.; Jawson, M.

    1992-01-01

    Soil quality is an elusive term; however, the quality of a soil can greatly impact land use, sustainability, and productivity. Soil microbial processes are an integral part of soil quality and a better understanding of these processes and microbial community structure is needed. Microbial biomass, respiration, and labile nutrient pool size have generally been used as intrinsic parameters of a soil's microbial status. These analyses may not fully identify inherent differences in soil quality, especially if environmental conditions or manmade pertubations alter microbial community structure. Assessment of microbial community structure is necessary to determine the long-term effects of stress on soil quality. Measurement of microbial diversity should include nucleic acid and fatty acid phospholipid profiles as well as substrate utilization patterns. Microbial indicators will allow us to characterize the ecological status of the soil microbial community. For soil quality indicators to be successful, integration with other soil parameters is essential.

  19. Stress Indicators Quiz Never Always

    E-print Network

    Wang, Hai

    Stress Indicators Quiz Never Always 0 1 2 3 4 5 How Often 1. Do you get sick? 2. Do you get burnout! Commit to making a big change! SSS T R E S ST R E S ST R E S S STRESS © University of Southern or tired · Be able to focus only on the stressful situation (i.e. work or family) · Feel irritable

  20. Thermodynamic indicators for environmental certification.

    PubMed

    Panzieri, Margherita; Porcelli, Marcello; Pulselli, Federico Maria

    2002-09-01

    The Earth is an open thermodynamic system, that remains in a steady state far from the equilibrium, through energy and matter exchanges with the surrounding environment. These natural constraints, which prevent the system from maximizing its entropy, are threatened by human action and our ecosystem needs urgent protection. In this viewpoint the environmental certification was born, according to international standards ISO 14001, ISO 14040, and European Regulation EMAS. These are voluntary adhesions to a program of environmental protection by companies, administrations and organizations which, starting from the respect of the existing environmental laws and regulations, decide to further improve their environmental performance. To obtain and maintain certification of a system is necessary to apply some indicators to evaluate its environmental performance and to demonstrate its progressive improvement. Here we propose to use for this purpose the thermodynamic indicators produced from energy analysis by Odum. The case study is Montalcino city (Italy) and energy indicators are used to evaluate environmental performance of this system where exist different activities, from agricultural productions, to tourism. Results show that energy analysis could become a valid standard monitoring method for environmental certification, especially in consideration of its wide application field. PMID:12407910

  1. Segregation indices for disease clustering.

    PubMed

    Ceyhan, Elvan

    2014-05-10

    Spatial clustering has important implications in various fields. In particular, disease clustering is of major public concern in epidemiology. In this article, we propose the use of two distance-based segregation indices to test the significance of disease clustering among subjects whose locations are from a homogeneous or an inhomogeneous population. We derive the asymptotic distributions of the segregation indices and compare them with other distance-based disease clustering tests in terms of empirical size and power by extensive Monte Carlo simulations. The null pattern we consider is the random labeling (RL) of cases and controls to the given locations. Along this line, we investigate the sensitivity of the size of these tests to the underlying background pattern (e.g., clustered or homogenous) on which the RL is applied, the level of clustering and number of clusters, or to differences in relative abundances of the classes. We demonstrate that differences in relative abundances have the highest influence on the empirical sizes of the tests. We also propose various non-RL patterns as alternatives to the RL pattern and assess the empirical power performances of the tests under these alternatives. We observe that the empirical size of one of the indices is more robust to the differences in relative abundances, and this index performs comparable with the best performers in literature in terms of power. We illustrate the methods on two real-life examples from epidemiology. PMID:24307306

  2. DOE performance indicators guidance document

    SciTech Connect

    Not Available

    1992-12-01

    SEN-29-91 directed that a Department-wide uniform process for trending and analysis of operational data be established for DOE facilities. This Performance Indicator (PI) Program establishes a uniform system for trending and analyzing operational data providing an important tool to help assess and support progress in improving performance and strengthening both DOE and contractor line management control of operations. DOE, similar to the commercial nuclear industry, considers that facilities with good performance, as measured by an overall set of performance indicators, are well-managed facilities. The Performance Indicator Program established by SEN-29-91 is but one of several initiatives undertaken by DOE to instill a new DOE and DOE contractor line management culture committed to achieving a rising standard of acceptable performance. Line management trending and analysis of data depicting the performance of their facilities is an essential element in creating this culture of ``continuous improvement,`` where performance gains achieved are maintained and early identification of deteriorating environmental, safety, and health conditions is accomplished.

  3. Shuttle wing panel stability analysis

    NASA Technical Reports Server (NTRS)

    Balderes, T.; Mason, P. W.; Ranalli, E.; Zalesak, J.; Levy, A.

    1975-01-01

    The use of the NASTRAN program in the shuttle wing stability analysis is described, and details of the actual structure, the finite element idealization, and the NASTRAN results are given. A comparison of the NASTRAN results with those obtained with another computer program and with hand generated results indicates good agreement. An alternate approach for solving eigenvalue problems is illustrated and shows a considerable savings in computer time. Some emphasis is placed on the relationship of the NASTRAN analysis in the design process bringing out more clearly the contribution of the results and showing the importance of the mode plots. A deficiency in the NASTRAN plate elements when used to model structures made up of intersecting plates is discussed.

  4. ICRF stabilization of sawteeth on TFTR

    SciTech Connect

    Phillips, C.K.; Hosea, J.; Stevens, J.; Wilson, J.R.; Bell, M.; Bitter, M.; Cheng, C.Z.; Darrow, D.; Fredrickson, E.; Hammett, G.W.; Hill, K.; Hsuan, H.; Jassby, D.; McCune, D.; McGuire, K.; Owens, D.K.; Park, H.; Ramsey, A.; Schilling, G.; Schivell, J.; Stratton, B.; Synakowski, E.; Taylor, G.; Towner, H.; White, R.; Zweben, S. (Princeton Univ., NJ (United States). Plasma Physics Lab.); Marmar, E.; Snipes, J.; Terry, J.; Bo

    1992-01-01

    Results obtained from experiments utilizing high power ICRF (ion cyclotron range of frequency) heating to stabilize sawtooth oscillations on TFTR are reviewed. The key observations include existence of a minimum ICRF power required to achieve stabilization, a dependence of the stabilization threshold on the relative size of the ICRF power deposition profile to the q=1 volume, and a peaking of the equilibrium pressure and current profiles during sawtooth-free phases of the discharges. In addition, preliminary measurements of the poloidal magnetic field profile indicate that q on axis decreases to a value of 0.55{plus minus}0.15 after a sawtooth-stabilized period of {approximately}0.5 sec has transpired. The results are discussed in the context of theory, which suggests that the fast ions produced by the ICRF heating suppress sawteeth by stabilizing the m=1 MHD instabilities believed to be the trigger for the sawtooth oscillations. Though qualitative agreement is found between the observations and the theory, further refinement of the theory coupled with more accurate measurements of experimental profiles will be required in order to complete quantitative comparisons.

  5. ICRF stabilization of sawteeth on TFTR

    SciTech Connect

    Phillips, C.K.; Hosea, J.; Stevens, J.; Wilson, J.R.; Bell, M.; Bitter, M.; Cheng, C.Z.; Darrow, D.; Fredrickson, E.; Hammett, G.W.; Hill, K.; Hsuan, H.; Jassby, D.; McCune, D.; McGuire, K.; Owens, D.K.; Park, H.; Ramsey, A.; Schilling, G.; Schivell, J.; Stratton, B.; Synakowski, E.; Taylor, G.; Towner, H.; White, R.; Zweben, S. [Princeton Univ., NJ (United States). Plasma Physics Lab.; Marmar, E.; Snipes, J.; Terry, J.; Boivin, R. [Massachusetts Inst. of Tech., Cambridge, MA (United States); Phillips, M.W.; Hughes, M. [Grumman Corp., Princeton, NJ (United States); Bush, C.; Goldfinger, R.; Hoffman, D.; Houlberg, W. [Oak Ridge National Lab., TN (United States); Nagayama, Y. [Tokyo Univ. (Japan); Smithe, D.N. [Mission Research Corp., Newington, VA (United States)

    1992-01-01

    Results obtained from experiments utilizing high power ICRF (ion cyclotron range of frequency) heating to stabilize sawtooth oscillations on TFTR are reviewed. The key observations include existence of a minimum ICRF power required to achieve stabilization, a dependence of the stabilization threshold on the relative size of the ICRF power deposition profile to the q=1 volume, and a peaking of the equilibrium pressure and current profiles during sawtooth-free phases of the discharges. In addition, preliminary measurements of the poloidal magnetic field profile indicate that q on axis decreases to a value of 0.55{plus_minus}0.15 after a sawtooth-stabilized period of {approximately}0.5 sec has transpired. The results are discussed in the context of theory, which suggests that the fast ions produced by the ICRF heating suppress sawteeth by stabilizing the m=1 MHD instabilities believed to be the trigger for the sawtooth oscillations. Though qualitative agreement is found between the observations and the theory, further refinement of the theory coupled with more accurate measurements of experimental profiles will be required in order to complete quantitative comparisons.

  6. Stability versus maneuverability in aquatic locomotion.

    PubMed

    Weihs, Daniel

    2002-02-01

    The dictionary definition of stability as "Firmly established, not easily to be changed" immediately indicates the conflict between stability and maneuverability in aquatic locomotion. The present paper addresses several issues resulting from these opposing requirements. Classical stability theory for bodies moving in fluids is based on developments in submarine and airship motions. These have lateral symmetry, in common with most animals. This enables the separation of the equations of motion into two sets of 3 each. The vertical (longitudinal) set, which includes motions in the axial (surge), normal (heave) and pitching directions, can thus be separated from the lateral-horizontal plane which includes yaw, roll and sideslip motions. This has been found useful in the past for longitudinal stability studies based on coasting configurations but is not applicable to the analysis of turning, fast starts and vigorous swimming, where the lateral symmetry of the fish body is broken by bending motions. The present paper will also examine some of the aspects of the stability vs. maneuverability tradeoff for these asymmetric motions. An analysis of the conditions under which the separation of equations of motions into vertical and horizontal planes is justified, and a definition of the equations to be used in cases where this separation is not accurate enough is presented. PMID:21708701

  7. Thermodynamic modeling of natural zeolite stability

    SciTech Connect

    Chipera, S.J.; Bish, D.L.

    1997-06-01

    Zeolites occur in a variety of geologic environments and are used in numerous agricultural, commercial, and environmental applications. It is desirable to understand their stability both to predict future stability and to evaluate the geochemical conditions resulting in their formation. The use of estimated thermodynamic data for measured zeolite compositions allows thermodynamic modeling of stability relationships among zeolites in different geologic environments (diagenetic, saline and alkaline lakes, acid rock hydrothermal, basic rock, deep sea sediments). This modeling shows that the relative cation abundances in both the aqueous and solid phases, the aqueous silica activity, and temperature are important factors in determining the stable zeolite species. Siliceous zeolites (e.g., clinoptilolite, mordenite, erionite) present in saline and alkaline lakes or diagenetic deposits formed at elevated silica activities. Aluminous zeolites (e.g., natrolite, mesolite/scolecite, thomsonite) formed in basic rocks in association with reduced silica activities. Likewise, phillipsite formation is favored by reduced aqueous silica activities. The presence of erionite, chabazite, and phillipsite are indicative of environments with elevated potassium concentrations. Elevated temperature, calcic water conditions, and reduced silica activity help to enhance the laumontite and wairakite stability fields. Analcime stability increases with increased temperature and aqueous Na concentration, and/or with decreased silica activity.

  8. Cover and floristics of microphytic soil crusts in relation to indices of landscape health

    Microsoft Academic Search

    D. J. Eldridge; T. B. Koen

    1998-01-01

    An extensive field survey of 282 sites over 500 000 km2 of rangeland in eastern Australia was carried out to investigate the relationships between cover and floristics of microphytic soil crusts and indices of landscape health. Empirical quadrat-based data were used to calculate three indices of landscape health (soil stability, infiltration capacity and nutrient status) according to the method of

  9. Taccalonolide microtubule stabilizers.

    PubMed

    Li, Jing; Risinger, April L; Mooberry, Susan L

    2014-09-15

    This review focuses on a relatively new class of microtubule stabilizers, the taccalonolides. The taccalonolides are highly oxygenated pentacyclic steroids isolated from plants of the genus Tacca. Originally identified in a cell-based phenotypic screen, the taccalonolides have many properties similar to other microtubule stabilizers. They increase the density of interphase microtubules, causing microtubule bundling, and form abnormal multi-polar mitotic spindles leading to mitotic arrest and, ultimately, apoptosis. However, the taccalonolides differ from other microtubule stabilizers in that they retain efficacy in taxane resistant cell lines and in vivo models. Binding studies with the newly identified, potent taccalonolide AJ demonstrated covalent binding to ?-tubulin at or near the luminal and/or pore taxane binding site(s) which stabilizes microtubule protofilaments in a unique manner as compared to other microtubule stabilizers. The isolation and semi-synthesis of 21 taccalonolides helped to identify key structure activity relationships and the importance of multiple regions across the taccalonolide skeleton for optimal biological potency. PMID:24491636

  10. Hot Strange Stars. III. Stability

    NASA Astrophysics Data System (ADS)

    Hajyan, G. S.; Alaverdyan, A. G.

    2015-06-01

    The stability of hot strange stars (HSS) is studied. It is shown that a static stability criterion can be used to determine the stability of these stars. It is also found that stability is lost after the maximum mass in the mass-central density curves for isothermal series of HSS. These two points are so close that, as a first approximation, the maximum point can be regarded as the point at which the isothermal series of HSS loses stability.

  11. Stabilizing the Hammick intermediate.

    PubMed

    Hollóczki, Oldamur; Nyulászi, László

    2008-07-01

    The possible stabilization of pyridine-2-ylidene has been investigated at B3LYP/6-31+G* and B3LYP/6-311+G** levels of theory. The aromaticity of this compound is a significant contributor to its stability (ISE(c) = 24-27 kcal mol(-1), Bird index = 77, NICS(0) = -6.8 ppm, NICS(1) = -9.1 ppm; all about 80% of those for the H-shift isomer pyridine). The stabilization energy of the carbene (measured by an appropriate isodesmic reaction) can be influenced by the substitution at nitrogen with bulky groups, and at the carbon atom by amino groups. Considering possible competitive deprotonation reactions of the most likely synthetic route, 1j, 1k, and 1L are suggested as synthesizeable new stable carbenes. PMID:18543975

  12. Stability of Lobed Balloons

    NASA Technical Reports Server (NTRS)

    Ball, Danny (Technical Monitor); Pagitz, M.; Pellegrino, Xu S.

    2004-01-01

    This paper presents a computational study of the stability of simple lobed balloon structures. Two approaches are presented, one based on a wrinkled material model and one based on a variable Poisson s ratio model that eliminates compressive stresses iteratively. The first approach is used to investigate the stability of both a single isotensoid and a stack of four isotensoids, for perturbations of in.nitesimally small amplitude. It is found that both structures are stable for global deformation modes, but unstable for local modes at su.ciently large pressure. Both structures are stable if an isotropic model is assumed. The second approach is used to investigate the stability of the isotensoid stack for large shape perturbations, taking into account contact between di.erent surfaces. For this structure a distorted, stable configuration is found. It is also found that the volume enclosed by this con.guration is smaller than that enclosed by the undistorted structure.

  13. Construction and demolition waste indicators.

    PubMed

    Mália, Miguel; de Brito, Jorge; Pinheiro, Manuel Duarte; Bravo, Miguel

    2013-03-01

    The construction industry is one of the biggest and most active sectors of the European Union (EU), consuming more raw materials and energy than any other economic activity. Furthermore, construction waste is the commonest waste produced in the EU. Current EU legislation sets out to implement construction and demolition waste (CDW) prevention and recycling measures. However it lacks tools to accelerate the development of a sector as bound by tradition as the building industry. The main objective of the present study was to determine indicators to estimate the amount of CDW generated on site both globally and by waste stream. CDW generation was estimated for six specific sectors: new residential construction, new non-residential construction, residential demolition, non-residential demolition, residential refurbishment, and non-residential refurbishment. The data needed to develop the indicators was collected through an exhaustive survey of previous international studies. The indicators determined suggest that the average composition of waste generated on site is mostly concrete and ceramic materials. Specifically for new residential and new non-residential construction the production of concrete waste in buildings with a reinforced concrete structure lies between 17.8 and 32.9 kg m(-2) and between 18.3 and 40.1 kg m(-2), respectively. For the residential and non-residential demolition sectors the production of this waste stream in buildings with a reinforced concrete structure varies from 492 to 840 kg m(-2) and from 401 to 768 kg/m(-2), respectively. For the residential and non-residential refurbishment sectors the production of concrete waste in buildings lies between 18.9 and 45.9 kg/m(-2) and between 18.9 and 191.2 kg/m(-2), respectively. PMID:23315370

  14. Space Weathering: An Ultraviolet Indicator

    NASA Technical Reports Server (NTRS)

    Hendrix, A. R.; Vilas, F.

    2004-01-01

    We present evidence suggesting that the spectral slope of airless bodies in the UV-visible wavelength range can be used as an indicator of exposure to space weathering. While space weathering generally produces a reddening of spectra in the visible-NIR spectral regions, it tends to result in a bluing of the UV-visible portion of the spectrum, and may in some cases produce a spectral reversal. The bluing effect may be detectable with smaller amounts of weathering than are necessary to detect the longer-wavelength weathering effects.

  15. Space Weathering: An Ultraviolet Indicator

    NASA Technical Reports Server (NTRS)

    Hendrix, A. R.; Vilas, F.

    2003-01-01

    We present evidence suggesting that the spectral slope of airless bodies in the UV-visible wavelength range can be used as an indicator of exposure to space weathering. While space weathering generally produces a reddening of spectra in the visible-NIR spectral regions, it tends to result in a bluing of the UV-visible portion of the spectrum, and may in some cases produce a spectral reversal. The bluing effect may be detectable with smaller amounts of weathering than are necessary to detect the longer-wavelength weathering effects.

  16. The Stability Tunnel

    NASA Technical Reports Server (NTRS)

    1943-01-01

    Engineers operate the controls of the Stability Tunnel: Plans for a new tunnel to study stability problems began in the late thirties. The Stability Tunnel was authorized in 1939 and began operations in June 1941. The installation was completed in December that year with the completion of a new 10,000 Horsepower Diesel-electric generating plant. It was a single return, closed jet tunnel with a 6-foot square test section. The tunnel was disassembled and shipped to Virginia Polytechnic Institute and State University in 1958. The tunnel had two separate test sections: one for curved flow, the other for rolling flow. 'The facility...simulates the motion of the aircraft in curved or rolling flight. This is done by actually curving or rolling the airstream as it passes over the model and at the same time providing the proper velocity distribution.' (From AIAA-80-0309) >From Alan Pope, Wind-Tunnel Testing: 'The only tunnel directly designed for dynamic stability work is located at the Langley Field branch of the NACA. Its most vital feature is its ability to subject the models to curving air streams that simulate those actually encountered when an airplane rolls, pitches, or yaws. the rotating airstream for simulating roll is produced by a motor-driven paddle just ahead of the test section. Curved air of properly varying velocity for simulating pitch and yaw is produced by a combination of a curved test section and velocity screens. The proper use of this apparatus makes possible the determination of the stability derivatives.' Published in F.H. Lutze, 'Experimental Determination of Pure Rotary Stability Derivatives using a Curved and Rolling Flow Wind Tunnel,' AIAA-80-0309, AIAA 18th Aerospace Sciences Meeting, Pasadena, CA, January 14-16, 1980; Alan Pope, Wind-Tunnel Testing (New York: John Wiley & Sons, 1947).

  17. Stability of regional configurations

    SciTech Connect

    Canavan, G.H.

    1998-08-13

    At moderate force levels the first strike stability index is proportional to the first strike cost, so as the attacker minimizes attack costs, he automatically minimizes stability. Weapons grow rapidly and saturate to levels comparable to the number of value targets held at risk. This growth could appear destabilizing to dominant regional powers, whose response could in turn appear threatening to the major nuclear powers, which could slow or halt efforts towards deep reductions. The fundamental way to alter these pressures appears to be through reducing the likelihood of regional crises by removing these fundamental antagonisms.

  18. Stability criteria for emulsions

    NASA Astrophysics Data System (ADS)

    Bibette, J.; Morse, D. C.; Witten, T. A.; Weitz, D. A.

    1992-10-01

    The coalescence of monodisperse silicone oil-in-water emulsions stabilized with sodium dodecyl sulfate has been studied. We report the existence of a sharp destabilization threshold, controlled by surfactant chemical potential, osmotic pressure, and droplet diameter, at which the rate of coalescence increases dramatically. We present evidence that the stability of the emulsions can be characterized by two microscopic parameters: a minimum stable value of the surfactant chemical potential and a maximum value of the pressure exerted upon a droplet-droplet interface.

  19. Stabilized Zeeman split laser

    NASA Technical Reports Server (NTRS)

    1981-01-01

    The development of a stablized Zeeman split laser for use in a polarization profilometer is discussed. A Hewlett-Packard laser was modified to stabilize the Zeeman split beat frequency thereby increasing the phase measurement accuracy from the Hewlett-Packard 3 degrees to an accuracy of .01 degrees. The addition of a two layered inductive winding converts the laser to a current controlled oscillator whose frequency is linearly related to coil current. This linear relationship between coil current and laser frequency permits phase locking the laser frequency to a stable crystal controlled reference frequency. The stability of the system is examined and the equipment operation procedures are outlined.

  20. The effect of UV light on the thermooxidative stability of linear low density polyethylene films crosslinked by ionizing radiation

    NASA Astrophysics Data System (ADS)

    Sen, M.; Basfar, A. A.

    1998-06-01

    The effect of ultraviolet (UV) light on the thermooxidative stability of Linear Low Density Polyethylene(LLDPE) films was studied. LLDPE was stabilized with phenolic type antioxidant known as Irganox 1010, hindered amine light stabilizer known as Chimmasorb 944 and phenolic type gamma stabilizer. The influence of these additives on the thermooxidative stability of gamma and UV irradiated LLDPE were investigated by isothermal Differential Scanning Calorimeter (DSC). The oxidation induction time (OIT) experiments indicate that antirad free LLDPE films which contains antioxidant and UV stabilizer are more sensitive to gamma and UV radiation. On the other hand, films which contain antirad and irradiated to different doses of ?-radiation demonstrated improved thermooxidative stability.

  1. Low latency counter event indication

    DOEpatents

    Gara, Alan G. (Mount Kisco, NY); Salapura, Valentina (Chappaqua, NY)

    2010-08-24

    A hybrid counter array device for counting events with interrupt indication includes a first counter portion comprising N counter devices, each for counting signals representing event occurrences and providing a first count value representing lower order bits. An overflow bit device associated with each respective counter device is additionally set in response to an overflow condition. The hybrid counter array includes a second counter portion comprising a memory array device having N addressable memory locations in correspondence with the N counter devices, each addressable memory location for storing a second count value representing higher order bits. An operatively coupled control device monitors each associated overflow bit device and initiates incrementing a second count value stored at a corresponding memory location in response to a respective overflow bit being set. The incremented second count value is compared to an interrupt threshold value stored in a threshold register, and, when the second counter value is equal to the interrupt threshold value, a corresponding "interrupt arm" bit is set to enable a fast interrupt indication. On a subsequent roll-over of the lower bits of that counter, the interrupt will be fired.

  2. Pleurodesis: indications and radiologic appearance.

    PubMed

    Sonoda, Akinaga; Jeudy, Jean; White, Charles S; Kligerman, Seth J; Nitta, Norihisa; Lempel, Jason; Frazier, Aletta Ann

    2015-05-01

    Pleurodesis is frequently performed to prevent recurrence of pneumothorax or recurrent pleural effusion in benign or malignant conditions. In essence, it involves producing an area of adhesion between the parietal and the visceral layers of the pleura. The approach to this procedure can be divided into chemical and mechanical methods. Chemical pleurodesis is performed by introducing various substances such as talc, bleomycin, povidone iodine or other chemicals into the pleural space typically using a pleural catheter. The instilled substances cause inflammation of the parietal and the visceral layers of the pleura and leads to adhesion of the pleural surfaces, preventing further fluid or air accumulation. Mechanical pleurodesis, which is performed with thoracotomy or thoracoscopy, involves mechanical irritation of the pleura or removal of parietal pleura. It is important for the radiologist to develop an understanding of the clinical indications for pleurodesis, methods for the procedure and post-procedure imaging appearance so the radiologist can provide a correct interpretation and avoid misdiagnosis of the radiologic appearance as chronic infection, tumor or other entities with a similar appearance. Thus, the aim of this article is to review the indications, techniques and post-procedural appearances of pleurodesis from an imaging perspective. PMID:25791777

  3. Fluctuating asymmetry as an indicator of mercury exposure

    SciTech Connect

    Woodward, L.A. [Univ. of California, Davis, CA (United States); [Savannah River Ecology Lab., Aiken, SC (United States); Newman, M.C.; Mulvey, M. [Savannah River Ecology Lab., Aiken, SC (United States)

    1995-12-31

    Developmental stability is the ability of a developing organism to produce a consistent phenotype in a given environment. It provides a simple method of detecting stressed populations and monitoring their recovery. Laboratory experiments have documented the effect of environmental stress on developmental stability as demonstrated by amounts of fluctuating asymmetry. Fluctuating asymmetry assesses the amount of deviation from perfect bilateral symmetry in traits that would normally be symmetrical. Fluctuating asymmetry was examined for chironomid larvae (Chironomus plumosus) collected from a mercury contaminated lake. Larvae were collected from a gradient of mercury concentrations ranging from 2.6--106 mg/kg (DW). Numerous characters were examined for evidence of fluctuating asymmetry and for their utility as indicators of chronic mercury stress.

  4. Multiple diversity-stability mechanisms enhance population and community stability in aquatic food webs.

    PubMed

    Downing, Amy L; Brown, Bryan L; Leibold, Mathew A

    2014-01-01

    Biodiversity has been shown to increase the temporal stability of community and ecosystem attributes through multiple mechanisms, but these same mechanisms make less consistent predictions about the effects of richness on population stability. The overall effects of biodiversity on population and community stability will therefore depend on the dominant mechanisms that are likely to vary with the nature of biodiversity loss and the degree of environmental variability. We conducted a mesocosm experiment in which we generated a gradient in zooplankton species richness by directly manipulating dominant species and by allowing/preventing immigration from a metacommunity. The mesocosms were maintained under either constant or variable nutrient environments. Population, community, and ecosystem data were collected for five months. We found that zooplankton population and community stability is enhanced in species-rich communities in both constant and variable environments. Species richness increased primarily through the addition of species with low abundance. The communities that were connected to a metacommunity via immigration were the most diverse and the most stable, indicating the importance of both metacommunity dynamics and rare species for stability. We found little evidence for selection effects or overyielding as stabilizing forces. We did find support for asynchronous dynamics and statistical averaging, both of which predict destabilizing effects at the population level. We also found support for weak interactions, which predicts that both populations and communities will become more stable as richness increases. In order to understand the effects of biodiversity loss on stability, we will need to understand when different stabilizing mechanisms tend to operate but also how multiple mechanisms interact. PMID:24649657

  5. Internet Economy Indicators: January 2001 Internet Economy Indicators

    NSDL National Science Digital Library

    2001-01-01

    Internet Economy Indicators published in January the third of its biannual reports on the state of the Internet economy (for information on the June 2000 report, see the September 7, 2000 Scout Report for Business & Economics). The latest report finds that "the addition of 612,375 jobs in the Internet Economy in the first six months of 2000 was nearly as much as all of 1999 (when 650,000 jobs were added)." These data apparently belie more dire recent predictions concerning the state of the Internet economy. The report offers data and analysis of employment, revenues, types of jobs, comparison of Internet employment growth to the rest of the economy, comparison of Internet employment growth to revenue growth, and more. Funded by Cisco systems, the report was conducted by the University of Texas. Questions about the influence of corporate sponsors aside, the information here serves as a counterbalance to concerns about dot.com crashes (the report points out that dot.coms make up less than ten percent of the Internet's economy). The full report is offered in .pdf format with an executive summary, key findings, an overview, and selected data also posted on-site in HTML. The site also features an extensive report entitled Dot Coms and Productivity in the Internet Economy as well as an archive of previous biannual reports.

  6. The Seabed Stability Zonation in Chinese Offshore

    NASA Astrophysics Data System (ADS)

    Du, J.

    2013-12-01

    There are abundant natural resources and energy in Chinese offshore continental shelf, and which should be the most development potential region now and in the future. But the seabed of Chinese offshore is often under the instable status caused by many factors which deeply affects the safety of marine development. Marine geohazards is an active one among the influence factors. The marine geohazards means the geological factors developed in the seabed surface and the strata below the seabed, such as fault, shallow gas, landslide, coastal erosion, buried river channel, sand wave and sand ridge, easily liquefied sand layer etc., which will cause damage to the human life and property. In this paper, the seabed stability were analyzed and divided it into five grades based on the marine geohazards evaluation result which made by fuzzy mathematic model. Firstly, by collecting the analyzing the marine geohazards which distributed on the seabed or under the seabed, the marine geohazards maps in Chinese offshore were made and the classification system of marine geohazards was established. Then, the evaluation index system of seabed stability was set which included the seismic peak acceleration, geomorphology, direct geohazards and restricted geohazards. And the weighted value of each indicator was calculated by using analytic hierarchy process. And, a group of appropriate number with normal distribution was selected to replace the membership grade function. Based on above, a fuzzy evaluation model for seabed stability is established. Using the maps of marine geohazards, geomorphology maps and seismic peak acceleration maps as data source, using the fuzzy matrix as calculated method, based on the principles of maximum membership grade of fuzzy mathematics, we get the evaluation result of Chinese offshore with 6' by 6' grid unit. The maximum membership grade should be taken as the stability level in each unit. Above all, the seabed stability of Chinese offshore is divided into five grades according to the maximum membership grade. In this paper, we defined 5 classes which respectively were basically stable, relatively stable, medium, relatively unstable and unstable. By using statistical analysis method, a stability zonation map of the Chinese offshore has been drawn based on the evaluation result of each unit. From the stability map, Chinese offshore seabed stability was divided into sixty sub-regions with 5 classes. And the unstable sub-regions were mainly located in the North-East of Liaodong Bay, north of Laizhou Bay, the shoal in north Jiangsu, north Taiwan offshore and around Nan'ao Islands of Guangdong. Most Chinese offshore seabed stability has been in the relatively stable status.

  7. Country Indicators for Foreign Policy

    NSDL National Science Digital Library

    Created and maintained by the Department of Foreign Affairs and International Trade and Norman Paterson School of International Affairs, Country Indicators for Foreign Policy (CIFP) "represents an on-going effort to identify and assemble statistical information conveying the key features of the economic, political, social and cultural environments of countries around the world." Started in 1997, this flexible database project is intended to serve the needs of NGOs, government departments, and the private sector, and can potentially be used to aid in strategic decision-making, for risk analysis, and to monitor countries for possible "peacebuilding intervention." The database may be searched by region, regional and global organization, or by issue area. New users will want to visit the Users Guide, which offers detailed instructions for searching the database. Registration by email is required, and a user name and password will be emailed within two days.

  8. [Ketamine: psychiatric indications and misuses].

    PubMed

    Delimbeuf, N; Petit, A; Karila, L; Lejoyeux, M

    2014-01-01

    Ketamine or -ketamine hydrochloride- is used as an anesthesic and a painkiller. It may also, in some indications, be prescribed in psychiatry and addictology. A literature review was conducted from 2003 to 2013, in PubMed, Google Scholar, Embase, and Psyclnfo, using the following key words (alone or combined): "ketamine", "abuse", "addiction", "dependence" and "misuse". Various studies have shown the benefit of kétamine in some psychiatric conditions such as major depressive episodes and electroconvulsive therapy. Others have demonstrated beneficial effects in alcohol or opiate abstinence maintenance. Ketamine seems to be a promising molecule in psychiatry and in the treatment of addictions, despite the absence of marketing approval for those specific uses. Being a strong psycho-stimulant, ketamine can be the source of abuse and dependence with somatic, psychiatric and cognitive complications. PMID:25158385

  9. [Indications for neuroleptics in children].

    PubMed

    Mouren-Siméoni, M C; Bouvard, M P

    1990-01-01

    The purpose of this article is to summarize those main indications where neuroleptics have been proven efficient in children. In some types of pathology (hyperactivity, conduct disorders, mental retardation with agressiveness...), their impact is purely symptomatic, generally sedative. In other cases (Tourette's syndrome, stuttering) they seem to have a more specific effect. Whichever may be the case, neuroleptics seem to be irremplaceable, whenever the symptoms become incapacitating such as when they hinder the person's social functioning and learning abilities. On a practical level, one has to avoid "poorly justified" prescriptions, including low-dose prescriptions. In children and adolescents, therapy cannot be considered for one angle only: the administration of neuroleptics has to be integrated into a general treatment plan which involves other therapeutic approaches which are not mutually exclusive. PMID:1693559

  10. Stabilization Wedges Game

    NSDL National Science Digital Library

    Carbon Mitigation Initiative

    This is a team-based activity that teaches students about the scale of the greenhouse gas problem and the technologies that already exist which can dramatically reduce carbon emissions. Students select carbon-cutting strategies to construct a carbon mitigation profile, filling in the wedges of a climate stabilization triangle.

  11. Waste Stabilization Ponds.

    ERIC Educational Resources Information Center

    Koundakjian, Philip

    This self-paced course contains reading assignments from a waste stabilization ponds operating manual, supportive text, example problems, and review questions, and a final examination. The course covers calculation of pond surface area, pond volume, organic load, detention time, drawdown, storage capacity, efficiency, and discharge. In addition,…

  12. Recasting Bourgeois Europe: Stabilization

    E-print Network

    Landweber, Laura

    national histories. Second, he rethought the po- litical structure of the European interwar periodRecasting Bourgeois Europe: Stabilization in France, Germany, and Italy in the Decade after World an unparalleled analysis of the crucial decade in Europe after 1918. Based on extensive archival research in each

  13. Diodes stabilize LED output

    NASA Technical Reports Server (NTRS)

    Deters, R. A.

    1977-01-01

    Small-signal diodes are placed in series with light-emitting diodes (LED's) to stabilize LED output against temperature fluctuations. Simple inexpensive method compensates for thermal fluctuations over a broad temperature range. Requiring few components, technique is particularly useful where circuit-board space is limited.

  14. Sprinkler Bifurcations and Stability

    ERIC Educational Resources Information Center

    Sorensen, Jody; Rykken, Elyn

    2010-01-01

    After discussing common bifurcations of a one-parameter family of single variable functions, we introduce sprinkler bifurcations, in which any number of new fixed points emanate from a single point. Based on observations of these and other bifurcations, we then prove a number of general results about the stabilities of fixed points near a…

  15. MHD stability and fluctuations

    Microsoft Academic Search

    A. C. Sicardi Schifino; C. Ferro Fontán

    1989-01-01

    The effect of fluctuations on the stability of magnetohydrodynamic plasma equilibria is studied by the direct Lyapunov method, using the Fokker-Planck equation to model stationary random fluctuations. A fluctuation-dissipation theorem is derived and it is demonstrated that a deterministic stable system is not destabilized by the fluctuations. Member of ``Carrera del Investigador Científico del Consejo Nacional de Investigaciones Científicas y

  16. Selection, stability and renormalization

    Microsoft Academic Search

    Lin-Yuan Chen; Nigel Goldenfeld; Y. Oono; Glenn Paquette

    1994-01-01

    We illustrate how to extend the concept of structural stability through applying it to the front propagation speed selection problem. This consideration leads us to a renormalization group study of the problem. The study illustrates two very general conclusions: (1) singular perturbations in applied mathematics are best understood as renormalized perturbation methods, and (2) amplitude equations are renormalization group equations.

  17. Selection, Stability and Renormalization

    E-print Network

    Lin-Yuan Chen; Nigel Goldenfeld; Y. Oono; Glenn Paquette

    1993-10-05

    We illustrate how to extend the concept of structural stability through applying it to the front propagation speed selection problem. This consideration leads us to a renormalization group study of the problem. The study illustrates two very general conclusions: (1) singular perturbations in applied mathematics are best understood as renormalized perturbation methods, and (2) amplitude equations are renormalization group equations.

  18. Orbit Stabilization of Nanosat

    SciTech Connect

    JOHNSON,DAVID J.

    1999-12-01

    An algorithm is developed to control a pulsed {Delta}V thruster on a small satellite to allow it to fly in formation with a host satellite undergoing time dependent atmospheric drag deceleration. The algorithm uses four short thrusts per orbit to correct for differences in the average radii of the satellites due to differences in drag and one thrust to symmetrize the orbits. The radial difference between the orbits is the only input to the algorithm. The algorithm automatically stabilizes the orbits after ejection and includes provisions to allow azimuthal positional changes by modifying the drag compensation pulses. The algorithm gives radial and azimuthal deadbands of 50 cm and 3 m for a radial measurement accuracy of {+-} 5 cm and {+-} 60% period variation in the drag coefficient of the host. Approaches to further reduce the deadbands are described. The methodology of establishing a stable orbit after ejection is illustrated in an appendix. The results show the optimum ejection angle to minimize stabilization thrust is upward at 86{sup o} from the orbital velocity. At this angle the stabilization velocity that must be supplied by the thruster is half the ejection velocity. An ejection velocity of 0.02 m/sat 86{sup o} gives an azimuthal separation after ejection and orbit stabilization of 187 m. A description of liquid based gas thrusters suitable for the satellite control is included in an appendix.

  19. Stabilized chromium oxide film

    DOEpatents

    Garwin, Edward L. (Los Altos, CA); Nyaiesh, Ali R. (Palo Alto, CA)

    1988-01-01

    Stabilized air-oxidized chromium films deposited on high-power klystron ceramic windows and sleeves having a thickness between 20 and 150.ANG. are useful in lowering secondary electron emission yield and in avoiding multipactoring and window failure due to overheating. The ceramic substrate for the film is chosen from alumina, sapphire or beryllium oxide.

  20. Stabilized chromium oxide film

    DOEpatents

    Nyaiesh, A.R.; Garwin, E.L.

    1986-08-04

    Stabilized air-oxidized chromium films deposited on high-power klystron ceramic windows and sleeves having a thickness between 20 and 150A are useful in lowering secondary electron emission yield and in avoiding multipactoring and window failure due to overheating. The ceramic substrate for the film is chosen from alumina, sapphire or beryllium oxide.