Science.gov

Sample records for acquity uplc column

  1. Ultrafast UPLC-ESI-MS and HPLC with monolithic column for determination of principal flavor compounds in vanilla pods.

    PubMed

    Sharma, Upendra K; Sharma, Nandini; Sinha, Arun K; Kumar, Neeraj; Gupta, Ajai P

    2009-10-01

    In this study, two novel chromatographic methods based on monolithic column high-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC) were developed for the ultrafast determination of principal flavor compounds namely vanillin, vanillic acid, p-hydroxybenzoic acid, and p-hydroxybenzaldehyde in ethanolic extracts of Vanilla planifolia pods. Good separation was achieved within 2.5 min using Chromolith RP18e column (100 mm x 4.6 mm) for HPLC and Acquity BEH C-18 (100 mm x 2.1 mm, 1.7 microm) column for UPLC. Both methods were compared in terms of total analysis time, mobile phase consumption, sensitivity, and validation parameters like precision, accuracy, LOD, and LOQ. Further, system suitability test data including resolution, capacity factor, theoretical plates, and tailing factor was determined for both the methods by ten replicate injections. Monolithic column based HPLC gave better results for most of the selected parameters while UPLC was found to be more eco-friendly with low mobile phase consumption and better sensitivity. Both methods may be used conveniently for the high throughput analysis of large number of samples in comparison to traditional particulate column.

  2. A Fast and Reliable UPLC-PAD Fingerprint Analysis of Chimonanthus salicifolius Combined with Chemometrics Methods.

    PubMed

    Liang, Xianrui; Zhao, Cui; Su, Weike

    2016-08-01

    A novel fingerprinting approach was developed by means of ultra-high-performance liquid chromatography with photodiode array detector (UPLC-PAD) for the quality control of Chimonanthus salicifolius (C. salicifolius). All UPLC analyses were carried out on a Waters Acquity BEH Phenyl column (2.1 × 50 mm, 1.7 μm particle size) at 48°C, with a gradient mobile phase composed of 0.1% aqueous phosphoric acid and acetonitrile at a flow rate of 0.2 mL/min. The method validation results demonstrated the developed method possessing desirable precision [<0.88% relative standard deviation (RSD)], reproducibility (<1.87% RSD), stability (<1.42% RSD) and allowing fingerprint analysis in one chromatographic run within 21 min. The quality assessment was achieved by using chemometrics methods including similarity analysis, hierarchical clustering analysis and principal component analysis. The developed method can be used for further quality control of C. salicifolius. PMID:27226461

  3. [Comparison of chemical composition between fresh and processed Bufonis Venenum by UPLC-TQ-MS].

    PubMed

    Wang, Zi-yue; Wang, Hong-lan; Zhou, Jing; Ma, Hong-yue; Gong, Yan; Yan, Wen-li; Qian, Da-wei

    2015-10-01

    Toad venom is the Bufo bufo gargarizans or B. melanostictus after the ears of the gland secretion, used in the treatment of various cancers in recent years. Research shows that the main anti-tumor components in bufadienolide. Bufadienolide have free type structure and conjunct type structure. To identify and clarify the difference between bufogenin and bufotoxin contained in Bufonis Venenum, which was from B. bufo gargarizans, an UPLC-TQ-MS method has been established. UPLC-TQ-MS method was used to identify and quantify the major bufadienolides in Bufonis Venenum. UPLC-TQ-MS assay with positive ion mode was performed on a Waters ACQUITY UPLC BEH C, (2.1 mm x 100 mm, 1.7 µm) with the mobile phase consisting of 0. 1% aqueous formic and acidacetonitrile in gradient elution at a flow rate of 0.4 mL · min⁻¹ and the column temperature was set at 35 °C. By comparing their retention time and high resolution mass data of Bufonis Venenum extracts, 37 effective components were primarily identified by MS/MS analysis in positive ion mode. Twenty-six of them were free-type bufadienolides (bufogenin), 11 of them were conjugated bufadienolides. There were significant differences in the main composition between fresh and processed Bufonis Venenum. The study found that the chemical composition of toad venom through great changes after processing, conjunct type content is much less, free type content as well change. PMID:27062811

  4. Determination of Asymmetric and Symmetric Dimethylarginine in Serum from Patients with Chronic Kidney Disease: UPLC-MS/MS versus ELISA

    PubMed Central

    Boelaert, Jente; Schepers, Eva; Glorieux, Griet; Eloot, Sunny; Vanholder, Raymond; Lynen, Frédéric

    2016-01-01

    Asymmetric dimethylarginine (ADMA), an endogenous inhibitor of nitric oxide (NO) synthesis, and its structural isomer symmetric dimethylarginine (SDMA) are uremic toxins accumulating in chronic kidney disease (CKD) patients. The objective of this study was to develop and validate a robust UPLC-MS/MS method for the simultaneous determination of ADMA and SDMA in human serum. Chromatographic separation after butyl ester derivatization was achieved on an Acquity UPLC BEH C18 column, followed by tandem mass spectrometric detection. After validation, the applicability of the method was evaluated by the analysis of serum samples from 10 healthy controls and 77 CKD patients on hemodialysis (CKD5HD). Both ADMA (0.84 ± 0.19 µM vs. 0.52 ± 0.07 µM) and SDMA concentrations (2.06 ± 0.82 µM vs. 0.59 ± 0.13 µM) were significantly (p < 0.001) elevated in CKD5HD patients compared to healthy controls. In general, low degrees of protein binding were found for both ADMA and SDMA. In addition, an established commercially available ELISA kit was utilized on the same samples (n = 87) to compare values obtained both with ELISA and UPLC-MS/MS. Regression analysis between these two methods was significant (p < 0.0001) but moderate for both ADMA (R = 0.78) and SDMA (R = 0.72). PMID:27187471

  5. [Content determination of twelve major components in Tibetan medicine Zuozhu Daxi by UPLC].

    PubMed

    Qu, Yan; Li, Jin-hua; Zhang, Chen; Li, Chun-xue; Dong, Hong-jiao; Wang, Chang-sheng; Zeng, Rui; Chen, Xiao-hu

    2015-05-01

    A quantitative analytical method of ultra-high performance liquid chromatography (UPLC) was developed for simultaneously determining twelve components in Tibetan medicine Zuozhu Daxi. SIMPCA 12.0 software was used a principal component analysis PCA) and partial small squares analysis (PLSD-DA) on the twelve components in 10 batches from four pharmaceutical factories. Acquity UPLC BEH C15 column (2.1 mm x 100 mm, 1.7 µm) was adopted at the column temperature of 35 °C and eluted with acetonitrile (A) -0.05% phosphate acid solution (B) as the mobile phase with a flow rate of 0. 3 mL · min(-1). The injection volume was 1 µL. The detection wavelengths were set at 210 nm for alantolactone, isoalantolactone and oleanolic; 260 nm for trychnine and brucine; 288 nm for protopine; 306 nm for protopine, resveratrol and piperine; 370 nm for quercetin and isorhamnetin. The results showed a good separation among index components, with a good linearity relationship (R2 = 0.999 6) within the selected concentration range. The average sample recovery rates ranged between 99.44%-101.8%, with RSD between 0.37%-1.7%, indicating the method is rapid and accurate with a good repeatability and stability. The PCA and PLSD-DA analysis on the sample determination results revealed a great difference among samples from different pharmaceutical factories. The twelve components included in this study contributed significantly to the quantitative determination of intrinsic quality of Zuozhu Daxi. The UPLC established for to the quantitative determination of the twelve components can provide scientific basis for the comprehensive quality evaluation of Zuozhu Daxi. PMID:26323157

  6. UPLC method for the determination of vitamin E homologues and derivatives in vegetable oils, margarines and supplement capsules using pentafluorophenyl column.

    PubMed

    Wong, Yong Foo; Makahleh, Ahmad; Saad, Bahruddin; Ibrahim, Mohamad Nasir Mohamad; Rahim, Afidah Abdul; Brosse, Nicolas

    2014-12-01

    A sensitive and rapid reversed-phase ultra performance liquid chromatographic (UPLC) method for the simultaneous determination of tocopherols (α-, β-, γ-, δ-), tocotrienols (α-, β-, γ-, δ-), α-tocopherol acetate and α-tocopherol nicotinate is described. The separation was achieved using a Kinetex pentafluorophenyl (PFP) column (150 × 2.1mm, 2.6 µm) with both photodiode array (PDA) and fluorescence (FL) detectors that were connected in series. Column was thermostated at 42°C. Under a gradient system consisting of methanol and water at a constant flow rate of 0.38 mL min(-1), all the ten analytes were well separated in less than 9.5 min. The method was validated in terms of linearity, limits of detection and quantitation, precision and recoveries. Calibration curves of the ten compounds were well correlated (r(2)>0.999) within the range of 100 to 25,000 μg L(-1) for α-tocopherol acetate and α-tocopherol nicotinate, 10 to 25,000 μg L(-1) for α-tocotrienol and 5 to 25,000 μg L(-1) for the other components. The method is simple and sensitive with detection limits (S/N, 3) of 1.0 to 3.0 μg L(-1) (FL detection) and 30 to 74 μg L(-1) (PDA detection). Relative standard deviations for intra- and inter-day retention times (<1%) and peak areas (≤ 4%) were obtained. The method was successfully applied to the determination of vitamin E in vegetable oils (extra virgin olive, virgin olive, pomace olive, blended virgin and refined olive, sunflower, soybean, palm olein, carotino, crude palm, walnut, rice bran and grape seed), margarines and supplements.

  7. Development of a multiple immunoaffinity column for simultaneous determination of multiple mycotoxins in feeds using UPLC-MS/MS.

    PubMed

    Hu, Xiaofeng; Hu, Rui; Zhang, Zhaowei; Li, Peiwu; Zhang, Qi; Wang, Min

    2016-09-01

    A sensitive and specific immunoaffinity column to clean up and isolate multiple mycotoxins was developed along with a rapid one-step sample preparation procedure for ultra-performance liquid chromatography-tandem mass spectrometry analysis. Monoclonal antibodies against aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, zearalenone, ochratoxin A, sterigmatocystin, and T-2 toxin were coupled to microbeads for mycotoxin purification. We optimized a homogenization and extraction procedure as well as column loading and elution conditions to maximize recoveries from complex feed matrices. This method allowed rapid, simple, and simultaneous determination of mycotoxins in feeds with a single chromatographic run. Detection limits for these toxins ranged from 0.006 to 0.12 ng mL(-1), and quantitation limits ranged from 0.06 to 0.75 ng mL(-1). Concentration curves were linear from 0.12 to 40 μg kg(-1) with correlation coefficients of R (2) > 0.99. Intra-assay and inter-assay comparisons indicated excellent repeatability and reproducibility of the multiple immunoaffinity columns. As a proof of principle, 80 feed samples were tested and several contained multiple mycotoxins. This method is sensitive, rapid, and durable enough for multiple mycotoxin determinations that fulfill European Union and Chinese testing criteria. PMID:27225172

  8. Stability-indicating UPLC method for determination of Imatinib Mesylate and their degradation products in active pharmaceutical ingredient and pharmaceutical dosage forms.

    PubMed

    Nageswari, A; Reddy, K V S R Krishna; Mukkanti, K

    2012-07-01

    A simple, precise, accurate stability-indicating gradient reverse phase ultra-performance liquid chromatographic (RP-UPLC) method was developed for quantitative determination of purity of Imatinib Mesylate (IMM) drug substance and drug products in the presence of its process related impurities, and degradation products. The proposed RP-UPLC method utilizes Acquity UPLC BEH 50-mm, 2.1mm and 1.7 μm C-18 column at 30 °C, with a gradient program of 9.0 min at a flow rate of 0.3 mL/min. The compounds of interest were monitored at 237 nm. Resolution for Imatinib and eight related components was found to be greater than 1.5 for any pair of components. The correlation coefficients (r(2)>0.9990) obtained indicate clear correlations between the concentrations and their peak areas for the investigated compounds. RSD obtained for the repeatability and intermediate precision experiments, was less than 5.0%. Accuracy of the method was further ascertained by performing recovery studies through spiking experiments. The drug substance was subjected to hydrolytic, oxidative, photolytic and thermal stress conditions as per ICH. The developed method was validated according to the current ICH guidelines for specificity, limit of detection, limit of quantitation, linearity, accuracy, precision, ruggedness and robustness. The method is also suitable for the assay determination of IMM in pharmaceutical dosage forms.

  9. Determination of six Alternaria toxins with UPLC-MS/MS and their occurrence in tomatoes and tomato products from the Swiss market.

    PubMed

    Noser, Jürg; Schneider, Patrick; Rother, Martin; Schmutz, Hansruedi

    2011-11-01

    An ultra performance liquid chromatography (UPLC)-tandem mass spectrometry (MS/MS) method was developed for the determination of the Alternaria toxins tenuazonic acid, alternariol, alternariol monomethyl ether, altenuene, altertoxin I and tentoxin. Owing to its instability, altenusin could not be determined. The sample preparation includes an acidic acetonitrile/water/methanol extraction, followed by SPE clean-up step, before injection into the UPLC-MS/MS system. The separation was made on an Acquity UPLC column using a water/acetonitrile gradient with ammonium hydrogen carbonate as a modifier. Matrix compounds of real samples led to enhancement as well as suppression of the target compounds, depending on analyte and matrix. The recoveries were between 58 and 109% at a level of 10 μg/kg. Eighty-five tomato products, consisting of peeled and minced tomatoes, soup and sauces, tomato purées and concentrates, ketchup as well as dried and fresh tomatoes, were taken from the Swiss market in 2010. Tenuazonic acid was found most frequently (81 out of 85 samples) and in the highest levels of up to 790 μg/kg. Alternariol and alternariol monomethyl ether were found in lower concentrations, ranging from <1 to 33 μg/kg for alternariol and <5 to 9 μg/kg for alternariol monomethyl ether. Only a few samples were positive for altenuene and tentoxin. Altertoxin I was never detected. PMID:23605928

  10. Force degradation behavior of glucocorticoid deflazacort by UPLC: isolation, identification and characterization of degradant by FTIR, NMR and mass analysis

    PubMed Central

    Deshmukh, Rajesh; Sharma, Lata; Tekade, Muktika; Kesharwani, Prashant; Trivedi, Piyush; Tekade, Rakesh K.

    2016-01-01

    Abstract In this investigation, sensitive and reproducible methods are described for quantitative determination of deflazacort in the presence of its degradation product. The method was based on high performance liquid chromatography of the drug from its degradation product on reverse phase using Acquity UPLC BEH C18 columns (1.7 µm, 2.1 mm × 150 mm) using acetonitrile and water (40:60 V/V) at a flow rate of 0.2 mL/minute in UPLC. UV detection was performed at 240.1 nm. Deflazacort was subjected to oxidative, acid, base, hydrolytic, thermal and photolytic degradation. The drug was found to be stable in water and thermal stress, as well as under neutral stress conditions. However, forced-degradation study performed on deflazacort showed that the drug degraded under alkaline, acid and photolytic stress. The degradation products were well resolved from the main peak, which proved the stability-indicating power of the method. The developed method was validated as per ICH guidelines with respect to accuracy, linearity, limit of detection, limit of quantification, accuracy, precision and robustness, selectivity and specificity. Apart from the aforementioned, the results of the present study also emphasize the importance of isolation characterization and identification of degradant. Hence, an attempt was made to identify the degradants in deflazacort. One of the degradation products of deflazacort was isolated and identified by the FTIR, NMR and LC-MS study.

  11. Rapid determination of eight oxoisoaporphine alkaloids in Rhizoma Menispermi by the optimal homogenate extraction followed by UPLC-MS/MS.

    PubMed

    Wei, Jinxia; Jiang, Zhen; Cui, Zhi; Guo, Xingjie

    2015-07-01

    The objective of this study was to develop a rapid and reliable homogenate extraction (HGE) and ultra high-performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method for simultaneous analysis of eight bioactive oxoisoaporphine alkaloids (including two new alkaloids) in Rhizoma Menispermi. HGE was optimized by response surface methodology (RSM) to obtain the maximum extraction efficiency of eight alkaloids. Separation was achieved on a Waters ACQUITY UPLC® BEH C18 column (50 × 2.1 mm(2), 1.7 μm) using gradient elution with a mobile phase consisting of acetonitrile and 0.2% formic acid in water. Quantification was performed with multiple reaction monitoring (MRM) mode using positive ESI as an interface. This is the first report of the simultaneous analysis of eight oxoisoaporphine alkaloids in Rhizoma Menispermi using a UPLC-MS/MS method; this analysis afforded good linearity, precision, and accuracy. Then, the method was successfully applied to determine the alkaloids in Rhizoma Menispermi from different sources.

  12. An UPLC-MS/MS method for the analysis of glimepiride and fluoxetine in human plasma.

    PubMed

    Qiu, Xiangjun; Wang, Hong-wei; Yuan, Ye; Wang, Ying-fei; Sun, Ming; Huang, Xue-sun

    2015-02-01

    A sensitive and rapid ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed to determine glimepiride (GPD) and fluoxetine (FLU) in human plasma using diazepam as the internal standard (IS) simultaneously. The presented method used an Acquity UPLC BEH C18 column for chromatographic separation with tandem mass spectrometric detection on a QTrap5500 mass spectrometer operated in positive ESI mode. The mobile phase is a mixture of acetonitrile and 1% formic acid in water with gradient elution at a flow rate of 0.40mL/min. The GPD, FLU and IS were eluted at 1.46, 1.27 and 1.39min, respectively. The MRM transitions of m/z 491.3→126.3 and m/z 310.5→148.1 were used to quantify for GPD and FLU, respectively. The linearity of this method was found to be within the concentration range of 2.5-300ng/mL and 0.1-20ng/mL for GPD and FLU in human plasma, respectively. The intra- and inter-day precision (RSD%) were less than 10.3% and accuracy (RE%) was within ±7.3%. The matrix effect were 95.3-100.7% for GPD and FLU. GPD and FLU were sufficiently stable under all relevant analytical conditions. The method was also successfully applied to the clinical samples after a single oral dose of 2mg GLP and 40mg FLU in patients. PMID:25589252

  13. Photodegradation assessment of ciprofloxacin, moxifloxacin, norfloxacin and ofloxacin in the presence of excipients from tablets by UPLC-MS/MS and DSC

    PubMed Central

    2013-01-01

    Background Ciprofloxacin (CIP), moxifloxacin (MOX), norfloxacin (NOR) and ofloxacin (OFL), are the antibacterial synthetic drugs, belonging to the fluoroquinolones group. Fluoroquinolones are compounds susceptible to photodegradation process, which may lead to reduction of their antibacterial activity and to induce phototoxicity as a side effect. This paper describes a simple, sensitive UPLC-MS/MS method for the determination of CIP, MOX, NOR and OFL in the presence of photodegradation products. Results Chromatographic separations were carried out using the Acquity UPLC BEH C18 column; (2.1 × 100 mm, 1.7 μm particle size). The column was maintained at 40°C, and the following gradient was used: 0 min, 95% of eluent A and 5% of eluent B; 10 min, 0% of eluent A and 100% of eluent B, at a flow rate of 0.3 mL min-1. Eluent A: 0.1% (v/v) formic acid in water; eluent B: 0.1% (v/v) formic acid in acetonitrile. The method was validated and all the validation parameters were in the ranges acceptable by the guidelines for analytical method validation. The photodegradation of examined fluoroquinolones in solid phase in the presence of excipients followed kinetic of the first order reaction and depended upon the type of analyzed drugs and coexisting substances. Photodegradation process of analyzed drugs was confirmed by differential scanning calorimetry. In addition, the identification of degradation products was carried out by mass spectrometry. Conclusion The developed UPLC-MS/MS method enables the determination of CIP, MOX, NOR and OFL in the presence of photodegradation products and identification of photodegradation products. PMID:23899303

  14. SPE-UPLC-MS/MS method for sensitive and rapid determination of aripiprazole in human plasma to support a bioequivalence study.

    PubMed

    Patel, Daxesh P; Sharma, Primal; Sanyal, Mallika; Shrivastav, Pranav S

    2013-04-15

    An improved and rugged UPLC-MS/MS method has been developed and validated for sensitive and rapid determination of aripiprazole in human plasma using aripiprazole-d8 as the internal standard (IS). The analyte and IS were extracted from 100 μL of human plasma by solid-phase extraction using Phenomenex Strata-X (30 mg, 1 cc) cartridges. Chromatography was achieved on an Acquity UPLC BEH C18 (50 mm × 2.1 mm, 1.7 μm) analytical column using methanol: 10mM ammonium formate (85:15, v/v) as the mobile phase with isocratic elution. Quantitation was done using multiple reaction monitoring in the positive ionization mode. The linearity of the method was established in the concentration range 0.05-80 ng/mL. The mean extraction recovery was greater than 96% across QC levels, while intra- and inter batch accuracy and precision (% CV) values ranged from 97.4 to 101.9% and from 1.20 to 3.72% respectively. The relative matrix effect in eight different lots of plasma samples, expressed as % CV for the calculated slopes of calibration curves was 1.08%. The stability of aripiprazole was studied under different storage conditions. The validated method was used to support a bioequivalence study of 10mg aripiprazole formulation in 36 healthy Indian subjects. PMID:23510852

  15. Development and validation of sensitive and rapid UPLC-MS/MS method for quantitative determination of daclatasvir in human plasma: Application to a bioequivalence study.

    PubMed

    Rezk, Mamdouh R; Bendas, Ehab R; Basalious, Emad B; Karim, Iman A

    2016-09-01

    A rapid and sensitive UPLC-MS/MS method was developed and validated for determination of daclatasvir (DAC) in human plasma using sofosbuvir (SOF) as an internal standard (IS). The Xevo TQD LC-MS/MS was operated under the multiple-reaction monitoring mode using electrospray ionization. Precipitation with acetonitrile was used in sample preparation. The prepared samples were chromatographed on Acquity UPLC HSS C18 (50×2.1mm, 1.8μm) column by pumping 10mM ammonium formate (pH 3.5) and acetonitrile in an isocratic mode at a flow rate of 0.30ml/min. Method validation was performed as per the FDA guidelines and the standard curves were found to be linear in the range of 5-4000ng/ml for DAC. The intra-day and inter-day precision and accuracy results were within the acceptable limits. A very short run time of 1.2min made it possible to analyze more than 500 human plasma samples per day. The wider range of quantification of DAC allowed the applicability of the developed method for its determination in a bioequivalence study in human volunteers. PMID:27232152

  16. Development and Validation of a UPLC Method by the QbD-Approach for the Estimation of Rabeprazole and Levosulpiride from Capsules

    PubMed Central

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

    2014-01-01

    Statistical experimental design was used to optimize the chromatographic separations of two pharmaceutical compounds from their respective potential impurities. A fractional factorial design was utilized to study the effects of pH, organic solvent in mobile phases A&B, and flow rate on the resolution of Rabeprazole and Rabeprazole Sulfone, which had closely eluting peaks. A desirability function applied to the optimized conditions predicted the peak resolution between 2.2 and 2.7 for the Rabeprazole & Rabeprazole Sulfone impurity. The chromatographic method employed an Acquity UPLC, BEH C18 column (100 × 2.1 mm i.d., 1.7 μm particle size) with the mobile phase consisting of a phosphate buffer, pH 6.5, and acetonitrile in a gradient program. The flow rate and injection volumes were 0.45 mL/min & 5 μl, respectively, and detection was done at 254 nm. The chromatographic method was validated for linearity, accuracy, precision, specificity, and ruggedness according to ICH guidelines. The results clearly showed that the quality by design concept could be effectively applied to optimize a UPLC chromatographic method with fewer trials and error-free experimentation. PMID:24959404

  17. Simultaneous Determination of Typhaneoside and Isorhamnetin-3-O-Neohesperidoside in Rats After Oral Administration of Pollen Typhae Extract by UPLC-MS/MS.

    PubMed

    Cao, Sali; Ni, Boran; Feng, Lijun; Yin, Xingbin; Dou, Haoran; Fu, Jing; Lin, Longfei; Ni, Jian

    2015-07-01

    For the first time, a selective and rapid ultra-performance liquid chromatography method with tandem mass spectrometric (UPLC-MS/MS) detection for simultaneous determination of typhaneoside and isorhamnetin-3-O-neohesperidoside in rat plasma was developed and validated, which was applied to the pharmacokinetic study of Pollen Typhae extract. The separation was carried out on an ACQUITY UPLC(TM) BEH C18 column with gradient elution using mobile phase including acetonitrile and water (containing 0.1% formic acid). The flow rate was 0.4 mL/min. The detection was conducted by means of electrospray ionization mass spectrometry in negative ion mode with multiple reaction monitoring. The assays were linear over the concentration range of 0.5-100 ng/mL, and the lower limit of quantification was 0.5 ng/mL for typhaneoside and isorhamnetin-3-O-neohesperidoside. The method was validated in terms of intra- and interday precision (<9.37%), accuracy (within ±10.91%), linearity, specificity and stability, and has been successfully applied to a pharmacokinetic study of Pollen Typhae extract in rats after oral administration.

  18. 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

  19. RP-UPLC method development and validation for the simultaneous estimation of ibuprofen and famotidine in pharmaceutical dosage form

    PubMed Central

    Reddy, Yarram Ramakoti; Kumar, Kakumani Kishore; Reddy, MRP; Mukkanti, K

    2012-01-01

    Aim and Backrgound: A stability-indicating LC method was developed for the simultaneous determination of Ibuprofen and Famotidine in pharmaceutical dosage forms. Materials and Methods: The chromatographic separation was achieved on Acquity UPLC BEH C-18,50 mm × 2.1 mm and 1.7 μm column with gradient elution. The mobile phase A contains a mixture of 50 mM sodium acetate buffer (pH 5.5): methanol (85:15, v/v), and the mobile phase B contains a mixture of 50 mM sodium acetate buffer (pH 5.5): methanol (25:75, v/v). The flow rate was 0.3 mL min-1, and the detection wavelength was 260 nm. Results: The limit of detection for Ibuprofen and Famotidine was 1.6 and 1.2 μg mL-1, respectively. The limit of quantification (LOQ) for Ibuprofen and Famotidine was 5.1 and 4.3 μg mL-1, respectively. Conclusion: This method was validated for accuracy, precision, and linearity. The method was also found to be stability indicating. PMID:23781479

  20. Chemical prospection of important ayurvedic plant Tinospora cordifolia by UPLC-DAD-ESI-QTOF-MS/MS and NMR.

    PubMed

    Bala, Manju; Verma, Praveen Kumar; Awasthi, Shiv; Kumar, Neeraj; Lal, Brij; Singh, Bikram

    2015-01-01

    A rapid, sensitive, and accurate ultra-performance liquid chromatography coupled with mass spectrometric method (UPLC-MS) was developed and validated for simultaneous determination of four bioactive compounds, syringin (3), cordifolioside A (4), magnoflorine (6) and tinocordiside (10) in the stem of Tinospora cordifolia. The analysis was performed using an Acquity C18 column and gradient elution of 0.05% formic acid in water and acetonitrile at a detection wavelength of 267 nm in 5 min. A high correlation coefficient (r2 > 0.998) indicated good correlation between investigated compounds concentration and their peak area within the test ranges. The LODs for compounds 3, 4, 6 and 10 were 1.95, 0.97, 3.90 and 0.97 ng/mL, respectively, and LOQs were 6.64, 3.20, 12.87 and 3.20 ng/mL, respectively. The overall intra- and inter-day variations of the four compounds were less than 1%. The variation of these four bioactive compounds in T. cordifolia hosted on fifteen different trees was also determined. The compounds (3, 4, 6 and 10) were found in high amount in the T. cordifolia hosted on Azadirachta indica and Mangifera indica as compared with other plants. Twelve compounds were identified on the basis of their mass and UV-vis spectra. The NMR fingerprinting of the extract revealed the presence of alkaloids, fatty acid methyl esters, polysaccharides and marker components of T. cordifolia. PMID:25920217

  1. Improved method to determine succinylacetone in dried blood spots for diagnosis of tyrosinemia type 1 using UPLC-MS/MS.

    PubMed

    Al-Dirbashi, Osama Y; Rashed, Mohamed S; Jacob, Minnie; Al-Ahaideb, Lujane Y; Al-Amoudi, Mohamed; Rahbeeni, Zuhair; Al-Sayed, Moeen M; Al-Hassnan, Zuhair; Al-Owain, Mohamed; Al-Zeidan, Hamad

    2008-11-01

    We describe an improved diagnostic method for tyrosinemia type 1 based on quantifying succinylacetone in dried blood spots by ultra-performance liquid chromatography tandem mass spectrometry. Succinylacetone extracted from a single 3/16 inch disk of specimen collection paper containing a dried blood spot was derivatized with dansylhydrazine, separated on an Acquity UPLC BEH C(18) column (2.1 x 50 mm, 1.7 microm) and detected by electrospray ionization tandem mass spectrometry. Succinylacetone derivative eluted at 0.6 min with a complete run time of 1 min. Using a 13C4 labeled succinylacetone as an internal standard, the calibration plot was linear up to 100 micromol/L with a detection limit (S/N = 3) of 0.2 micromol/L. Intra-day (n = 13) and inter-day (n = 10) variations were better than 10%. The cutoff level of succinylacetone in dried blood spots from healthy infants obtained by the current method was 0.63 micromol/L (n = 151). In dried blood spots from patients with established tyrosinemia type 1 (n = 11), concentration of succinylacetone was 6.4-30.8 micromol/L.

  2. UPLC-MS-MS Method for the Determination of Vilazodone in Human Plasma: Application to a Pharmacokinetic Study.

    PubMed

    El-Bagary, Ramzia; Hashem, Hanaa; Fouad, Marwa; Tarek, Sally

    2016-09-01

    A sensitive, rapid and simple liquid chromatographic-electrospray ionization tandem mass spectrometric (LC-ESI-MS-MS) method was developed for the quantitative determination of vilazodone in human plasma and for the study of the pharmacokinetic behavior of vilazodone in healthy Egyptian volunteers. With escitalopram as internal standard (IS), liquid-liquid extraction was used for the purification and preconcentration of analytes from human plasma matrix using diethyl ether. The separation was performed on an Acquity UPLC BEH shield RP C18 column (1.7 µm, 2.1 × 150 mm). Isocratic elution was applied using methanol-0.2% formic acid (90:10, v/v). Detection was performed on a triple-quadrupole tandem mass spectrometer with multiple reaction monitoring mode via an electrospray ionization source at m/z 442.21 → 155.23 for vilazodone and m/z 325.14 → 109.2 for escitalopram. Linear calibration curves were obtained over the range of 1-200 ng/mL with the lower limit of quantification at 1 ng/mL. The intra- and inter-day precision showed relative standard deviation ≤3.3%. The total run time was 1.5 min. This method was successfully applied for clinical pharmacokinetic investigation, and a preliminary metabolic study was also carried out. PMID:27209054

  3. Simultaneous determination of loganin, morroniside, catalpol and acteoside in normal and chronic kidney disease rat plasma by UPLC-MS for investigating the pharmacokinetics of Rehmannia glutinosa and Cornus officinalis Sieb drug pair extract.

    PubMed

    Zhao, Min; Tao, Jinhua; Qian, Dawei; Liu, Pei; Shang, Er-xin; Jiang, Shu; Guo, Jianming; Su, Shu-lan; Duan, Jin-ao; Du, Leyue

    2016-01-15

    A sensitive and rapid method for determination of loganin, morroniside, catalpol and acteoside in rat plasma after oral administration of Rehmannia glutinosa Libosch and Cornus officinalis Sieb drug pair based on ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS). Chromatographic separation was achieved using an Acquity UPLC BEH C18 column (100mm×2.1mm, 1.7μm) at a flow rate of 0.4mL/min, using gradient mode containing 0.1% formic acid in water and acetonitrile were used as the mobile phase A and B. Loganin, morroniside, catalpol, acteoside and the internal standard (chloramphenicol) were detected by selected reaction monitoring in the negative ion mode with the mass transition of m/z 451.0→179.0 (morroniside), m/z 435.0→227.0 (loganin), m/z 407.1→199.1 (catalpol), m/z 623.2→161.0 (acteoside) and m/z 320.8→151.9 (chloramphenicol), respectively. All calibration curves showed good linearity (r>0.991). The precision was evaluated by intra-day and inter-day assays and the RSD% were all within 9.58%. The recovery ranged from 67.62 to 80.14%. The method was successfully applied to pharmacokinetic study of the analytes in normal and doxorubicin-induced chronic kidney disease rat plasma.

  4. Determination of N-nitrosodiethanolamine, NDELA in cosmetic ingredients and products by mixed mode solid phase extraction and UPLC-tandem mass spectrometry with porous graphitic carbon column through systemic sample pre-cleanup procedure.

    PubMed

    Joo, Kyung-Mi; Shin, Mi-Sook; Jung, Ji-hee; Kim, Boo-Min; Lee, John-Whan; Jeong, Hye-Jin; Lim, Kyung-Min

    2015-05-01

    A rapid, sensitive, accurate and specific ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) method for the detection of N-nitrosodiethanolamine (NDELA), a highly toxic contaminant in cosmetic raw materials and products was developed and validated. Systematized sample preparation steps were developed according to product types. Various SPE cartridges and columns were examined to establish the condition of SPE and chromatographic separation for NDELA. Sample cleanup steps consisting of solvent and liquid-liquid extraction tailored to the various sample matrix types were established prior to mixed mode SPE (Bond Elut AccuCAT). Chromatographic separation was achieved within 7 min on a porous graphitic carbon (PGC) column using a gradient elution with the mobile phase of 1mM ammonium acetate containing 0.1% acetic acid and methanol. NDELA was monitored using an electrospray positive ionization mass spectrometry in the multiple reaction monitoring (MRM) mode (m/z 134.9>103.7(quantifier) and 73.7(qualifier ion)) with d8-NDELA (m/z 143.1>111.0) as internal standard. The standard curves were linear over the concentration range of 1-100 ng/mL with a correlation coefficient higher than 0.99. The limit of detection (LOD) and the limit of quantification (LOQ) was 10 and 20 μg/kg, respectively (0.5 and 1 ng/mL in standard solution). The intra- and inter-day precisions were estimated to be below 11.1% and accuracies were within the range of 90.8-115.8%. The validated method was successfully applied to the analysis of real samples including raw materials, skin care, make-up, shampoos and hair products. PMID:25770613

  5. Validated UPLC-MS/MS assay for the determination of synthetic phosphodiesterase type-5 inhibitors in postmortem blood samples.

    PubMed

    Proença, Paula; Mustra, Carla; Marcos, Mariana; Franco, João Miguel; Corte-Real, Francisco; Vieira, Duarte Nuno

    2013-08-01

    The use of synthetic phosphodiesterase type 5 (PDE-5) inhibitors for the treatment of erectile dysfunction: sildenafil citrate (Viagra(®)), tadalafil (Cialis(®)) and vardenafil hydrochloride (Levitra(®)) has increased dramatically over the past 2 years. These substances are prescription drugs and must be used under medical supervision. However, they can easily be obtained over the internet from illegal sites, being a potential for a threat to public health. The development of an electrospray ionisation (ESI) ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) procedure for the simultaneous identification and quantification of three PDE5 inhibitors in blood samples was desired. Samples were prepared using Oasis(®) HLB solid-phase cartridges (3 cc, 60 mg) and chromatographic separation was achieved on an Acquity UPLC(®) HSS T3 (100 × 2.1 mm i.d., 1.8 μm particles) column with a gradient mobile phase of 0.1% formic acid and acetonitrile at a 0.5 mL/min flow rate. Quantification was achieved by multiple reaction monitoring (MRM) of two transitions per compound: m/z 475.1 > 58 e m/z 475.1 > 311.1 for sildenafil; m/z 389.9 > 267.9 e m/z 389.9 > 134.8 for tadalafil and m/z 489 > 71.9 e m/z 489 > 150.9 for vardenafil. Zolpidem-d6 (m/z 314.5 > 235.3) was used as the internal standard. Calibration curves were linear over the concentration range of 5-1000 ng/mL, with a coefficient of determination better than 0.997. The lower limits of detection and quantification for these substances were ≤ 3 ng/mL and ≤ 8 ng/mL, respectively. The method showed a satisfactory sensitivity, precision, accuracy, recovery and selectivity. A rapid, selective and sensitive UPLC-MS/MS method using solid-phase extraction was developed for the simultaneous determination and quantification of sildenafil, vardenafil and tadalafil in blood samples. PMID:23910856

  6. Development and validation of a selective, sensitive and stability indicating UPLC-MS/MS method for rapid, simultaneous determination of six process related impurities in darunavir drug substance.

    PubMed

    A, Vijaya Bhaskar Reddy; Yusop, Zulkifli; Jaafar, Jafariah; Aris, Azmi B; Majid, Zaiton A; Umar, Khalid; Talib, Juhaizah

    2016-09-01

    In this study a sensitive and selective gradient reverse phase UPLC-MS/MS method was developed for the simultaneous determination of six process related impurities viz., Imp-I, Imp-II, Imp-III, Imp-IV, Imp-V and Imp-VI in darunavir. The chromatographic separation was performed on Acquity UPLC BEH C18 (50 mm×2.1mm, 1.7μm) column using gradient elution of acetonitrile-methanol (80:20, v/v) and 5.0mM ammonium acetate containing 0.01% formic acid at a flow rate of 0.4mL/min. Both negative and positive electrospray ionization (ESI) modes were operated simultaneously using multiple reaction monitoring (MRM) for the quantification of all six impurities in darunavir. The developed method was fully validated following ICH guidelines with respect to specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision, robustness and sample solution stability. The method was able to quantitate Imp-I, Imp-IV, Imp-V at 0.3ppm and Imp-II, Imp-III, and Imp-VI at 0.2ppm with respect to 5.0mg/mL of darunavir. The calibration curves showed good linearity over the concentration range of LOQ to 250% for all six impurities. The correlation coefficient obtained was >0.9989 in all the cases. The accuracy of the method lies between 89.90% and 104.60% for all six impurities. Finally, the method has been successfully applied for three formulation batches of darunavir to determine the above mentioned impurities, however no impurity was found beyond the LOQ. This method is a good quality control tool for the trace level quantification of six process related impurities in darunavir during its synthesis.

  7. Simultaneous quantification of vortioxetine, carvedilol and its active metabolite 4-hydroxyphenyl carvedilol in rat plasma by UPLC-MS/MS: Application to their pharmacokinetic interaction study.

    PubMed

    Huang, Yi; Zheng, Shuangli; Pan, Yongyang; Li, Tao; Xu, Zhi-Sheng; Shao, Meng-Meng

    2016-09-01

    To establish a rapid and sensitive ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for the determination of vortioxetine, carvedilol and its metabolite 4-hydroxyphenyl carvedilol in rat plasma. The analytes and the internal standard (diazepam) were separated on an Acquity UPLC BEH C18 chromatography column (2.1mm×50mm, 1.7μm) using gradient elution with a mobile phase of acetonitrile and 0.1% formic acid in water at a flow rate of 0.4mL/min. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) mode to monitor the precursor-to-product ion transitions of m/z 299.2→150.1 for vortioxetine, m/z 407.2→100.3 for carvedilol, m/z 423.2→100.1 for 4-hydroxyphenyl carvedilol and m/z 285.2→193.1 for diazepam (IS) using a positive electrospray ionization interface. The method was validated over a concentration range of 0.5-100ng/mL for vortioxetine, 0.5-1000ng/mL for carvedilol and 0.1-50ng/mL for 4-hydroxyphenyl carvedilol. Total time for each chromatograph was 3.0min. The intra- and inter-day precision and accuracy of the quality control samples at low, medium, and high concentration levels exhibited relative standard deviations (RSD)<11.6% and the accuracy values ranged from -12.2% to 11.3%. The analytical method was successfully applied to a pharmacokinetic interaction study of vortioxetine and carvedilol after oral administration vortioxetine and carvedilol in rats. Results suggested that the co-administration of vortioxetine and carvedilol results in a significant drug interaction in rats. PMID:27262994

  8. Simultaneous determination of ledipasvir, sofosbuvir and its metabolite in rat plasma by UPLC-MS/MS and its application to a pharmacokinetic study.

    PubMed

    Pan, Chenwei; Chen, Yongping; Chen, Weilai; Zhou, Guangyao; Jin, Lingxiang; Zheng, Yi; Lin, Wei; Pan, Zhenzhen

    2016-01-01

    In this work, a rapid and sensitive ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for the determination of ledipasvir, sofosbuvir and its metabolite GS-331007 in rat plasma was developed. The analytes and the internal standard (diazepam) were separated on an Acquity UPLC BEH C18 chromatography column (2.1mm×50mm, 1.7μm) using gradient elution with a mobile phase of acetonitrile and 0.1% formic acid in water at a flow rate of 0.4mL/min. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) mode to monitor the precursor-to-product ion transitions of m/z 889.8→130.1 for ledipasvir, m/z 530.3→243.1 for sofosbuvir, m/z 261.5→113.1 for GS-331007 and m/z 285.2→193.1 for diazepam (IS) using a positive electrospray ionization interface. The method was validated over a concentration range of 2-500ng/mL for ledipasvir, 10-2000ng/mL for sofosbuvir and 10-2000ng/mL for GS-331007. Total time for each chromatography was 3.0min. The intra- and inter-day precision and accuracy of the quality control samples at low, medium, and high concentration levels exhibited relative standard deviations (RSD)<10.2% and the accuracy values ranged from -9.8% to 11.2%. The method was successfully applied to a pharmacokinetic study of ledipasvir, sofosbuvir and GS-331007 in rats.

  9. Evaluation of a rapid method for the simultaneous quantification of ribavirin, sofosbuvir and its metabolite in rat plasma by UPLC-MS/MS.

    PubMed

    Shi, Xiaojun; Zhu, Dedong; Lou, Jie; Zhu, Bo; Hu, Ai-rong; Gan, Dongmei

    2015-10-01

    A rapid and sensitive ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for the determination of ribavirin, sofosbuvir and its metabolite GS-331007 in rat plasma was established. The analytes and the internal standard (midazolam) were separated on an Acquity UPLC BEH C18 chromatography column (2.1mm×50mm, 1.7μm) using gradient elution with a mobile phase of acetonitrile and 0.1% formic acid in water at a flow rate of 0.4mL/min. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) mode to monitor the precursor-to-product ion transitions of m/z 245.1→113.1 for ribavirin, m/z 530.3→243.1 for sofosbuvir, m/z 261.5→113.1 for GS-331007 and m/z 326.2→291.1 for midazolam (IS) using a positive electrospray ionization interface. The method was validated over a concentration range of 5-1000ng/mL for ribavirin, 10-2000ng/mL for sofosbuvir and 10-2000ng/mL for GS-331007. Total time for each chromatograph was 3.0min. The intra- and inter-day precision and accuracy of the quality control samples at low, medium, and high concentration levels exhibited relative standard deviations (RSD) <10.0% and the accuracy values ranged from -10.6% to 11.6%. The method was successfully applied to a pharmacokinetic study of ribavirin, sofosbuvir and GS-331007 in rats.

  10. Stability-Indicating UPLC Method for Tramadol HCl Impurities in the Tramadol Injection after Dilution by Infusion Fluids (5% Dextrose and 0.9% Sodium Chloride)

    PubMed Central

    Binnor, Anil K.; Mukkanti, Khagga; Suryanarayana, Mulukutla V.; Roy, Sunilendu B.

    2013-01-01

    A novel, rapid, and sensitive ultra-performance liquid chromatography (UPLC) method has been developed and validated as per ICH guidelines for the determination of tramadol HCl impurities in the tramadol HCl injection after reconstitution by infusion fluids (5% dextrose and 0.9% sodium chloride). The tramadol HCl injection is for the treatment of patients with moderate-to-severe pain. The stability of the reconstituted solution is critical before intravenous injection. The literature search resulted in few published articles on assays of tramadol in infusion fluids by conventional HPLC. No attempts have yet been made to determine the impurities in infusion fluids, as the concentration of tramadol after reconstitution is extremely low (0.4 mg/mL) and that of impurities is even lower. The proposed method is novel as it allows the quantitation of the impurities of tramadol HCl and is based on modern chromatographic techniques like UPLC. The method was developed using the Waters Acquity BEH C18 column with a mobile phase consisting of a gradient mixture of solvent A (trifluroacetic acid buffer) and solvent B (methanol: acetonitrile). The model stability study was designed by diluting the tramadol HCl injection in the 5% dextrose injection and 0.9% sodium chloride injection. Each mixture was kept under storage at room temperature (25 ± 2°C) for testing at initial, 2, 4, 8, 12, 18 & 24 hours. The validation study illustrates that the proposed method is suitable for the determination of tramadol and its impurities. The proposed method makes use of the LC-MS-compatible mobile phase. It can be useful for the determination of tramadol HCl and its impurities in plasma samples and other pharmaceutical dosage forms. PMID:24482769

  11. Simultaneous determination of nintedanib and its metabolite BIBF 1202 in different tissues of mice by UPLC-MS/MS and its application in drug tissue distribution study.

    PubMed

    Xu, Xiao-wei; Su, Xin-juan; Zhang, Yu-niao; Zheng, Xiao-kang; Lv, Peng-fei; Hu, Jie

    2015-10-01

    A sensitive and rapid ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed to simultaneous determine nintedanib and BIBF 1202 in mice plasma and tissue using carbamazepine as the internal standard (IS). Sample preparation was accomplished through a protein precipitation procedure with acetonitrile. The analyte and IS were separated on an Acquity UPLC BEH C18 column (2.1mm×50mm, 1.7μm) with the mobile phase of acetonitrile and 0.1% formic acid in water with gradient elution at a flow rate of 0.40mL/min. The detection was performed on a triple quadrupole tandem mass spectrometer equipped with electrospray ionization (ESI) by multiple reactions monitoring (MRM) of the transitions at m/z 540.3→113.1 for nintedanib, m/z 526.3→113.1 for BIBF 1202 and m/z 237.1→194.1 for IS, respectively. The linearity of this method was found to be within the concentration range of 1-1000ng/mL with a lower limit of quantification of 1.0ng/mL for each drug. Only 3.0min was needed for an analytical run. The inter-day and intra-day precision and accuracy of quality control (QC) samples, evaluated both in plasma and tissue homogenates, were all within 15%. The method was successfully applied to the pharmacokinetic and tissue distribution study of nintedanib and BIBF 1202 in mice after oral administration of nintedanib.

  12. [UPLC-MS/MS determination of content of three iridoids of xingnaojing oral preparation in rat brains and study on their brain pharmacokinetics].

    PubMed

    Xu, Pan; Du, Shou-Ying; Lu, Yang; Bai, Jie; Liu, Hui-Min; Du, Qiu; Chen, Zhen-Zhen; Wang, Zhen

    2014-06-01

    To establish a UPLC-MS/MS method for the simultaneous determination of geniposide, genipin 1-O-beta-D-gentiobioside and geniposidic acid in rat brains and study the brain pharmacokinetics of the three iridoid glycosides in stroke rat after the oral administration of Xingnaojing. In this experiment, brain samples were precipitated with protein for twice. Acquity BEH C18 column was adopted, with acetonitrile-0.1% formic acid-water as the mobile phase for gradient elution. ESI source was adopted for mass spectra; multiple reaction monitoring (MRM) was conducted to detect negative ions. The time for sample analysis was 3.5 min. the results showed good linear relations among the three iridoid glycosides, with the extraction recovery between 99.6% and 114.3%, good intra- and inter-day precisions and accuracies and stability in line with the requirements. The t1/2 and MRT in the three components were similar in brains of stroke rats. Geniposide and genipin 1-O-beta-D-gentiobioside showed double peaks; where as geniposidic acid showed a single peak. In conclusion, the method is so specific, sensitive, accurate and reliable that it can be used to study the brain pharmacokinetics of Xingnaojing oral preparation.

  13. Determination of Pinaverium Bromide in Human Plasma by a Sensitive and Robust UPLC-MS-MS Method and Application to a Pharmacokinetic Study in Mexican Subjects.

    PubMed

    Patiño-Rodríguez, Omar; Zapata-Morales, Juan Ramón; Escobedo-Moratilla, Abraham; Díaz de León-Cabrero, Manuel; Torres-Roque, Irma; Pérez-Urizar, José

    2015-09-01

    A high-throughput ultra-performance liquid chromatography coupled to tandem mass spectrometry (LC-ESI-MS-MS) method was developed for the determination of pinaverium bromide in human plasma. Protein precipitation with acetonitrile was used to extract pinaverium and itraconazole (as internal standard) from 500 µL plasma samples. The chromatographic separation was achieved with an Acquity UPLC BEH C18 column (1.7 µm, 2.1 × 100 mm) using a mixture of acetonitrile-5 mM ammonium formate (80:20, v/v) as mobile phase. Isocratic elution at 0.3 mL/min was used. Detection was performed by positive ion electrospray tandem mass spectrometry on a XEVO TQ-S by multiple reaction monitoring mode. The mass transitions monitorized were as follows: m/z 511.2 → 230 for pinaverium bromide, and m/z 705.29 → 392.18 for the itraconazole. The method was validated over a concentration range of 12-12,000 pg/mL. The chromatographic method runtime is 2.5 min and was applied to characterize the pharmacokinetics of pinaverium bromide after the oral administration of 100 mg to healthy Mexican subjects. PMID:25862744

  14. A fast, sensitive, and high throughput method for the determination of cefuroxime lysine in dog plasma by UPLC-MS/MS.

    PubMed

    Zhao, Longshan; Zhao, Yunli; Li, Qing; Chen, Xiaohui; Xiao, Feng; He, Bosai; Wang, Jie; Bi, Kaishun

    2012-01-30

    In order to investigate the preclinical pharmacokinetics of cefuroxime lysine, a fast, sensitive and high throughput UPLC-ESI-MS/MS method has been developed and validated for the quantitative determination of cefuroxime in dog plasma. Cefuroxime and IS phenacetin were extracted from plasma samples by PPT or LLE procedure, and then separated on an ACQUITY UPLC™ BEH C(18) column with an isocratic elution of acetonitrile-0.1% formic acid in 10mM ammonium acetate (40:60, v/v). MRM using the fragmentation transitions of m/z 442 → 364 and 180 → 110 in positive ESI mode was performed to quantify cefuroxime and IS, respectively. The calibration curves were linear over the concentration range of 2-400 μg/ml for PPT and 0.01-5 μg/ml for LLE. The LLOQ was 0.01 μg/ml. The intra- and inter-day precisions in all samples were no more than 8.1%, while the accuracy was within ± 6.2% of nominal values. The method was successfully applied to the evaluation of pharmacokinetic parameters of cefuroxime lysine in beagle dogs.

  15. Quantification of sofosbuvir and ledipasvir in human plasma by UPLC-MS/MS method: Application to fasting and fed bioequivalence studies.

    PubMed

    Rezk, Mamdouh R; Bendas, Ehab R; Basalious, Emad B; Karim, Iman A

    2016-08-15

    A rapid and sensitive LC-MS/MS method was developed, optimized and validated for quantification of sofosbuvir (SF) and ledipasvir (LD) in human plasma using eplerenone as an internal standard (IS). Analytes and IS were extracted from plasma by simple liquid-liquid extraction technique using methyl tertiary butyl ether. The prepared samples were chromatographed on Acquity UPLC BEH C18 column. Separation was done using a mobile phase formed of 0.1% formic acid and acetonitrile (50:50, v/v) in an isocratic mode at a flow rate of 0.4ml/min. The Xevo TQD LC-MS/MS was operated under the multiple-reaction monitoring mode using electrospray ionization. A full validation of the method was performed according to the FDA guidelines. Linearity was found to be in the range of 0.25-3500ng/ml for SF and 5-2000ng/ml for LD. The intra-day and inter-day precision and accuracy results were within the acceptable limits. A short run time of 2min allows analysis of more than 400 plasma samples per day. The developed method was successfully applied to both fasting and fed bioequivalence studies in healthy human volunteers. PMID:27322631

  16. Development of a sensitive UPLC-ESI-MS/MS method for quantification of sofosbuvir and its metabolite, GS-331007, in human plasma: Application to a bioequivalence study.

    PubMed

    Rezk, Mamdouh R; Basalious, Emad B; Karim, Iman A

    2015-10-10

    A rapid and simple LC-MS/MS method was developed and validated for the simultaneous estimation of sofosbuvir (SF) and its metabolite GS-331007 (GS) using famotidine as an internal standard (IS). The Xevo TQD LC-MS/MS was operated under the multiple-reaction monitoring mode using electrospray ionization. Extraction with ethyl acetate was used in sample preparation. The prepared samples were chromatographed on Acquity UPLC HSS C₁₈ (50 mm × 2.1 mm, 1.8 μm) column by pumping 0.1% formic acid and acetonitrile (50:50, v/v) in an isocratic mode at a flow rate of 0.3 ml/min. Method validation was performed as per the FDA guidelines and the standard curves were found to be linear in the range of 10-2500 ng/ml for both SF and its metabolite. The intra-day and inter-day precision and accuracy results were within the acceptable limits. A very short run time of 1.2 min made it possible to analyze more than 300 human plasma samples per day. The developed assay method was successfully applied to a bioequivalence study in human volunteers.

  17. Analytical Method for the Identification and Assay of Kojic Acid, Methylparaben, and Propylparaben in Cosmetic Products Using UPLC: Application of ISO 12787:2011 Standard.

    PubMed

    Qadir, Muhammad Abdul; Ahmed, Mahmood; Shafiq, Muhammad Imtiaz; Ali, Amir; Sadiq, Asma

    2016-09-01

    A straightforward, fast UPLC method is developed for the identification and quantification of kojic acid (KA), methylparaben (MP), and propylparaben (PP) in 15 cosmetic products (skin whitening creams and lotions). Chromatographic separations for KA, MP, and PP were obtained in 3.5 min on an Acquity BEH-C18 column (100 × 2.1 mm, 1.7 μm particle size) as the stationary phase at 260 nm (diode-array detector), with the mobile phase comprising a mixture of 0.01 M dibasic potassium phosphate and methanol-acetonitrile (50 + 50). Validation studies were performed according to in-house established criteria. There was a linear function of concentrations over the range of 0.4-1.6 μg/mL for KA, MP, and PP. The LOQ for all components was 0.2 μg/mL using the S/N method. Good separation of analytes was observed, with acceptable values of resolution and tailing. The analytical approach defined in the ISO 12787:2011 standard ("Cosmetics-Analytical methods-Validation criteria for analytical results using chromatographic techniques") was used for the assay of cosmetic samples. PMID:27329740

  18. Determination of Pinaverium Bromide in Human Plasma by a Sensitive and Robust UPLC-MS-MS Method and Application to a Pharmacokinetic Study in Mexican Subjects.

    PubMed

    Patiño-Rodríguez, Omar; Zapata-Morales, Juan Ramón; Escobedo-Moratilla, Abraham; Díaz de León-Cabrero, Manuel; Torres-Roque, Irma; Pérez-Urizar, José

    2015-09-01

    A high-throughput ultra-performance liquid chromatography coupled to tandem mass spectrometry (LC-ESI-MS-MS) method was developed for the determination of pinaverium bromide in human plasma. Protein precipitation with acetonitrile was used to extract pinaverium and itraconazole (as internal standard) from 500 µL plasma samples. The chromatographic separation was achieved with an Acquity UPLC BEH C18 column (1.7 µm, 2.1 × 100 mm) using a mixture of acetonitrile-5 mM ammonium formate (80:20, v/v) as mobile phase. Isocratic elution at 0.3 mL/min was used. Detection was performed by positive ion electrospray tandem mass spectrometry on a XEVO TQ-S by multiple reaction monitoring mode. The mass transitions monitorized were as follows: m/z 511.2 → 230 for pinaverium bromide, and m/z 705.29 → 392.18 for the itraconazole. The method was validated over a concentration range of 12-12,000 pg/mL. The chromatographic method runtime is 2.5 min and was applied to characterize the pharmacokinetics of pinaverium bromide after the oral administration of 100 mg to healthy Mexican subjects.

  19. Development and validation of a UPLC-MS/MS method for the determination of 7-hydroxymitragynine, a μ-opioid agonist, in rat plasma and its application to a pharmacokinetic study.

    PubMed

    Vuppala, Pradeep K; Jamalapuram, Seshulatha; Furr, Edward B; McCurdy, Christopher R; Avery, Bonnie A

    2013-12-01

    A simple, sensitive and specific ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated to determine the concentrations of 7-hydroxymitragynine in rat plasma. Following a single-step liquid-liquid extraction of plasma samples using chloroform, 7-hydroxymitragynine and the internal standard (tryptoline) were separated on an Acquity UPLC(TM) BEH C18 (1.7 µm, 2.1 × 50 mm) column using an isocratic elution at a flow rate of 0.2 mL/min. The mobile phase consisted of 0.1% acetic acid in water and 0.1% acetic acid in acetonitrile (10:90, v/v). The run time was 2.5 min. The analysis was carried out under the multiple reaction-monitoring mode using positive electrospray ionization. Protonated ions [M + H](+) and their respective product ions were monitored at the following transitions: 415 → 190 for 7-hydroxymitragynine and 173 → 144 for the internal standard. The calibration curve was linear over the range of 10-4000 ng/mL (r(2) = 0.999) with a lower limit of quantification of 10 ng/mL. The extraction recoveries ranged from 62.0 to 67.3% at concentrations of 20, 600 and 3200 ng/mL). Intra- and inter-day assay precisions (relative standard deviation) were <15% and the accuracy was within 96.5-104.0%. This validated method was successfully applied to quantify 7-hydroxymitragynine in rat plasma following intravenous administration. PMID:23893615

  20. Simultaneous determination of paeoniflorin, albiflorin, ferulic acid, tetrahydropalmatine, protopine, typhaneoside, senkyunolide I in Beagle dogs plasma by UPLC-MS/MS and its application to a pharmacokinetic study after Oral Administration of Shaofu Zhuyu Decoction.

    PubMed

    Huang, Xiaochen; Su, Shulan; Cui, Wenxia; Liu, Pei; Duan, Jin-ao; Guo, Jianming; Li, Zhenhao; Shang, Erxin; Qian, Dawei; Huang, Zhijun

    2014-07-01

    In this present study, a sensitive and rapid UPLC-MS/MS method was developed for simultaneous quantification of paeoniflorin, albiflorin, ferulic acid, tetrahydropalmatine, protopine, typhaneoside and senkyunolide I in Beagle dog plasma after oral administration of the Shao-Fu-Zhu-Yu Decoction. Chloramphenicol and clarithromycin were used as internal standards. Plasma samples were processed by protein precipitation with methanol. The separation was performed on an Acquity BEH C18 column (100mm×2.1mm, 1.7μm) at a flow-rate of 0.4mL/min, using 0.1% formic acid-acetonitrile as mobile phase. Method validation was performed as per Food and Drug Administration guidelines and the results met the acceptance criteria. After validation, this method was successfully applied to a pharmacokinetic study. The results showed that the apparent plasma clearance of paeoniflorin, albiflorin, typhaneoside and senkyunolide I were significantly higher than others. Double peak was observed in plasma concentration curves of tetrahydropalmatine, the ferulic acid had a good absorption in Beagle dog plasma, and senkyunolide I was detected in plasma from the first blood sampling time (15min) and rapidly reached Tmax. The compound of typhaneoside has a low bioavailability according to the results. PMID:24907546

  1. Determination of newly synthesized lipoic acid-niacin dimer in rat plasma by UPLC/electrospray ionization tandem mass spectrometry: assay development, validation and application to a pharmacokinetic study.

    PubMed

    Chen, Xiao; Gao, Jingwen; Jiang, Yiming; Huang, Ping; Xie, Yuhui; Pi, Rongbiao; Zhu, Shuzhen; Yao, Meicun

    2014-02-01

    A simple, sensitive and specific ultra-performance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS) method was developed to determine the newly synthesized compound lipoic acid-niacin dimer (N2L) in plasma. Plasma samples were precipitated by methanol using tetrahydropalmatine as internal standard. Chromatographic separation was achieved on an Acquity BEH C18 (2.1 × 50 mm i.d., 1.7 µm) column; the mobile phase contains methanol and buffer solution (water with 0.5% formic acid and 10 mmol/L ammonium acetate). Multiple reaction monitoring (m/z 353.9 → 148.6 for N2L and m/z 356.0 → 192.0 for internal standard) was performed for detection and quantification. The method was validated to be rapid, specific, accurate and precise over the concentration range of 1-750 ng/mL; N2L was not stable on the bench-top or during freeze-freeze-thaw cycles in plasma, but was stable in the stock solution and after preparation in the autosampler for 24 h. The utility of the assay was confirmed by pharmacokinetic study of N2L in rats.

  2. Validation and application of an UPLC-MS/MS method for the quantification of synthetic cannabinoids in urine samples and analysis of seized materials from the Portuguese market.

    PubMed

    Simões, Susana Sadler; Silva, Inês; Ajenjo, Antonio Castañera; Dias, Mário João

    2014-10-01

    An UPLC-MS/MS method using ESI+ionization and MRM was developed and fully validated according to international guidelines for the qualitative and quantitative analysis of nine synthetic cannabinoids and/or their metabolites in urine samples (1mL). Prior to extraction the samples were subjected to an enzymatic hydrolysis using β-glucuronidase followed by a SPE procedure using Oasis(®) HLB 3cc (60mg) columns. The chromatographic separation was performed with an Acquity UPLC(®) HSS T3 (50mm×2.1mm i.d., 1.8μm) reversed-phase column using a gradient with methanol-ammonium formate 2mM (0.1% formic acid) and with a run time of 9.5min. The method was validated in terms of selectivity, capacity of identification, limits of detection (0.01-0.5ng/mL) and quantification (0.05-0.5ng/mL), recovery (58-105%), carryover, matrix effect, linearity (0.05-50ng/mL), intra-assay precision, inter-assay accuracy and precision (CV<20%). The method was applied to 80 authentic samples, five of them (6.2%) were confirmed or suspected to be positive for the metabolites JWH-018 N-hydroxypentyl and JWH-018 N-pentanoic acid of JWH-018 and for the metabolite JWH-122 N-(5-hydroxypentyl) of JWH-122, and three of them in association with THC and/or THCCOOH (substances included in the method, together with the 11-OH-THC). Additionally, 17 spice products were analyzed, for which were confirmed the presence of the following substances: AM-2201, JWH-018, JWH-022 JWH-073, JWH-122, JWH-203, JWH-210, JWH-250, HU-210 and RCS-4, according to the comparison with authentic reference material and published data. The analytical method developed allowed the analysis of synthetic cannabinoids and the notification of the first cases in Portugal. PMID:25127518

  3. Simultaneous Determination of Bosentan, Glimepiride, HYBOS and M1 in Rat Plasma by UPLC-MS-MS and its Application to Pharmacokinetic Study.

    PubMed

    Chen, Mengchun; Song, Wenjie; Wang, Shuanghu; Chen, Qiulei; Pan, Peipei; Xu, Tao; Hu, Guoxin; Zheng, Zhiqiang

    2016-08-01

    A rapid and sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method for the simultaneous determination of bosentan (BOS), glimepiride (GLP), hydroxyl bosentan (HYBOS) and hydroxyl glimepiride (M1) in rat plasma using one-step protein precipitation was developed and validated. After addition of ambrisentan as an internal standard (IS), protein precipitation by acetonitrile was used in sample preparation. Chromatographic separation was achieved on a Waters ACQUITY UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm particle size, Waters Corp., Milford, MA, USA) and inline 0.2 μm stainless steel frit filter (Waters Corp.) with acetonitrile-0.1% formic acid as the mobile phase at a flow rate of 0.4 mL/min with gradient elution. The column temperature was maintained at 40°C. Only 4 min was needed for an analytical run. The retention times were ∼3.29 min for BOS, 3.56 min for GLP, 1.42 min for HYBOS, 1.53 min for M1 and 3.22 min for IS. Electrospray ionization source was employed and operated in positive-ion mode; multiple reaction monitoring mode was applied to target fragment ions m/z 552 → 202, m/z 568 → 202, m/z 491 → 352, m/z 507 → 352 and m/z 379 → 347 for BOS, HYBOS, GLP, M1 and IS, respectively. The assay was validated over concentration ranges of 25-5,000 ng/mL (r(2) = 0.9984) for BOS, 1-200 ng/mL (r(2) = 0.9999) for GLP, 0.5-100 ng/mL (r(2) = 0.9999) for HYBOS and 0.1-20 ng/mL (r(2) = 0.9984) for M1. Intra- and interday precision values for replicate quality control samples were within 14.2% for all analytes during the assay validation. Mean quality control accuracy values were within -3.3 to 14.4% of nominal values for all analytes. The mean recoveries of BOS, GLP, HYBOS, M1 and ambrisentan from the plasma exceeded 90.4%. The analytes were stable in rat plasma for at least 2 h at room temperature, 30 days at -40°C and following at least three freeze-thaw cycles (-40°C to room temperature). This method was

  4. Validation and application of an UPLC-MS/MS method for the quantification of synthetic cannabinoids in urine samples and analysis of seized materials from the Portuguese market.

    PubMed

    Simões, Susana Sadler; Silva, Inês; Ajenjo, Antonio Castañera; Dias, Mário João

    2014-10-01

    An UPLC-MS/MS method using ESI+ionization and MRM was developed and fully validated according to international guidelines for the qualitative and quantitative analysis of nine synthetic cannabinoids and/or their metabolites in urine samples (1mL). Prior to extraction the samples were subjected to an enzymatic hydrolysis using β-glucuronidase followed by a SPE procedure using Oasis(®) HLB 3cc (60mg) columns. The chromatographic separation was performed with an Acquity UPLC(®) HSS T3 (50mm×2.1mm i.d., 1.8μm) reversed-phase column using a gradient with methanol-ammonium formate 2mM (0.1% formic acid) and with a run time of 9.5min. The method was validated in terms of selectivity, capacity of identification, limits of detection (0.01-0.5ng/mL) and quantification (0.05-0.5ng/mL), recovery (58-105%), carryover, matrix effect, linearity (0.05-50ng/mL), intra-assay precision, inter-assay accuracy and precision (CV<20%). The method was applied to 80 authentic samples, five of them (6.2%) were confirmed or suspected to be positive for the metabolites JWH-018 N-hydroxypentyl and JWH-018 N-pentanoic acid of JWH-018 and for the metabolite JWH-122 N-(5-hydroxypentyl) of JWH-122, and three of them in association with THC and/or THCCOOH (substances included in the method, together with the 11-OH-THC). Additionally, 17 spice products were analyzed, for which were confirmed the presence of the following substances: AM-2201, JWH-018, JWH-022 JWH-073, JWH-122, JWH-203, JWH-210, JWH-250, HU-210 and RCS-4, according to the comparison with authentic reference material and published data. The analytical method developed allowed the analysis of synthetic cannabinoids and the notification of the first cases in Portugal.

  5. Simultaneous Determination of L-tetrahydropalmatine and Cocaine in Human Plasma by Simple UPLC-FLD Method: Application in Clinical Studies

    PubMed Central

    Yu, Mingming; Hassan, Hazem E.; Ibrahim, Ahmed; Bauer, Kenneth S.; Kelly, Deanna L.; Wang, Jia Bei

    2014-01-01

    Currently, there are no FDA approved medications for treatment of cocaine addiction underscoring the dire need to develop such a product. There is an accumulating body of evidence that L-tetrahydropalmatine (L-THP), a non-selective dopamine antagonist, can be used for the treatment of cocaine addiction. Indeed, the FDA recently approved its usage in a Phase I study in cocaine abusers and it was indispensable to develop a simple and sensitive method for the simultaneous determination of L-THP and cocaine in human plasma. We developed a UPLC-FLD method for quantitation of these molecules using an ACQUITY BEH C18 column (2.1 × 50mm, 1.7um) and a mobile phase that consisted of 5 mM ammonium phosphate (PH=4.75), methanol, and acetonitrile (v:v:v, 78:16:6). Venlafaxine was used as the internal standard while hexane was used for the liquid-liquid extraction. The flow rate was 0.4ml/min with fluorescence detection using an excitation wavelength of 230nm and emission detection wavelength of 315nm. This method was selective, linear and sensitive with a lower limit of quantification of 2.5 ng/mL for both cocaine and L-THP. The intra-day precision of cocaine and L-THP was <9.50% while the accuracy was <4.29%. The inter-day precision of cocaine and L-THP was <9.14%, and the accuracy was <12.49%. The recovery for cocaine and L-THP ranged from (43.95 - 50.02%) and (54.65 - 58.31%), respectively. In comparison to forty reported cocaine quantitation methods this method is simple, sensitive and cost-effective and can be used for simultaneous quantitation of L-THP and cocaine. This method meets the FDA guidelines and can be used in current and future clinical studies. PMID:24996068

  6. A novel stability-indicating UPLC method development and validation for the determination of seven impurities in various diclofenac pharmaceutical dosage forms.

    PubMed

    Azougagh, M; Elkarbane, M; Bakhous, K; Issmaili, S; Skalli, A; Iben Moussad, S; Benaji, B

    2016-09-01

    An innovative simple, fast, precise and accurate ultra-high performance liquid chromatography (UPLC) method was developed for the determination of diclofenac (Dic) along with its impurities including the new dimer impurity in various pharmaceutical dosage forms. An Acquity HSS T3 (C18, 100×2.1mm, 1.8μm) column in gradient mode was used with mobile phase comprising of phosphoric acid, which has a pH value of 2.3 and methanol. The flow rate and the injection volume were set at 0.35ml·min(-1) and 1μl, respectively, and the UV detection was carried out at 254nm by using photodiode array detector. Dic was subjected to stress conditions from acid, base, hydrolytic, thermal, oxidative and photolytic degradation. The new developed method was successfully validated in accordance to the International Conference on Harmonization (ICH) guidelines with respect to specificity, limit of detection, limit of quantitation, precision, linearity, accuracy and robustness. The degradation products were well resolved from main peak and its seven impurities, proving the specificity power of the method. The method showed good linearity with consistent recoveries for Dic content and its impurities. The relative percentage of standard deviation obtained for the repeatability and intermediate precision experiments was less than 3% and LOQ was less than 0.5μg·ml(-1) for all compounds. The new proposed method was found to be accurate, precise, specific, linear and robust. In addition, the method was successfully applied for the assay determination of Dic and its impurities in the several pharmaceutical dosage forms. PMID:27475309

  7. UPLC-MS-MS method for simultaneous determination of caffeine, tolbutamide, metoprolol, and dapsone in rat plasma and its application to cytochrome P450 activity study in rats.

    PubMed

    Liu, Yan; Li, Xiang; Yang, Chunjuan; Tai, Sheng; Zhang, Xiangning; Liu, Gaofeng

    2013-01-01

    A specific ultra-performance liquid chromatography tandem mass spectrometry method has been described for the simultaneous determination of caffeine, tolbutamide, metoprolol and dapsone in rat plasma, which are the four probe drugs of the four cytochrome P450 (CYP450) isoforms CYP1A2, CYP2C9, CYP2D6 and CYP3A4. The chromatographic separation was achieved using a Waters Acquity UPLC BEH HILIC C(18) column (2.1 × 50 mm, 1.7 µm). The mobile phase consisted of acetonitrile and water (containing 0.1% formic acid) (15:85, v/v). The triple quadrupole mass spectrometric detection was operated by positive electrospray ionization. Phenacetin was chosen as internal standard. Plasma samples were extracted with dichloromethane-butanol (10:1, v/v). The recoveries ranged from 67.5% to 98.5%. The calibration curves in plasma were linear in the range of 2.5-1,000 ng/mL for caffeine and dapsone, 5-5,000 ng/mL for tolbutamide and 2.5-250 ng/mLfor metoprolol, with correlation coefficient (r(2)) of 0.9936, 0.9966, 0.9990 and 0.9998, respectively. The method was successfully applied to pharmacokinetic studies of the four probe drugs of the four CYP450 isoforms and used to evaluate the effects of breviscapine on the activities of CYP1A2, CYP2C9, CYP2D6 and CYP3A4 in rats.

  8. A New Method to Quantify Ifosfamide Blood Levels Using Dried Blood Spots and UPLC-MS/MS in Paediatric Patients with Embryonic Solid Tumours.

    PubMed

    Torres, Luz-María; Rivera-Espinosa, Liliana; Chávez-Pacheco, Juan L; Navas, Carlos F; Demetrio, Joel A; Alemón-Medina, Radamés; Trujillo, Francisca; Pérez, Martín; Zapata, Martha M; Cárdenas, Rocío; Salinas, Citlaltepetl; Aquino, Arnoldo; Velázquez-Cruz, Rafael; Castillejos, Manuel-de-Jesús

    2015-01-01

    Ifosfamide blood concentrations are necessary to monitor its therapeutic response, avoiding any adverse effect. We developed and validated an analytical method by UPLC-MS/MS to quantify ifosfamide in dried blood spots (DBS). Blood samples were collected on Whatman 903® filter paper cards. Five 3 mm disks were punched out from each dried blood spot. Acetonitrile and ethyl acetate were used for drug extraction. Chromatographic separation was carried out in an Acquity UPLC equipment with a BEH-C18 column, 2.1 x 100 mm, 1.7 μm (Waters®). The mobile phase consisted in 5 mM ammonium formate and methanol:acetonitrile (40:48:12 v/v/v) at 0.2 mL/min. LC-MS/MS detection was done by ESI+ and multiple reaction mode monitoring, ionic transitions were m/z1+ 260.99 > 91.63 for ifosfamide and 261.00 > 139.90 for cyclophosphamide (internal standard). This method was linear within a 100-10000 ng/mL range and it was accurate, precise and selective. Ifosfamide samples in DBS were stable for up to 52 days at -80°C. The procedure was tested in 14 patients, ages 1 month to 17 years (9 males and 5 females), with embryonic tumours treated with ifosfamide, alone or combined, at a public tertiary referral hospital. Ifosfamide blood levels ranged from 11.1 to 39.7 μmol/L at 12 hours after the last infusion, while 24-hour levels ranged from 0.7-19.7 μmol/L. The median at 12 hours was 19.5 μmol/L (Q25 14.4-Q75 29.0) and 3.8 μmol/L (Q25 1.5-Q75 9.9) at 24 hours, p<0.001. This method is feasible to determine ifosfamide plasma levels in paediatric patients.

  9. A New Method to Quantify Ifosfamide Blood Levels Using Dried Blood Spots and UPLC-MS/MS in Paediatric Patients with Embryonic Solid Tumours

    PubMed Central

    Chávez-Pacheco, Juan L.; Navas, Carlos F.; Demetrio, Joel A.; Alemón-Medina, Radamés; Trujillo, Francisca; Pérez, Martín; Zapata, Martha M.; Cárdenas, Rocío; Salinas, Citlaltepetl; Aquino, Arnoldo; Velázquez-Cruz, Rafael; Castillejos, Manuel-de-Jesús

    2015-01-01

    Ifosfamide blood concentrations are necessary to monitor its therapeutic response, avoiding any adverse effect. We developed and validated an analytical method by UPLC-MS/MS to quantify ifosfamide in dried blood spots (DBS). Blood samples were collected on Whatman 903® filter paper cards. Five 3 mm disks were punched out from each dried blood spot. Acetonitrile and ethyl acetate were used for drug extraction. Chromatographic separation was carried out in an Acquity UPLC equipment with a BEH-C18 column, 2.1 x 100 mm, 1.7 μm (Waters®). The mobile phase consisted in 5 mM ammonium formate and methanol:acetonitrile (40:48:12 v/v/v) at 0.2 mL/min. LC-MS/MS detection was done by ESI+ and multiple reaction mode monitoring, ionic transitions were m/z1+ 260.99 > 91.63 for ifosfamide and 261.00 > 139.90 for cyclophosphamide (internal standard). This method was linear within a 100–10000 ng/mL range and it was accurate, precise and selective. Ifosfamide samples in DBS were stable for up to 52 days at -80°C. The procedure was tested in 14 patients, ages 1 month to 17 years (9 males and 5 females), with embryonic tumours treated with ifosfamide, alone or combined, at a public tertiary referral hospital. Ifosfamide blood levels ranged from 11.1 to 39.7 μmol/L at 12 hours after the last infusion, while 24-hour levels ranged from 0.7–19.7 μmol/L. The median at 12 hours was 19.5 μmol/L (Q25 14.4–Q75 29.0) and 3.8 μmol/L (Q25 1.5–Q75 9.9) at 24 hours, p<0.001. This method is feasible to determine ifosfamide plasma levels in paediatric patients. PMID:26600181

  10. Development and validation of an UPLC-MS/MS assay for quantitative analysis of the ghrelin receptor inverse agonist PF-5190457 in human or rat plasma and rat brain.

    PubMed

    Ghareeb, Mwlod; Leggio, Lorenzo; El-Kattan, Ayman; Akhlaghi, Fatemeh

    2015-07-01

    PF-5190457 is a ghrelin receptor inverse agonist that is currently undergoing clinical development for the treatment of alcoholism. Our aim was to develop and validate a simple and sensitive assay for quantitative analysis of PF-5190457 in human or rat plasma and rat brain using liquid chromatography-tandem mass spectrometry. The analyte and stable isotope internal standard were extracted from 50 μL plasma or rat brain homogenate by protein precipitation using 0.1% formic acid in acetonitrile. Chromatography was carried out on an Acquity UPLC BEH C18 (2.1 mm × 50 mm) column with 1.7 μm particle size and 130 Å pore size. The flow rate was 0.5 mL/min and total chromatographic run time was 2.2 min. The mobile phase consisted of a gradient mixture of water: acetonitrile 95:5% (v/v) containing 0.1% formic acid (solvent A) and 100% acetonitrile containing 0.1% formic acid (solvent B). Multiple reaction monitoring was carried out in positive electro-spray ionization mode using m/z 513.35 → 209.30 for PF-5190457 and m/z 518.47 → 214.43 for the internal standard. The recovery ranged from 102 to 118% with coefficient of variation (CV) less than 6% for all matrices. The calibration curves for all matrices were linear over the studied concentration range (R(2) ≥ 0.998, n = 3). The lower limit of quantification was 1 ng/mL in rat or human plasma and 0.75 ng/g in rat brain. Intra- and inter-run mean percent accuracies were between 85 and 115% and percent imprecision was ≤15%. The assays were successfully utilized to measure the concentration of PF-5190457 in pre-clinical and clinical pharmacology studies of the compound.

  11. Preclinical pharmacokinetics, tissue distribution and excretion studies of a novel anti-candidal agent-thiosemicarbazide derivative of isoniazid (TSC-INH) by validated UPLC-MS/MS assay.

    PubMed

    Iqbal, Muzaffar; Ezzeldin, Essam; Bhat, Mashooq A; Raish, Mohammad; Al-Rashood, Khalid A

    2016-01-01

    A simple and sensitive UPLC-MS/MS assay was developed and validated for rapid determination of thiosemicarbazide derivative of isoniazid (TSC-INH), a potent anti-candidal agent in rat plasma, tissues, urine and feces. All biological samples were prepared by protein precipitation method using celecoxib as an internal standard (IS). Chromatographic separation was achieved on Acquity BEH™ C18 (50×2.1 mm, 1.7 μm) column using gradient mobile phase of acetonitrile and water (containing 0.1% formic acid) at flow rate of 0.3 mL/min. The MRM transitions were monitored at m/z 305.00→135.89 for TSC-INH and m/z 380.08→316.03 for IS in ESI negative mode. All validation parameter results were within the acceptable range described in guideline for bioanalytical method validation. The pharmacokinetic study showed that the compound TSC-INH was orally active with 66% absolute bioavailability in rats. It was rapidly absorbed with peak plasma concentration of 1985.92 ng/mL achieved within 1 h after single oral dose (10 mg/kg) administration. TSC-INH exhibited rapid distribution across the body with highest levels in liver and lungs. Penetration in brain tissues suggests that TSC-INH crossed the blood brain barrier. Only 5.23% of the orally administered drug was excreted as unconverted form in urine and feces implying that TSC-INH was metabolized extensively before excretion. With the preliminary knowledge of in vivo pharmacokinetics and disposition properties, this study will be beneficial for further development of compound TSC-INH in future studies.

  12. Development and validation of an UPLC-MS/MS method for the determination of 7-hydroxymitragynine, a μ-opioid agonist, in rat plasma and its application to a pharmacokinetic study

    PubMed Central

    Vuppala, Pradeep K.; Jamalapuram, Seshulatha; Furr, Edward B.; McCurdy, Christopher R.; Avery, Bonnie A.

    2014-01-01

    A simple, sensitive and specific ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method has been developed and validated to determine the concentrations of 7-hydroxymitragynine in rat plasma. Following a single step liquid-liquid extraction of plasma samples using chloroform, 7-hydroxymitragynine and the internal standard (tryptoline) were separated on an Acquity UPLC™ BEH C18 (1.7 μm, 2.1 mm×50 mm) column using an isocratic elution at a flow rate of 0.2 mL/min. The mobile phase consisted of 0.1% acetic acid in water and 0.1% acetic acid in acetonitrile (10:90, v/v). The run was 2.5 min. The analysis was carried out under the multiple reaction-monitoring mode using positive electrospray ionization. Protonated ions [M+H]+ and their respective product ions were monitored at the following transitions: 415>190 for 7-hydroxymitragynine and 173>144 for the internal standard. The calibration curve was linear over the range of 10 to 4000 ng/mL (r2=0.999) with a lower limit of quantification (LLOQ) of 10 ng/mL. The extraction recoveries ranged from 62.0% to 67.3% at concentrations (20, 600, 3200 ng/mL). Intra- and inter-day assay precisions (relative standard deviation) were less than 15% and the accuracy was within 96.5% to 104.0%. This validated method was successfully applied to quantify 7-hydroxymitragynine in rat plasma following intravenous administration. PMID:23893615

  13. Development of RP UPLC-TOF/MS, stability indicating method for omeprazole and its related substances by applying two level factorial design; and identification and synthesis of non-pharmacopoeial impurities.

    PubMed

    Jadhav, Sushant Bhimrao; Kumar, C Kiran; Bandichhor, Rakeshwar; Bhosale, P N

    2016-01-25

    A new UPLC-TOF/MS compatible, reverse phase-stability indicating method was developed for determination of Omeprazole (OMP) and its related substances in pharmaceutical dosage forms by implementing Design of Experiment (DoE) i.e. two level full factorial Design (2(3)+3 center points=11 experiments) to understand the Critical Method Parameters (CMP) and its relation with Critical Method Attribute (CMA); to ensure robustness of the method. The separation of eleven specified impurities including conversion product of OMP related compound F (13) and G (14) i.e. Impurity-I (1), OMP related compound-I (11) and OMP 4-chloro analog (12) was achieved in a single method on Acquity BEH shield RP18 100 × 2.1 mm, 1.7 μm column, with inlet filter (0.2 μm) using gradient elution and detector wavelength at 305 nm and validated in accordance with ICH guidelines and found to be accurate, precise, reproducible, robust and specific. The drug was found to degrade extensively in heat, humidity and acidic conditions and forms unknown degradation products during stability studies. The same method was used for LC-MS analysis to identify m/z and fragmentation of maximum unknown impurities (Non-Pharmacopoeial) i.e. Impurity-I (1), Impurity-III (3), Impurity-V (5) and Impurity-VIII (9) formed during stability studies. Based on the results, degradation pathway for the drug has been proposed and synthesis of identified impurities i.e. impurities (Impurity-I (1), Impurity-III (3), Impurity-V (5) and Impurity-VIII (9)) are discussed in detail to ensure in-depth understanding of OMP and its related impurities and optimum performance during lifetime of the product. PMID:26600119

  14. Development of RP UPLC-TOF/MS, stability indicating method for omeprazole and its related substances by applying two level factorial design; and identification and synthesis of non-pharmacopoeial impurities.

    PubMed

    Jadhav, Sushant Bhimrao; Kumar, C Kiran; Bandichhor, Rakeshwar; Bhosale, P N

    2016-01-25

    A new UPLC-TOF/MS compatible, reverse phase-stability indicating method was developed for determination of Omeprazole (OMP) and its related substances in pharmaceutical dosage forms by implementing Design of Experiment (DoE) i.e. two level full factorial Design (2(3)+3 center points=11 experiments) to understand the Critical Method Parameters (CMP) and its relation with Critical Method Attribute (CMA); to ensure robustness of the method. The separation of eleven specified impurities including conversion product of OMP related compound F (13) and G (14) i.e. Impurity-I (1), OMP related compound-I (11) and OMP 4-chloro analog (12) was achieved in a single method on Acquity BEH shield RP18 100 × 2.1 mm, 1.7 μm column, with inlet filter (0.2 μm) using gradient elution and detector wavelength at 305 nm and validated in accordance with ICH guidelines and found to be accurate, precise, reproducible, robust and specific. The drug was found to degrade extensively in heat, humidity and acidic conditions and forms unknown degradation products during stability studies. The same method was used for LC-MS analysis to identify m/z and fragmentation of maximum unknown impurities (Non-Pharmacopoeial) i.e. Impurity-I (1), Impurity-III (3), Impurity-V (5) and Impurity-VIII (9) formed during stability studies. Based on the results, degradation pathway for the drug has been proposed and synthesis of identified impurities i.e. impurities (Impurity-I (1), Impurity-III (3), Impurity-V (5) and Impurity-VIII (9)) are discussed in detail to ensure in-depth understanding of OMP and its related impurities and optimum performance during lifetime of the product.

  15. Screening β1AR inhibitors by cell membrane chromatography and offline UPLC/MS method for protecting myocardial ischemia.

    PubMed

    Yue, Yuan; Dou, Lili; Wang, Xin; Xue, Hui; Song, Yanhong; Li, Xiaoni

    2015-11-10

    A high expression β1AR/cell membrane chromatography (β1AR-CMC) and offline UPLC/MS method has been developed for screening active ingredients from Coptis chinensis. In this study, the fractions retained by CMC column were separated and identified by UPLC/MS system. Using metoprolol as a positive control drug, coptisine from C. chinensis was identified as the active component which could inhibit β1AR. Compared with the control group: coptisine could attenuate the infarct size and release malondialdehyde (MDA) while increasing superoxide dismutase (SOD) activity, suggesting a role in reducing myocardial injury. In vitro, coptisine could decrease apoptosis, showing their protective effects upon cardiomyocytes. This β1AR-CMC-offline-UPLC/MS method can be applied for screening active components acting on β1AR from traditional Chinese medicines. PMID:26263062

  16. UPLC: a preeminent technique in pharmaceutical analysis.

    PubMed

    Kumar, Ashok; Saini, Gautam; Nair, Anroop; Sharma, Rishbha

    2012-01-01

    The pharmaceutical companies today are driven to create novel and more efficient tools to discover, develop, deliver and monitor the drugs. In this contest the development of rapid chromatographic method is crucial for the analytical laboratories. In precedent decade, substantial technological advances have been done in enhancing particle chemistry performance, improving detector design and in optimizing the system, data processors and various controls of chromatographic techniques. When all was blended together, it resulted in the outstanding performance via ultra-high performance liquid chromatography (UPLC), which holds back the principle of HPLC technique. UPLC shows a dramatic enhancement in speed, resolution as well as the sensitivity of analysis by using particle size less than 2 pm and the system is operational at higher pressure, while the mobile phase could be able to run at greater linear velocities as compared to HPLC. This technique is considered as a new focal point in field of liquid chromatographic studies. This review focuses on the basic principle, instrumentation of UPLC and its advantages over HPLC, furthermore, this article emphasizes various pharmaceutical applications of this technique.

  17. A New UPLC Approach for the Simultaneous Quantitative Estimation of Four Compounds in a Cough Syrup Formulation.

    PubMed

    Turak, Fatma; Güzel, Remziye; Dinç, Erdal

    2016-01-01

    A new ultra-performance liquid chromatographic (UPLC) method was developed for the simultaneous estimation of potassium guaiacolsulfonate (PGS), guaifenesin (GUA), diphenhydramine HCl (DIP) and carbepentane citrate (CAR) in a commercial cough syrup. The chromatographic separation of four compounds PGS, GUA, DIP and CAR was performed on a BEH phenyl column (100 × 2.1 mm, 1.7 µm i.d.) using a mobile phase consisting of acetonitrile and 0.1 M HCl (50 : 50, v/v). In addition, the optimized conditions of the chromatographic analysis were found with the flow rate of 0.38 mL/min, the column temperature of 30°C and the injection volume of 1.2 µL with the photodiode array detection of 220 nm. Calibration curves in the concentration ranges of 10-98 µg/mL for PGS, 5-80 µg/mL for GUA, 5-25 µg/mL for DIP and CAR were computed by the regression of the analyte concentration on the chromatographic peak area. The newly developed UPLC method was validated by analyzing the quaternary mixtures of the related compounds, intraday and interday experiment and standard addition samples. After method validation, the proposed UPLC approach was successfully applied for the analysis of the commercial syrup formulation containing PGS, GUA, DIP and CAR compounds. PMID:26202585

  18. [Simultaneous determination of 11 mycotoxins in malt by isotope internal standard-UPLC-MS/MS].

    PubMed

    Wang, Sha; Kong, Wei-jun; Yang, Mei-hua

    2016-01-01

    A suitable ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of 11 mycotoxins with isotope internal standard in malt. The mycotoxins in malt were extracted and purified by one-step ultrasonic extraction procedure using acetonitrile/water/acetic acid (80 : 19 : 1), and then detected and confirmed by UPLC-MS/MS, and quantified by isotope labeled AFB1 ([13C17]-AFB1) and ZEN ([13C18]-ZEN) internal standards. Rapid separation of the 11 mycotoxins was successfully achieved on a Phenomenex Kinetex C18 column (100 mm x 2.1 mm, 2.6 μm) with gradient elution using the mobile phase of methanol containing 0.1% formic acid and 2 mmol x L(-1) ammonium acetate in water. Simultaneous acquisition was performed in multiple reaction monitoring (MRM) mode with electrospray ionization (ESI) source operated in both positive and negative ionization modes. The established method provided a good linearity for the 11 mycotoxins within their respective linear ranges with correlation coefficients all higher than 0.999 1. The average recoveries ranged from 75.0% to 117.0% with relative standard deviations (RSDs) below 5.1%. The limits of detection (LODs) and quantitation (LOQs) ranged from 0.05 to 30 μg x kg(-1) and 0.15 to 87.5 μg x kg(-1), respectively, which were below the maximum residue levels (MRLs) set by the European Union. Twenty malt samples were analyzed and nine samples were detected with mycotoxins, which were confirmed according to the same fragment ions found in positive samples and the standards at the same retention time. This study has demonstrated that the one-step extraction procedure of mycotoxins from complex matrices coupled to UPLC-MS/MS method is simple, quick, accurate and sensitive for quantitative and qualitative analysis of multiple mycotoxins in malt. PMID:27405171

  19. [Simultaneous determination of 11 mycotoxins in malt by isotope internal standard-UPLC-MS/MS].

    PubMed

    Wang, Sha; Kong, Wei-jun; Yang, Mei-hua

    2016-01-01

    A suitable ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of 11 mycotoxins with isotope internal standard in malt. The mycotoxins in malt were extracted and purified by one-step ultrasonic extraction procedure using acetonitrile/water/acetic acid (80 : 19 : 1), and then detected and confirmed by UPLC-MS/MS, and quantified by isotope labeled AFB1 ([13C17]-AFB1) and ZEN ([13C18]-ZEN) internal standards. Rapid separation of the 11 mycotoxins was successfully achieved on a Phenomenex Kinetex C18 column (100 mm x 2.1 mm, 2.6 μm) with gradient elution using the mobile phase of methanol containing 0.1% formic acid and 2 mmol x L(-1) ammonium acetate in water. Simultaneous acquisition was performed in multiple reaction monitoring (MRM) mode with electrospray ionization (ESI) source operated in both positive and negative ionization modes. The established method provided a good linearity for the 11 mycotoxins within their respective linear ranges with correlation coefficients all higher than 0.999 1. The average recoveries ranged from 75.0% to 117.0% with relative standard deviations (RSDs) below 5.1%. The limits of detection (LODs) and quantitation (LOQs) ranged from 0.05 to 30 μg x kg(-1) and 0.15 to 87.5 μg x kg(-1), respectively, which were below the maximum residue levels (MRLs) set by the European Union. Twenty malt samples were analyzed and nine samples were detected with mycotoxins, which were confirmed according to the same fragment ions found in positive samples and the standards at the same retention time. This study has demonstrated that the one-step extraction procedure of mycotoxins from complex matrices coupled to UPLC-MS/MS method is simple, quick, accurate and sensitive for quantitative and qualitative analysis of multiple mycotoxins in malt.

  20. Pharmacokinetic study of indocyanine Green after intravenous administration by UPLC-MS/MS.

    PubMed

    Chen, Yu; Chen, Dongxin; Hu, Wenhao; Lin, Guanyang; Huang, Shiyong

    2015-01-01

    Indocyanine Green is widely used in medical diagnosis and to evaluate liver function and other regional blood flows in clinical application or animal experiments. In this work, a sensitive and selective ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for determination of Indocyanine Green in rat plasma was developed and validated. After addition of rutin as an internal standard (IS), protein precipitation by acetonitrile-methanol (9:1, v/v) was used to prepare samples. Chromatographic separation was achieved on a UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm) with 0.1% formic acid and acetonitrile as the mobile phase with gradient elution. An electrospray ionization source was applied and operated in positive ion mode; multiple reactions monitoring (MRM) mode was used for quantification using target fragment ions m/z 753.4→330.2 for Indocyanine Green, and m/z 611.1→303.1 for IS. Calibration plots were linear throughout the range 20-5000 ng/mL for Indocyanine Green in rat plasma. Mean recoveries of Indocyanine Green in rat plasma ranged from 79.5% to 85.4%. RSD of intra-day and inter-day precision were both < 12%. The accuracy of the method was between 95.9% and 113.9%. The method was successfully applied to pharmacokinetic study of Indocyanine Green after intravenous administration.

  1. Analysis of phenolic compounds in Matricaria chamomilla and its extracts by UPLC-UV.

    PubMed

    Haghi, G; Hatami, A; Safaei, A; Mehran, M

    2014-01-01

    Chamomile (Matricaria chamomilla L.) is a widely used medicinal plant possessing several pharmacological effects due to presence of active compounds. This study describes a method of using ultra performance liquid chromatography (UPLC) coupled with photodiode array (PDA) detector for the separation of phenolic compounds in M. chamomilla and its crude extracts. Separation was conducted on C18 column (150 mm × 2 mm, 1.8 μm) using a gradient elution with a mobile phase consisting of acetonitrile and 4% aqueous acetic acid at 25°C. The method proposed was validated for determination of free and total apigenin and apigenin 7-glucoside contents as bioactive compounds in the extracts by testing sensitivity, linearity, precision and recovery. In general, UPLC produced significant improvements in method sensitivity, speed and resolution. Extraction was performed with methanol, 70% aqueous ethanol and water solvents. Total phenolic and total flavonoid contents ranged from 1.77 to 50.75 gram (g) of gallic acid equivalent (GAE)/100 g and 0.82 to 36.75 g quercetin equivalent (QE)/100 g in dry material, respectively. There was a considerable difference from 40 to 740 mg/100 g for apigenin and 210 to 1110 mg/100 g for apigenin 7-glucoside in dry material. PMID:25598797

  2. UPLC and HPLC of caffeoyl esters in wild and cultivated Arctium lappa L.

    PubMed

    Haghi, Ghasem; Hatami, Alireza; Mehran, Mehdi

    2013-05-01

    Analytical methods including ultra-performance liquid chromatography (UPLC) and high-performance liquid chromatography (HPLC) with photodiode array (PDA) detector were developed for the analysis of caffeoylquinic acid derivatives in seeds, leaves and roots of Arctium lappa L. Separation was performed on C(18) column utilising 5% (v/v) acetic acid in water and acetonitrile at 330 nm. Both methodologies were validated in terms of linearity, precision, and recovery. The results showed that the major advantages of UPLC, over HPLC were the fast analysis, narrow peaks, high sensitivity, and reduction of solvent consumption. Subsequently the methods were applied for the identification and quantification of chlorogenic acid (5-CQA) and 1,5-dicaffeoylquinic acid (1,5-DCQA) as main compounds in samples. The total phenolic content of samples ranged from 3.93 to 14.13 g of 5-CQA equivalent/100g dry weight (DW). There was a significant variability from 89 to 571 mg/100g for 5-CQA and 48 to 486 mg/100g for 1,5-DCQA in dry material.

  3. UPLC and HPLC of caffeoyl esters in wild and cultivated Arctium lappa L.

    PubMed

    Haghi, Ghasem; Hatami, Alireza; Mehran, Mehdi

    2013-05-01

    Analytical methods including ultra-performance liquid chromatography (UPLC) and high-performance liquid chromatography (HPLC) with photodiode array (PDA) detector were developed for the analysis of caffeoylquinic acid derivatives in seeds, leaves and roots of Arctium lappa L. Separation was performed on C(18) column utilising 5% (v/v) acetic acid in water and acetonitrile at 330 nm. Both methodologies were validated in terms of linearity, precision, and recovery. The results showed that the major advantages of UPLC, over HPLC were the fast analysis, narrow peaks, high sensitivity, and reduction of solvent consumption. Subsequently the methods were applied for the identification and quantification of chlorogenic acid (5-CQA) and 1,5-dicaffeoylquinic acid (1,5-DCQA) as main compounds in samples. The total phenolic content of samples ranged from 3.93 to 14.13 g of 5-CQA equivalent/100g dry weight (DW). There was a significant variability from 89 to 571 mg/100g for 5-CQA and 48 to 486 mg/100g for 1,5-DCQA in dry material. PMID:23265494

  4. Pharmacokinetic study of indocyanine Green after intravenous administration by UPLC-MS/MS

    PubMed Central

    Chen, Yu; Chen, Dongxin; Hu, Wenhao; Lin, Guanyang; Huang, Shiyong

    2015-01-01

    Indocyanine Green is widely used in medical diagnosis and to evaluate liver function and other regional blood flows in clinical application or animal experiments. In this work, a sensitive and selective ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for determination of Indocyanine Green in rat plasma was developed and validated. After addition of rutin as an internal standard (IS), protein precipitation by acetonitrile-methanol (9:1, v/v) was used to prepare samples. Chromatographic separation was achieved on a UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm) with 0.1% formic acid and acetonitrile as the mobile phase with gradient elution. An electrospray ionization source was applied and operated in positive ion mode; multiple reactions monitoring (MRM) mode was used for quantification using target fragment ions m/z 753.4→330.2 for Indocyanine Green, and m/z 611.1→303.1 for IS. Calibration plots were linear throughout the range 20-5000 ng/mL for Indocyanine Green in rat plasma. Mean recoveries of Indocyanine Green in rat plasma ranged from 79.5% to 85.4%. RSD of intra-day and inter-day precision were both < 12%. The accuracy of the method was between 95.9% and 113.9%. The method was successfully applied to pharmacokinetic study of Indocyanine Green after intravenous administration. PMID:26629038

  5. Pharmacokinetic and bioavailability study of angeloylgomisin H in rat plasma by UPLC-MS/MS.

    PubMed

    Chen, Shanjiang; Jia, Zhuyin; Dong, Ledan; Geng, Peiwu; Liu, Zezheng; Yang, Suping; Wen, Congcong; Liu, Fuli

    2015-01-01

    Angeloylgomisin H, as a major lignin in the fruits, was reported to have the potential to improve insulin-stimulated glucose uptake by activating PPAR-γ. In this work, a sensitive and selective UPLC-MS/MS method for determination of angeloylgomisin H in rat plasma is developed. After addition of rutin as an internal standard (IS), protein precipitation by acetonitrile was used to prepare samples. Chromatographic separation was achieved on a UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm) with 0.1% formic acid and acetonitrile as the mobile phase with gradient elution. An electrospray ionization source was applied and operated in positive ion mode; multiple reactions monitoring (MRM) mode was used for quantification using target fragment ions m/z 523.2-315.1 for angeloylgomisin H, and m/z 611.1-303.1 for IS. Calibration plots were linear throughout the range 5-2000 ng/mL for angeloylgomisin H in rat plasma. Mean recoveries of angeloylgomisin H in rat plasma ranged from 86.2% to 92.5%. RSD of intra-day and inter-day precision were both < 11%. The accuracy of the method was between 93.0% and 104.1%. The method was successfully applied to pharmacokinetic study of angeloylgomisin H after either oral or intravenous administration. The absolute bioavailability of angeloylgomisin H was reported as high as 4.9%.

  6. Profiling the Oxylipin and Endocannabinoid Metabolome by UPLC-ESI-MS/MS in Human Plasma to Monitor Postprandial Inflammation.

    PubMed

    Gouveia-Figueira, Sandra; Späth, Jana; Zivkovic, Angela M; Nording, Malin L

    2015-01-01

    Bioactive lipids, including oxylipins, endocannabinoids, and related compounds may function as specific biochemical markers of certain aspects of inflammation. However, the postprandial responsiveness of these compounds is largely unknown; therefore, changes in the circulating oxylipin and endocannabinoid metabolome in response to a challenge meal were investigated at six occasions in a subject who freely modified her usual diet. The dietary change, and especially the challenge meal itself, represented a modification of precursor fatty acid status, with expectedly subtle effects on bioactive lipid levels. To detect even the slightest alteration, highly sensitive ultra-performance liquid chromatography (UPLC) coupled to electrospray ionization (ESI) tandem mass spectrometry (MS/MS) methods for bioactive lipid profiling was employed. A previously validated UPLC-ESI-MS/MS method for profiling the endocannabinoid metabolome was used, while validation of an UPLC-ESI-MS/MS method for oxylipin analysis was performed with acceptable outcomes for a majority of the parameters according to the US Food and Drug Administration guidelines for linearity (0.9938 < R2 < 0.9996), limit of detection (0.0005-2.1 pg on column), limit of quantification (0.0005-4.2 pg on column), inter- and intraday accuracy (85-115%) and precision (< 5%), recovery (40-109%) and stability (40-105%). Forty-seven of fifty-two bioactive lipids were detected in plasma samples at fasting and in the postprandial state (0.5, 1, and 3 hours after the meal). Multivariate analysis showed a significant shift of bioactive lipid profiles in the postprandial state due to inclusion of dairy products in the diet, which was in line with univariate analysis revealing seven compounds (NAGly, 9-HODE, 13-oxo-ODE, 9(10)-EpOME, 12(13)-EpOME, 20-HETE, and 11,12-DHET) that were significantly different between background diets in the postprandial state (but not at fasting). The only change in baseline levels at fasting was

  7. Development and validation of a UPLC method for rapid and simultaneous analysis of proton pump inhibitors.

    PubMed

    Addo, Richard T; Davis, Kenneth; Ubale, Ruhi; Owen, Joel S; Watkins, E Blake

    2015-02-01

    Proton pump inhibitors (PPIs) are used extensively for the relief of gastroesophageal reflux, peptic ulcers, and other hypersecretory conditions. Some of the commonly used PPIs-omeprazole, esomeprazole, lansoprazole, pantoprazole, and rabeprazole-were used in this study with the aim of developing a rapid ultra performance liquid chromatography (UPLC) method for detecting each and allowing separation and quantification of a mixture of PPIs. An analysis of samples was performed on a UPLC system equipped with a quaternary solvent delivery system, a refrigerated sample manager, a column heater, a photo diode array detector scanning from 210 to 400 nm, and a C18 analytical column (50 mm × 3.0 mm, 1.7-μm particle size). The chromatographic analysis of the PPI samples and standards was performed using gradient elution with acetonitrile and water. The calibration curve range varied for each of the PPIs ranging from a lower limit of 0.75-1.78 μg/mL to a maximum concentration of 200 μg/mL with a regression coefficient (r (2)) of ≥0.98. The accuracy and precision were calculated, and the %RSD was determined to be ≤0.21% (intraday) and ≤5% (interday). The LOD was 0.23-0.59 μg/mL and the LOQ was 0.71-1.78 μg/mL for each of the drugs analyzed. The method was capable of detecting and quantifying each drug in a mixture with good resolution and a total run time of less than 5 min. Herein, we report an efficient and rapid analytical method for the simultaneous detection of multiple PPIs in a mixture. PMID:25160675

  8. PULSE COLUMN

    DOEpatents

    Grimmett, E.S.

    1964-01-01

    This patent covers a continuous countercurrent liquidsolids contactor column having a number of contactor states each comprising a perforated plate, a layer of balls, and a downcomer tube; a liquid-pulsing piston; and a solids discharger formed of a conical section at the bottom of the column, and a tubular extension on the lowest downcomer terminating in the conical section. Between the conical section and the downcomer extension is formed a small annular opening, through which solids fall coming through the perforated plate of the lowest contactor stage. This annular opening is small enough that the pressure drop thereacross is greater than the pressure drop upward through the lowest contactor stage. (AEC)

  9. A Novel, Rapid, and Validated Stability-Indicating UPLC Method for the Estimation of Drotaverine Hydrochloride and Ibuprofen Impurities in Oral Solid Dosage Form

    PubMed Central

    Vijay Kumar, Rekulapally; Rao, Vinay U.; Anil Kumar, N.; Venkata Subbaiah, B.

    2015-01-01

    A novel, stability-indicating, reversed-phase ultra-performance liquid chromatographic (RP-UPLC) method was developed for the determination of pure drotaverine hydrochloride and ibuprofen in the presence of their impurities and degradation products. The method was developed using a Waters UPLC BEH C18, 100 × 2.1 mm, 1.7 µm column with a flow rate of 0.3 mL/min and detector wavelength at 210 nm. The mobile phase consisted of potassium dihydrogen orthophosphate buffer and acetonitrile. Drotaverine hydrochloride and ibuprofen were subjected to the stress conditions of oxidative, acid, base, photolytic, and thermal degradation. Degradation products resulting from the stress studies were well-resolved, thus confirming the test method as stability-indicating. Validation of the method was carried out as per International Conference on Harmonization guidelines. PMID:26839839

  10. Simultaneous Analysis of Cannabinoid and Synthetic Cannabinoids in Dietary Supplements Using UPLC with UV and UPLC-MS-MS.

    PubMed

    Heo, Seok; Yoo, Geum Joo; Choi, Ji Yeon; Park, Hyoung Joon; Do, Jung-Ah; Cho, Sooyeul; Baek, Sun Young; Park, Sung-Kwan

    2016-06-01

    The primary purpose of this study was to develop and validate a method based on UPLC with UV and UPLC-MS-MS for the simultaneous analysis of different cannabinoids and synthetic cannabinoids in food as well as in herbal and dietary supplements. The limits of detection and quantitation of the method ranged from 0.1 to 0.3 and 0.3 to 0.9 μg/mL by UPLC with UV, respectively. The coefficient of determination was >0.999; the intra- and interday precision of the method were 0.1-3.7 and 0.9-4.1%, respectively. The intra- and interday accuracy were 94.8-103.1 and 98.3-100.9%, respectively. The mean recoveries of nine cannabinoids obtained from tablet samples ranged from 81.1 to 105.4%. The mean extraction recoveries of nine target cannabinoids obtained from various types of samples (tablets, capsules, powders, liquids, cookies and candies) ranged from 82.26 to 112.40%. The relative standard deviation (RSD) of the stability of the prepared sample solutions was <1.80%. Identification and quantification of the nine cannabinoids were accomplished by ion spray UPLC-MS-MS using multiple reaction monitoring. The UPLC-MS-MS method was validated for linearity (R(2) > 0.99); the precision was 0.1-4.0% (intraday) and 0.1-2.8% (interday), and the accuracy was 98.0-103.5% (intraday) and 97.1-103.2% (interday). The mean extraction recoveries of six types of samples were 82.2-114.5% and the RSD of stability was <6.54%, complying with the established international guidelines. The results indicated that the method can be used for rapid and accurate screening of cannabinoids present in food.

  11. Simultaneous Analysis of Cannabinoid and Synthetic Cannabinoids in Dietary Supplements Using UPLC with UV and UPLC-MS-MS.

    PubMed

    Heo, Seok; Yoo, Geum Joo; Choi, Ji Yeon; Park, Hyoung Joon; Do, Jung-Ah; Cho, Sooyeul; Baek, Sun Young; Park, Sung-Kwan

    2016-06-01

    The primary purpose of this study was to develop and validate a method based on UPLC with UV and UPLC-MS-MS for the simultaneous analysis of different cannabinoids and synthetic cannabinoids in food as well as in herbal and dietary supplements. The limits of detection and quantitation of the method ranged from 0.1 to 0.3 and 0.3 to 0.9 μg/mL by UPLC with UV, respectively. The coefficient of determination was >0.999; the intra- and interday precision of the method were 0.1-3.7 and 0.9-4.1%, respectively. The intra- and interday accuracy were 94.8-103.1 and 98.3-100.9%, respectively. The mean recoveries of nine cannabinoids obtained from tablet samples ranged from 81.1 to 105.4%. The mean extraction recoveries of nine target cannabinoids obtained from various types of samples (tablets, capsules, powders, liquids, cookies and candies) ranged from 82.26 to 112.40%. The relative standard deviation (RSD) of the stability of the prepared sample solutions was <1.80%. Identification and quantification of the nine cannabinoids were accomplished by ion spray UPLC-MS-MS using multiple reaction monitoring. The UPLC-MS-MS method was validated for linearity (R(2) > 0.99); the precision was 0.1-4.0% (intraday) and 0.1-2.8% (interday), and the accuracy was 98.0-103.5% (intraday) and 97.1-103.2% (interday). The mean extraction recoveries of six types of samples were 82.2-114.5% and the RSD of stability was <6.54%, complying with the established international guidelines. The results indicated that the method can be used for rapid and accurate screening of cannabinoids present in food. PMID:27185817

  12. Column internals

    SciTech Connect

    Bravo, J.L.

    1998-02-01

    In the fields of distillation, absorption, stripping and extraction, theory and technology go hand in hand. The thermodynamic principles of phase equilibrium and the concepts of mass transfer and fluid flow are of primary importance in all of these operations. The engineer must understand these phenomena to select equipment effectively. This article discusses the latest in commercial technology in column internals for gas-liquid and liquid-liquid contacting. The principles of operation are explained vis-a-vis the characteristics of the applications in which they are used. The focus is on moderate-to-large columns for refining and chemical applications. Guidelines for selecting the most appropriate type of device are presented, and examples of typical applications are described.

  13. A validated stability-indicative UPLC method for nilotinib hydrochloride for the determination of process-related and degradation impurities.

    PubMed

    Kondra, Sudhakar Babu; Madireddy, Venkataramanna; Chilukuri, Mohanareddy; Papadasu, Narayanareddy; Jonnalagadda, Latha

    2014-09-01

    A novel stability-indicating ultra performance liquid chromatographic (UPLC) method has been developed for quantitative determination of nilotinib hydrochloride in active pharmaceutical ingredients along with four impurities (imp-1, imp-2, imp-3 and imp-4). The method is applicable to the quantification of related compounds and assay of nilotinib hydrochloride drug. Efficient chromatographic separation was achieved on a Shim-pack XR-ODS II, 75 × 3.0 mm, 1.8-µm column with a gradient mobile phase combination. Quantification was carried at 260 nm at a flow rate of 0.6 mL min(-1). Stress degradation conditions were established for nilotinib hydrochloride by subjecting it to acid, base, oxidation, humidity, thermal and photolysis. The stress samples were assayed against a qualified reference standard and the mass balance was found close to 97.0%. The developed UPLC method was validated according to the present International Conference on Harmonisation guidelines for specificity, detection limit, quantitation limit, linearity, accuracy, precision, intermediate precision and robustness. The resolution between nilotinib hydrochloride and four potential impurities is found to be >2.0. Regression analysis shows as r value (correlation coefficient) of >0.999 for nilotinib hydrochloride and four potential impurities.

  14. Pharmacokinetic properties of isorhamnetin, kaempferol and quercetin after oral gavage of total flavones of Hippophae rhamnoides L. in rats using a UPLC-MS method.

    PubMed

    Li, Guowen; Zeng, Xiaoli; Xie, Yan; Cai, Zhenzhen; Moore, Jeffrey C; Yuan, Xiurong; Cheng, Zhihong; Ji, Guang

    2012-01-01

    An ultra performance liquid chromatography-mass spectrometric (UPLC-MS) method was developed to investigate the pharmacokinetic properties of isorhamnetin, kaempferol and quercetin from a total flavone extract of Hippophae rhamnoides L. (TFH) after single dose oral administration. Rat plasma samples were pretreated using liquid-liquid extraction, and chromatographic separation was performed on a C(18) column using a linear gradient of methanol and formic acid (0.1%). The pharmacokinetic parameters of isorhamnetin, kaempferol and quercetin from TFH in rats were quantitatively determined by UPLC with photodiode array detection (PDA). The qualitative detection of the three flavones was accomplished by selected ion monitoring in negative ion mode ESI-MS. Results of the pharmacokinetic study indicate that the three flavones in TFH were absorbed by passive diffusion in rats, and no "double-peak" phenomenon was observed in C-t curves of the three flavones from TFH except for quercetin. Results of this study indicate that the pharmacokinetic behaviors of isorhamnetin, kaempferol and quercetin when administered together in a complex herbal extract might be different than the individual behaviors of the same compounds administered in their pure forms. Results of this study also demonstrate that UPLC-MS is a rapid and practical method to determine the pharmacokinetic parameters of flavones present in an herbal extract. PMID:22056665

  15. Profiling the Oxylipin and Endocannabinoid Metabolome by UPLC-ESI-MS/MS in Human Plasma to Monitor Postprandial Inflammation

    PubMed Central

    Gouveia-Figueira, Sandra; Späth, Jana; Zivkovic, Angela M.; Nording, Malin L.

    2015-01-01

    Bioactive lipids, including oxylipins, endocannabinoids, and related compounds may function as specific biochemical markers of certain aspects of inflammation. However, the postprandial responsiveness of these compounds is largely unknown; therefore, changes in the circulating oxylipin and endocannabinoid metabolome in response to a challenge meal were investigated at six occasions in a subject who freely modified her usual diet. The dietary change, and especially the challenge meal itself, represented a modification of precursor fatty acid status, with expectedly subtle effects on bioactive lipid levels. To detect even the slightest alteration, highly sensitive ultra-performance liquid chromatography (UPLC) coupled to electrospray ionization (ESI) tandem mass spectrometry (MS/MS) methods for bioactive lipid profiling was employed. A previously validated UPLC-ESI-MS/MS method for profiling the endocannabinoid metabolome was used, while validation of an UPLC-ESI-MS/MS method for oxylipin analysis was performed with acceptable outcomes for a majority of the parameters according to the US Food and Drug Administration guidelines for linearity (0.9938 < R2 < 0.9996), limit of detection (0.0005–2.1 pg on column), limit of quantification (0.0005–4.2 pg on column), inter- and intraday accuracy (85–115%) and precision (< 5%), recovery (40–109%) and stability (40–105%). Forty-seven of fifty-two bioactive lipids were detected in plasma samples at fasting and in the postprandial state (0.5, 1, and 3 hours after the meal). Multivariate analysis showed a significant shift of bioactive lipid profiles in the postprandial state due to inclusion of dairy products in the diet, which was in line with univariate analysis revealing seven compounds (NAGly, 9-HODE, 13-oxo-ODE, 9(10)-EpOME, 12(13)-EpOME, 20-HETE, and 11,12-DHET) that were significantly different between background diets in the postprandial state (but not at fasting). The only change in baseline levels at fasting

  16. Development and Validation of a Stability-Indicating RP-UPLC Method for the Estimation of Impurities in Cinacalcet Hydrochloride API and its Formulation.

    PubMed

    Sunil Reddy, Pingili; Raju, Thummala Veera Raghava; Raju, Penmetsa Satyanarayana; Varma, Nadimpalli Sunil; Babu, Kondra Sudhakar

    2015-01-01

    A sensitive, stability-indicating, gradient reversed-phase ultra-performance liquid chromatography method has been developed for the quantitative estimation of cinacalcet hydrochloride impurities in active pharmaceutical ingredients and pharmaceutical formulations. Efficient chromatographic separation was achieved on an Acquity BEH Shield RP18, 100 × 2.1 mm, 1.7 µm column with the mobile phase containing pH 6.6 phosphate buffer and acetonitrile. The flow rate of the mobile phase was 0.3 mL min(-1) with a column temperature of 35°C and detection wavelength at 223 nm. The relative response factor values of (+)-R-1-(1-Naphthyl)ethylamine, regioisomer, diastereomer isomer-1, and diastereomer isomer-2 were 1.79, 0.99, 0.89, and 0.88, respectively. The cinacalcet hydrochloride formulation sample was subjected to the stress conditions of acid, base, oxidative, hydrolytic, thermal, humidity, and photolytic degradation. Cinacalcet hydrochloride was found to degrade significantly under the peroxide stress conditions. The degradation products were well-resolved from cinacalcet hydrochloride and its impurities. The peak purity test results confirmed that the cinacalcet hydrochloride peak was homogenous in all stress samples and the mass balance was found to be more than 96%, thus proving the stability-indicating power of the method. The developed method was validated according to ICH guidelines. PMID:26839840

  17. Simultaneous determination of six constituents in Mahuang Fuzi Xixin by UPLC-PDA-MS/MS.

    PubMed

    Zhang, Lin; Wang, Chengying; Miao, Dezu; Yuan, Dan; Bi, Kaishun; Yang, Jingyu; Zhan, Libin

    2015-01-01

    Mahuang Fuzi Xixin (MFX), a classic recipe in traditional Chinese medicine, belongs to an exterior-relieving formula. For quality control of the MFX products, qualitative analysis using ultra-high performance liquid chromatography with diode-array detector-tandem mass spectrometry (UPLC-PDA-MS/MS) was undertaken. Six compounds from the MFX were simultaneously detected. Among them, astragalin and kaempferol 3-rutinoside were quantified through the UPLC-MS/MS method, while asarinin, sesamin, kakuol and methyleugenol were quantified through the UPLC-PDA method. This method can be applied to the quantitative determination of the six compounds in the MFX. PMID:25428280

  18. Effect of the pressure on pre-column sample dispersion theory, experiments, and practical consequences.

    PubMed

    Gritti, Fabrice; Guiochon, Georges

    2014-07-25

    The effect of the pressure on the dispersion of a low molecular weight compound along 0.508 and 1.016 mm i.d. × 50 cm long open circular tubes was investigated theoretically and experimentally. The theoretical predictions were based on the early models of dispersion derived by Aris and Taylor (1953) and on the approximate model of Alizadeh for the time moments (1980). Experimentally, the system pressure was increased at constant flow rate (0.15 mL/min) from less than 20 to nearly 1,000 bar by using a series of capillary tubes (25 μm i.d. PEEKSIL tubes) of increasing flow resistances placed upstream the detection cell of a commercial very high pressure liquid chromatograph (vHPLC) but downstream the 50 cm long tube. Theoretical and experimental results agree that the peak variance increases linearly with increasing pressure in the tube volume. The relative increase of the peak variance is 7% above that measured at low pressure (<20 bar) for each 100 bar increment in the tube volume. This result confirms that accurate measurements of the column efficiency corrected for extra-column contribution cannot be made by replacing the column with a zero dead volume union connector, because the pressures applied in the pre-column volume are significantly different in these two cases. This work shows also that increasing the pressure in the pre-column volume by increasing the flow rate affects the apparent column efficiency that is measured, independently of the direct effect of the flow rate. For a 2.1 × 50mm column packed with 1.3 μm core-shell particles run with a classic Acquity system, the associated relative decreases of the column efficiency are expected to be -30%, -20%, and -5% for retention factors of 1, 3, and 10, respectively. The column HETP is no longer independent of its length.

  19. Development and validation of UPLC method for quality control of Curcuma longa Linn.: Fast simultaneous quantitation of three curcuminoids.

    PubMed

    Cheng, Jin; Weijun, Kong; Yun, Luo; Jiabo, Wang; Haitao, Wang; Qingmiao, Li; Xiaohe, Xiao

    2010-09-21

    A new reversed phase ultra performance liquid chromatography (UPLC) method was developed for the rapid quantification of three curcuminoids (curcumin (C), desmethoxycurcumin (DMC) and bisdesmethoxycurcumin (BDMC)) in Curcuma longa Linn. (C. longa) using a Waters BEH Shield RP C(18), 2.1 mm x 100 mm, 1.7 microm column. The runtime was 2 min. The influence of column temperature and mobile phase on resolution was investigated. The method was validated according to the ICH guideline for validation of analytical procedures with respect to precision, accuracy, and linearity. The limits of detection were 40.66, 49.38 and 29.28 pg for C, DMC and BDMC, respectively. Limits of quantitation for C, DMC and BDMC, were 134.18, 164.44 and 97.50 pg, respectively. Linear range was from 3.28 to 46.08 microg/ml. The mean+/-SD percent recoveries of curcuminoids were 99.47+/-1.66, 99.50+/-1.99 and 97.77+/-2.37 of C, DMC and BDMC, respectively. Comparison of system performance with conventional HPLC was made with respect to analysis time, efficiency and sensitivity. The proposed method was found to be reproducible and convenient for quantitative analysis of three curcuminoids in C. longa. This work provided some references for quality control of C. longa. PMID:20395103

  20. Rapid analysis of lignans from leaves of Podophyllum peltatum L. samples using UPLC-UV-MS.

    PubMed

    Avula, Bharathi; Wang, Yan-Hong; Moraes, Rita M; Khan, Ikhlas A

    2011-11-01

    A new rapid UPLC-UV-MS method has been developed that permits the analysis of four lignans (4'-O-demethylpodophyllotoxin, podophyllotoxin, α-peltatin and β-peltatin) in P. peltatum L. Podophyllotoxin is a natural lignan that is being used as a precursor for the semi-synthetic anti-cancer drugs etoposide, teniposide and etopophos. The chromatographic separation was achieved using a reversed-phase C18 column with a mobile phase of water and acetonitrile, both containing 0.05% formic acid. Analyses of P. peltatum leaves collected from different colonies within a single site indicated a significant variation in 4'-O-demethylpodophyllotoxin, α-peltatin, podophyllotoxin and β-peltatin content. Within 3.0 min four main lignans could be separated with detection limits of 0.1, 0.3, 0.3 and 0.2 μg/mL, respectively. 4'-O-demethylpodophyllotoxin and α-peltatin appeared most prominently among the lignans obtained. The podophyllotoxin content was found in the range of 0.004-0.77% from 16 samples collected from 6 colonies within the same site. The content of podophyllotoxin is directly proportional to the content of 4'-O-demethylpodophyllotoxin and inversely proportional to α-peltatin and β-peltatin content. LC-mass spectrometry coupled with electrospray ionization (ESI) interface method is described for the identification of four lignans in various populations of plant samples. By applying principal component analysis and hierarchical cluster analysis, Podophyllum samples collected from various colonies within a location were distinguished.

  1. Enhanced lipid isomer separation in human plasma using reversed-phase UPLC with ion-mobility/high-resolution MS detection[S

    PubMed Central

    Damen, Carola W. N.; Isaac, Giorgis; Langridge, James; Hankemeier, Thomas; Vreeken, Rob J.

    2014-01-01

    An ultraperformance LC (UPLC) method for the separation of different lipid molecular species and lipid isomers using a stationary phase incorporating charged surface hybrid (CSH) technology is described. The resulting enhanced separation possibilities of the method are demonstrated using standards and human plasma extracts. Lipids were extracted from human plasma samples with the Bligh and Dyer method. Separation of lipids was achieved on a 100 × 2.1 mm inner diameter CSH C18 column using gradient elution with aqueous-acetonitrile-isopropanol mobile phases containing 10 mM ammonium formate/0.1% formic acid buffers at a flow rate of 0.4 ml/min. A UPLC run time of 20 min was routinely used, and a shorter method with a 10 min run time is also described. The method shows extremely stable retention times when human plasma extracts and a variety of biofluids or tissues are analyzed [intra-assay relative standard deviation (RSD) <0.385% and <0.451% for 20 and 10 min gradients, respectively (n = 5); interassay RSD <0.673% and <0.763% for 20 and 10 min gradients, respectively (n = 30)]. The UPLC system was coupled to a hybrid quadrupole orthogonal acceleration time-of-flight mass spectrometer, equipped with a traveling wave ion-mobility cell. Besides demonstrating the separation for different lipids using the chromatographic method, we demonstrate the use of the ion-mobility MS platform for the structural elucidation of lipids. The method can now be used to elucidate structures of a wide variety of lipids in biological samples of different matrices. PMID:24891331

  2. Identification of ginsenoside markers from dry purified extract of Panax ginseng by a dereplication approach and UPLC-QTOF/MS analysis.

    PubMed

    Yang, Heejung; Lee, Dong Young; Kang, Kyo Bin; Kim, Jeom Yong; Kim, Sun Ok; Yoo, Young Hyo; Sung, Sang Hyun

    2015-05-10

    A dry purified extract of Panax ginseng (PEG) was prepared using a manufacturing process that includes column chromatography, acid hydrolysis, and an enzyme reaction. During the manufacturing process, the more polar ginsenosides were altered into less polar forms via cleavage of their sugar chains and structural modifications of the aglycones, such as hydroxylation and dehydroxylation. The structural changes of ginsenosides during the intermediate steps from dried ginseng extract (DGE) to PEG were monitored by ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectroscopy (UPLC-QTOF/MS). 22 ginsenosides isolated from PEG were used as the reference standards for determining of unknown ginsenosides and further suggesting of the metabolic markers. The elution order of 22 ginsenosides based on the type of aglycones, and the location and number of sugar chains can be used for the structural elucidation of unknown ginsenosides. This information could be used in a dereplication process for quick and efficient identification of ginsenoside derivatives in ginseng preparations. A dereplication approach helped the identification of the metabolic markers in the UPLC-QTOF/MS chromatograms during the conversion process with multivariate analyses, including principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) plots. These metabolic markers were identified by comparing with the dereplication information of the reference standards of 22 ginsenosides, or they were assigned using the pattern of the MS/MS fragmented ions. Consequently, the developed metabolic profiling approach using UPLC-QTOF/MS and multivariate analysis represents a new method for providing quality control as well as useful criteria for a similarity evaluation of the manufacturing process of ginseng preparations.

  3. Development and validation of a sensitive UPLC-MS/MS method for the analysis of narcotic analgesics in urine and whole blood in forensic context.

    PubMed

    Verplaetse, Ruth; Tytgat, Jan

    2012-02-10

    Narcotic analgesics are widely (ab) used and sometimes only occur in low concentrations in biological samples. Therefore, a highly sensitive liquid chromatography tandem mass spectrometry method was developed for simultaneous analysis of 9 narcotic analgesics and metabolites (buprenorphine, O-desmethyltramadol, fentanyl, norbuprenorphine, norfentanyl, pethidine, piritramide, tilidine and tramadol) in urine and whole blood. Sample preparation was performed on a mixed-mode cation exchange solid phase extraction cartridge with an additional alkaline wash step to decrease matrix effects and thus increase sensitivity. Ionization with electrospray ionization was found to be more efficient than atmospheric pressure chemical ionization. The use of a mobile phase of high pH resulted in higher electrospray ionization signals than the conventional low pH mobile phases. In the final method, gradient elution with 10mM ammonium bicarbonate (pH 9) and methanol was performed on a small particle column (Acquity C18, 1.7 μm, 2.1 mm × 50 mm). Selectivity, matrix effects, recovery, linearity, sensitivity, precision, accuracy and stability were validated in urine and whole blood. All parameters were successfully evaluated and the method showed very high sensitivity, which was the major aim of this study. The applicability of the method was demonstrated by analysis of several forensic cases involving narcotic analgesics. PMID:21356580

  4. Determination of polyphenols in Mentha longifolia and M. piperita field-grown and in vitro plant samples using UPLC-TQ-MS.

    PubMed

    Krzyzanowska, Justyna; Janda, Bogdan; Pecio, Lukasz; Stochmal, Anna; Oleszek, Wieslaw; Czubacka, Anna; Przybys, Marcin; Doroszewska, Teresa

    2011-01-01

    Nine polyphenols in the aerial parts of Mentha longifolia have been separated by chromatographic techniques. Their structures have been confirmed by HPLC/electrospray ionization-MS/MS. The compounds identified included rosmarinic acid, salvianolic acid L, dedihydro-salvianolic acid, luteolin-glucuronide, luteolin-diglucuronide, luteolin-glucopyranosyl-rhamnopyranoside, and eriodictyol-glucopyranosyl-rhamnopyranoside. The extracts of M. longifolia and M. piperita field plants, in vitro plants, callus tissues, and cell suspension cultures were profiled, and their polyphenol composition was compared in different tissues and quantified using ultra-performance column liquid chromatography (UPLC)/triple-quadrupole-MS in the selected-ion recording detection mode. Determination of desired compounds was based on calibration curves obtained for standards, which were previously isolated from M. longifolia aerial parts. The UPLC profiles revealed considerable differences in the synthesis of secondary metabolites among samples coming from field plants, in vitro plants, callus tissues, and cell suspension cultures. Plant tissues coming from field cultivation (for both M. piperita and M. longifolia) contained several phenolic compounds (flavonoids and phenolic acids), whereas plants from in vitro conditions, callus tissues, and suspension cultures contained only a few of them. Rosmarinic acid dominated in all of these samples. These results show that under in vitro conditions, the metabolism of phenolics undergoes a fundamental change.

  5. Development and validation of a sensitive UPLC-ESI-MS/MS method for the simultaneous quantification of 15 endocannabinoids and related compounds in milk and other biofluids.

    PubMed

    Gouveia-Figueira, Sandra; Nording, Malin L

    2014-01-21

    The endocannabinoid (eCB) system has gained an increasing interest over the past decades since the discovery of anandamide and 2-arachidonoyl glycerol (2-AG). These, and structurally related compounds, are associated with a wide variety of physiological processes. For instance, eCB levels in milk have been associated with infants' feeding and sleeping behavior. A method based on ultraperformance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) was developed and validated for the simultaneous quantification of 15 eCBs and related compounds, including both fatty acid amides and glycerols. Linearity (0.9845 < R(2) < 1), limit of detection and quantification (0.52-293 pg on column), inter- and intraday accuracy (>70%) and precision (CV < 15%), stability, and recovery (in milk and plasma) were established in accordance to the U.S. Food and Drug Administration guidelines. The method was successfully applied to bovine and elk milk revealing species-specific eCB profiles, with significant different levels of 2-AG, 2-linoleoyl glycerol, docosahexaenoyl ethanolamide, palmitoyl ethanolamide, and oleoyl ethanolamide. Furthermore, stearoyl ethanolamide and docosatetraenoyl ethanolamide were only detected in elk milk. In summary, our UPLC-ESI-MS/MS method may be used for quantification of eCBs and related compounds in different biofluids and applied to investigations of the role of these emerging compounds in various physiological processes. PMID:24377270

  6. Validation of a confirmatory method of salbutamol in sheep hair by UPLC-MS/MS and its application to pharmacokinetic study.

    PubMed

    Decheng, Suo; Wei, Zhang; Yu, Zhang; Genlong, Zhao; Ruigou, Wang; PeiLong, Wang; Xiaoou, Su

    2015-10-10

    A new method for determining salbutamol in hair of sheep by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was established. Samples were extracted with 0.1M of HCl solution. The mixture was heated to 60 °C in a water bath and kept at this temperature for 4h. The extracts were purified through SPE method and then dried with nitrogen. Residues were redissolved in mobile phase. The target compound was determined by UPLC-MS/MS with BEH-C18 column. The usefulness and feasibility of different treatment procedures of hair containing salbutamol were evaluated. The range of linearity was 1-100 ng/g. The LOD was 0.3 ng/g, and the LOQ was 1 ng/g. Recoveries were 89-106%, and coefficients of variation were 3.2-13.9%. Pharmacokinetics of salbutamol was studied in healthy sheep after oral administration of 150 μg/kg body weight salbutamol for 21 consecutive days. Salbutamol residues in hair were still detected after 21 days of administration. PMID:25988297

  7. Validation of a confirmatory method of salbutamol in sheep hair by UPLC-MS/MS and its application to pharmacokinetic study.

    PubMed

    Decheng, Suo; Wei, Zhang; Yu, Zhang; Genlong, Zhao; Ruigou, Wang; PeiLong, Wang; Xiaoou, Su

    2015-10-10

    A new method for determining salbutamol in hair of sheep by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was established. Samples were extracted with 0.1M of HCl solution. The mixture was heated to 60 °C in a water bath and kept at this temperature for 4h. The extracts were purified through SPE method and then dried with nitrogen. Residues were redissolved in mobile phase. The target compound was determined by UPLC-MS/MS with BEH-C18 column. The usefulness and feasibility of different treatment procedures of hair containing salbutamol were evaluated. The range of linearity was 1-100 ng/g. The LOD was 0.3 ng/g, and the LOQ was 1 ng/g. Recoveries were 89-106%, and coefficients of variation were 3.2-13.9%. Pharmacokinetics of salbutamol was studied in healthy sheep after oral administration of 150 μg/kg body weight salbutamol for 21 consecutive days. Salbutamol residues in hair were still detected after 21 days of administration.

  8. 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 μm (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

  9. Starch columns: Analog model for basalt columns

    NASA Astrophysics Data System (ADS)

    Müller, Gerhard

    1998-07-01

    Desiccation of starch-water mixtures produces tensile-crack patterns which appear to be interesting, but largely unknown study objects for fracture mechanics, structural geology, and volcanology. This paper concentrates on columnar jointing and on columns in starch. Starch columns have polygonal cross sections and are very similar to basalt columns. They are produced by lamp drying starch specimens with dimensions of several centimeters and have diameters in the millimeter range. The columns develop behind a crack front which propagates from the surface into the interior. The experiments, supported by X ray tomograms, show that polygonal regularity of the crack pattern is not present at the surface but develops during penetration. This transition is steered by a minimum-fracture-energy principle. The analogy between basalt cooling and starch desiccation is far reaching: water concentration in starch is analogous to temperature in basalt, both quantities obey diffusion equations, water loss is equivalent to heat loss, the resulting contraction stresses have similar dependences on depth and time, and in both cases the material strength is exceeded. The starch experiments show that column diameters are controlled by the depth gradient of water concentration at the crack front. High (low) gradients are connected with thin (thick) columns. By analogy, a similar relation with the temperature gradient exists for basalt columns. The (normalized) starch gradients are about 3 orders of magnitude larger than the (normalized) gradients in basalt. This explains why starch columns are much thinner than basalt columns. The gradients are so different, because the crack front speeds differ by a factor of about 10: after 3 days the speed is about 10 mm/d in starch but about 100 mm/d in basalt [Peck, 1978]. The speed difference, in turn, results from the difference of the diffusion constants: the hydraulic diffusivity of starch is 2 orders of magnitude lower than the thermal

  10. Column Liquid Chromatography.

    ERIC Educational Resources Information Center

    Majors, Ronald E.; And Others

    1984-01-01

    Reviews literature covering developments of column liquid chromatography during 1982-83. Areas considered include: books and reviews; general theory; columns; instrumentation; detectors; automation and data handling; multidimensional chromatographic and column switching techniques; liquid-solid chromatography; normal bonded-phase, reversed-phase,…

  11. HPLC and UPLC methods for the determination of zearalenone in noodles, cereal snacks and infant formula.

    PubMed

    Ok, Hyun Ee; Choi, Sung-Wook; Kim, Meehye; Chun, Hyang Sook

    2014-11-15

    High-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC) were compared to validate a method for determination of zearalenone (ZON) in noodles, cereal snacks, and infant formulas. The limits of detection and quantification in HPLC and UPLC were found to be 4.0 and 13.0 μg kg(-1) and 2.5 and 8.3 μg kg(-1), respectively. The average recoveries of ZON by HPLC and UPLC ranged from 79.1% to 105.3% and from 85.1% to 114.5%, respectively. The measurement uncertainties of the two methods for ZON determination were within the maximum standard uncertainty. The two methods showed that the levels of ZON in 163 naturally contaminated samples ranged from 4.3 to 8.3 μg kg(-1) by HPLC and 3.1 to 17.6 μg kg(-1) by UPLC. These findings indicate that either method is suitable for the determination of ZON in noodles, cereal snacks, and infant formulas, but UPLC gives faster results with better sensitivity. PMID:24912723

  12. Simultaneous determination of toltrazuril and its metabolites in chicken and pig skin+fat by UPLC-UV method.

    PubMed

    Zheng, Wenli; Jiang, Zhaoling; Zhang, Lifang; Zhang, Chong; Zhang, Xiao; Fei, Chenzhong; Zhang, Keyu; Wang, Xiaoyang; Wang, Mi; Li, Tao; Xiao, Sui; Wang, Chunmei; Xue, Feiqun

    2014-12-01

    A reliable method for the simultaneous determination of toltrazuril and its main metabolites (toltrazuril sulphone and toltrazuril sulphoxide) in chicken and pig skin+fat was developed and validated. Analytes were extracted from skin+fat with acetonitrile. The crude extracts were subjected to liquid-liquid extraction with n-hexane, and then further cleaned using primary secondary amine and Oasis™ MAX solid phase extraction cartridges. Chromatographic separation by UPLC-UV was performed on a C18+ reversed-phase column with gradient elution. Relative recovery from the spiked samples ranged from 84.8% to 109.1%. Limits of detection and quantification for the analytes were within 25-37.5μgkg(-1) and 50-75μgkg(-1), respectively. The developed method has been successfully applied to the depletion study of toltrazuril drug residues in chicken skin+fat. The recommended withdrawal period with oral administration based on our research is 24.18 days.

  13. Simultaneous quantification of picfeltarraenins IA and IB in rat plasma by UPLC-MS/MS: Application to a pharmacokinetic study.

    PubMed

    He, Xin; Zhang, Yingjie; Gao, Hang; Li, Keyan; Zhang, Yazhuo; Sun, Limin; Tao, Guizhou

    2016-02-20

    A simple and rapid quantitative UPLC-MS/MS method for simultaneous determination of picfeltarraenins IA and IB in rat plasma was developed and validated in accordance with the US FDA Bioanalytical Guidance (2001). Analytes were extracted from rat plasma by using methanol and separated on Agilent ZORBAX SB-C18 (50mm×2.1mm, 1.8μm) column by using a mobile phase composed of methanol and water (70:30, v/v). Eluents were monitored by ESI tandem mass spectrometry detection with SRM mode using ion transitions m/z 785.4→639.5, m/z 815.5→669.5, and m/z 763.5→455.3 for picfeltarraenin IA, picfeltarraenin IB, and internal standard, respectively. The method was validated over the linear range of 11.5-1150ng/mL and 13.0-1300ng/mL. The developed analytical method was applied to support a pharmacokinetic study on simultaneous estimation of picfeltarraenins IA and IB in rats.

  14. Metabolomic Analysis of Key Central Carbon Metabolism Carboxylic Acids as Their 3-Nitrophenylhydrazones by UPLC/ESI-MS

    PubMed Central

    Han, Jun; Gagnon, Susannah; Eckle, Tobias; Borchers, Christoph H.

    2014-01-01

    Multiple hydroxy-, keto-, di-, and tri-carboxylic acids are among the cellular metabolites of central carbon metabolism (CCM). Sensitive and reliable analysis of these carboxylates is important for many biological and cell engineering studies. In this work, we examined 3-nitrophenylhydrazine as a derivatizing reagent and optimized the reaction conditions for the measurement of ten CCM related carboxylic compounds, including glycolate, lactate, malate, fumarate, succinate, citrate, isocitrate, pyruvate, oxaloacetate, and α-ketoglutarate as their 3-nitrophenylhydrazones using LC/MS with electrospray ionization. With the derivatization protocol which we have developed, and using negative-ion multiple reaction monitoring on a triple-quadrupole instrument, all of the carboxylates showed good linearity within a dynamic range of ca. 200 to more than 2000. The on-column limits of detection and quantitation were from high femtomoles to low picomoles. The analytical accuracies for eight of the ten analytes were determined to be between 89.5 to 114.8% (CV≤7.4%, n=6). Using a quadrupole time-of-flight instrument, the isotopic distribution patterns of these carboxylates, extracted from a 13C-labeled mouse heart, were successfully determined by UPLC/MS with full-mass detection, indicating the possible utility of this analytical method for metabolic flux analysis. In summary, this work demonstrates an efficient chemical derivatization LC/MS method for metabolomic analysis of these key CCM intermediates in a biological matrix. PMID:23580203

  15. Interferon-alpha 2b quantification in inclusion bodies using reversed phase-ultra performance liquid chromatography (RP-UPLC).

    PubMed

    Cueto-Rojas, H F; Pérez, N O; Pérez-Sánchez, G; Ocampo-Juárez, I; Medina-Rivero, E

    2010-04-15

    Interferon-alpha 2b (IFN-alpha 2b) is a recombinant therapeutic cytokine produced as inclusion bodies using a strain of Escherichia coli as expression system. After fermentation and recovery, it is necessary to know the amount of recombinant IFN-alpha 2b, in order to determine the yield and the load for solubilization, and chromatographic protein purification steps. The present work details the validation of a new short run-time and fast sample-preparation method to quantify IFN-alpha 2b in inclusion bodies using Reversed Phase-Ultra Performance Liquid Chromatography (RP-UPLC). The developed method demonstrated an accuracy of 100.28%; the relative standard deviations for method precision, repeatability and inter-day precision tests were found to be 0.57%, 1.54% and 1.83%, respectively. Linearity of the method was assessed in the range of concentrations from 0.05 mg/mL to 0.5 mg/mL, the curve obtained had a determination coefficient (r(2)) of 0.9989. Detection and quantification limits were found to be 0.008 mg/mL and 0.025 mg/mL, respectively. The method also demonstrated robustness for changes in column temperature, and specificity against host proteins and other recombinant protein expressed in the same E. coli strain. PMID:20299292

  16. A qualitative, and quantitative determination and pharmacokinetic study of four polyacetylenes from Radix Bupleuri by UPLC-PDA-MS.

    PubMed

    Liu, Jiali; Fang, Yuan; Yang, Lan; Qin, Xuemei; Du, Guanhua; Gao, Xiaoxia

    2015-01-01

    This study was carried out to identify some new antidepressant compounds present in Radix Bupleuri (RB) and to develop a method for their quantitative analysis in rat serum for the first time. Four polyacetylenes, including two new compounds, were isolated from Bupleurum scorzonerifoliu and identified. An in vitro uptake study using rat synaptosomes showed that the polyacetylenes potently inhibited serotonin, norepinephrine and dopamine reuptake, and exhibited an antidepressant activity with a potency comparable with or better than their corresponding specific inhibitors. An ultra-performance liquid chromatography coupled with photodiode array detector (UPLC-PDA) method was developed for their quantitative analysis in rat serum. The analysis was performed on a Waters BEH C18 column (1.7 μm, 100 × 2.1 mm i.d.) using a gradient system of acetonitrile and 0.03% trifluoroacetic acid water, with a detector wavelength of 315 nm. Only two polyacetylenes, ((2 Z,8 E,10 E)-pentadecatriene-4,6-diyn-1-ol (RB-2) and bupleurynol (RB-4)), were detected in the primarily pharmacokinetic study of the petroleum ether fraction of RB. Both were rapidly absorbed and slowly eliminated. The rat exposure was approximately linear under the studied dosages ranging from 22.5 to 90 g/kg herb. In summary, polyacetylenes appear to be the key components responsible for the antidepressant activity of RB, and could be used as chemical standards for the quality evaluation of RB.

  17. Inelastic column behavior

    NASA Technical Reports Server (NTRS)

    Duberg, John E; Wilder, Thomas W , III

    1952-01-01

    The significant findings of a theoretical study of column behavior in the plastic stress range are presented. When the behavior of a straight column is regarded as the limiting behavior of an imperfect column as the initial imperfection (lack of straightness) approaches zero, the departure from the straight configuration occurs at the tangent-modulus load. Without such a concept of the behavior of a straight column, one is led to the unrealistic conclusion that lateral deflection of the column can begin at any load between the tangent-modulus value and the Euler load, based on the original elastic modulus. A family of curves showing load against lateral deflection is presented for idealized h-section columns of various lengths and of various materials that have a systematic variation of their stress-strain curves.

  18. Distillation Column Modeling Tools

    SciTech Connect

    2001-09-01

    Advanced Computational and Experimental Techniques will Optimize Distillation Column Operation. Distillation is a low thermal efficiency unit operation that currently consumes 4.8 quadrillion BTUs of energy...

  19. Measuring Ochratoxin A Concentrations in Coffee Beverages with Immunoaffinity Columns and Ultra-Performance Liquid Chromatography/Tandem Mass Spectrometry.

    PubMed

    Chen, Wen-Ling; Chang, Chiung-Wen; Chen, Chia-Yang

    2016-01-01

    This study developed and validated a method for measuring concentrations of ochratoxin A (OTA) in coffee beverages, not coffee beans. The new method involved extraction using immunoaffinity columns and ultra-performance LC (UPLC)-MS/MS using isotope-dilution techniques. The combination of a fused-core column and UPLC significantly shortened chromatographic time to 3 min compared to reported UPLC methods. The method was sensitive, with an LOD and LOQ of 0.52 and 1.73 pg/mL, respectively. Quantitative intraday (n = 4) and interday (n = 4) biases and RSD were both below 15%. The OTA levels in 40 samples of freshly brewed coffee from chain stores, 24 samples of canned ready-to-drink coffee, and 6 beverages made from instant coffee granules ranged from 1.60 to 93.2 pg/mL (90% positive), 6.00 to 131 pg/mL (100% positive), and 21.8 to 59.0 pg/mL (100% positive), respectively. Based on published tolerable daily intake, men and women in Taiwan should consume no more than 6.3 and 5.1 fifteen gram packages of instant coffee per day, respectively. Specific suggestions were not made for brewed coffee and canned coffee because of their large variation in OTA concentrations. This study should be more relevant to actual human exposure than those studying OTA in green, roasted, and ground coffee beans alone. PMID:26965577

  20. Rapid separation and characterization of active flavonolignans of Silybum marianum by ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry.

    PubMed

    Wang, Kuiwu; Zhang, Hong; Shen, Lianqing; Du, Qizhen; Li, Jianrong

    2010-12-01

    Ultra-performance liquid chromatography (UPLC) interfaced with the electrospray ionization (ESI) tandem mass spectrometer (MS(n)) was developed for the simultaneous determination of silychristins A (1) and B (2), silydianin (3), silybins A (4) and B (5), and isosilybins A (6) and B (7), major bioactive flavonolignans in silymarin, a herbal remedy derived from the milk thistle Silybum marianum. In this study, the seven major active flavonolignans including the diastereomers 1/2, 4/5, and 6/7 were completely separated using UPLC with an ACQUITY UPLC C(18) column and a MeOH/water/formic acid mobile phase system. The collision-induced dissociation (CID) MS(n) spectra of these flavonolignans were studied systematically using ESI-MS. The results with the present methodology show that UPLC-MS(n) can be useful for general screening of active natural products from plant extracts and for the specific quality control of silymarin.

  1. Inflatable Column Structure

    NASA Technical Reports Server (NTRS)

    Hedgepeth, J. M.

    1985-01-01

    Lightweight structural member easy to store. Billowing between circumferential loops of fiber inflated column becomes series of cells. Each fiber subjected to same tension along entire length (though tension is different in different fibers). Member is called "isotensoid" column. Serves as jack for automobiles or structures during repairs. Also used as support for temporary bleachers or swimming pools.

  2. Glass-silicon column

    DOEpatents

    Yu, Conrad M.

    2003-12-30

    A glass-silicon column that can operate in temperature variations between room temperature and about 450.degree. C. The glass-silicon column includes large area glass, such as a thin Corning 7740 boron-silicate glass bonded to a silicon wafer, with an electrode embedded in or mounted on glass of the column, and with a self alignment silicon post/glass hole structure. The glass/silicon components are bonded, for example be anodic bonding. In one embodiment, the column includes two outer layers of silicon each bonded to an inner layer of glass, with an electrode imbedded between the layers of glass, and with at least one self alignment hole and post arrangement. The electrode functions as a column heater, and one glass/silicon component is provided with a number of flow channels adjacent the bonded surfaces.

  3. Rapid analysis of lignans from leaves of Podophyllum peltatum l. samples using UPLC-UV-MS

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A new rapid UPLC-UV-MS method has been developed that permits the analysis of four lignans in P. peltatum L. Podophyllotoxin is a natural lignan that is being used as a precursor for the semi-synthetic anti-cancer drugs etoposide, teniposide and etopophos. The chromatographic separation was achieved...

  4. Rapid analysis of lignans from leaves of Podophyllum peltatum L samples using UPLC-UV-MS

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A new rapid UPLC-UV-MS method has been developed that permits the analysis of four lignans in P. peltatum L. Podophyllotoxin is a natural lignan that is being used as a precursor for the semi-synthetic anti-cancer drugs etoposide, teniposide and etopophos. The chromatographic separation was achieved...

  5. Determination of anthelmintic drug residues in milk using UPLC-MS/MS with rapid polarity switching

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A new UPLC-MS/MS (ultra-performance liquid chromatography coupled to tandem mass spectrometry) method was developed and validated to detect 38 anthelmintic drug residues, consisting of benzimidazoles, avermectins and flukicides. A modified QuEChERS-type extraction method was developed with an added...

  6. Distillation Column Flooding Predictor

    SciTech Connect

    George E. Dzyacky

    2010-11-23

    The Flooding Predictor™ is a patented advanced control technology proven in research at the Separations Research Program, University of Texas at Austin, to increase distillation column throughput by over 6%, while also increasing energy efficiency by 10%. The research was conducted under a U. S. Department of Energy Cooperative Agreement awarded to George Dzyacky of 2ndpoint, LLC. The Flooding Predictor™ works by detecting the incipient flood point and controlling the column closer to its actual hydraulic limit than historical practices have allowed. Further, the technology uses existing column instrumentation, meaning no additional refining infrastructure is required. Refiners often push distillation columns to maximize throughput, improve separation, or simply to achieve day-to-day optimization. Attempting to achieve such operating objectives is a tricky undertaking that can result in flooding. Operators and advanced control strategies alike rely on the conventional use of delta-pressure instrumentation to approximate the column’s approach to flood. But column delta-pressure is more an inference of the column’s approach to flood than it is an actual measurement of it. As a consequence, delta pressure limits are established conservatively in order to operate in a regime where the column is never expected to flood. As a result, there is much “left on the table” when operating in such a regime, i.e. the capacity difference between controlling the column to an upper delta-pressure limit and controlling it to the actual hydraulic limit. The Flooding Predictor™, an innovative pattern recognition technology, controls columns at their actual hydraulic limit, which research shows leads to a throughput increase of over 6%. Controlling closer to the hydraulic limit also permits operation in a sweet spot of increased energy-efficiency. In this region of increased column loading, the Flooding Predictor is able to exploit the benefits of higher liquid

  7. Nuclear reactor control column

    DOEpatents

    Bachovchin, Dennis M.

    1982-01-01

    The nuclear reactor control column comprises a column disposed within the nuclear reactor core having a variable cross-section hollow channel and containing balls whose vertical location is determined by the flow of the reactor coolant through the column. The control column is divided into three basic sections wherein each of the sections has a different cross-sectional area. The uppermost section of the control column has the greatest cross-sectional area, the intermediate section of the control column has the smallest cross-sectional area, and the lowermost section of the control column has the intermediate cross-sectional area. In this manner, the area of the uppermost section can be established such that when the reactor coolant is flowing under normal conditions therethrough, the absorber balls will be lifted and suspended in a fluidized bed manner in the upper section. However, when the reactor coolant flow falls below a predetermined value, the absorber balls will fall through the intermediate section and into the lowermost section, thereby reducing the reactivity of the reactor core and shutting down the reactor.

  8. Depletion of urinary zilpaterol residues in horses as measured by ELISA and UPLC-MS/MS.

    PubMed

    Shelver, Weilin L; Thorson, Jennifer F; Hammer, Carolyn J; Smith, David J

    2010-04-14

    Three horses were dosed with dietary zilpaterol and the urine concentrations measured from withdrawal day 0 to withdrawal day 21. The analyses were carried out using both enzyme-linked immunosorbent assay (ELISA) and an ultraperformance liquid chromatography with triple-quadrupole-tandem mass spectrometric detection (UPLC-MS/MS). The UPLC-MS/MS method was developed to provide rapid analysis with positive analyte identification by following three product ions and computing the two independent ion ratios. When urinary zilpaterol concentrations were between 0.2 and 2 ng/mL, the ELISA had interday recoveries of 114-120% with coefficients of variation (CV) of <22%; intraday recoveries were 79-111% with CVs of <13%. For urinary zilpaterol concentrations of 0.4-40 ng/mL the UPLC-MS/MS method had interday recoveries of 94-104% with CVs of <8%; intraday recoveries were 97-102% with CVs of < or = 7.5%. Correlation analysis demonstrated that the ELISA and UPLC-MS/MS methods returned essentially the same results, especially at urinary zilpaterol concentrations below 2000 ng/mL. Urinary excretion peaked rapidly after dosing between 5300 and 10800 ng/mL (UPLC-MS/MS) or between 5900 and 17900 ng/mL (ELISA) for the different horses, much higher than observed in other species. Urinary zilpaterol concentrations declined rapidly to below 3000 ng/mL within 24 h of study day 1. After about 5 days, zilpaterol elimination slowed markedly, taking nearly 10 days for an order of magnitude decrease. The analytical methods were able to detect zilpaterol in the urine even at withdrawal day 21, demonstrating the sensitivity of each analytical method and the slow rate of zilpaterol depuration from horses.

  9. Antihepatotoxic Effect and Metabolite Profiling of Panicum turgidum Extract via UPLC-qTOF-MS

    PubMed Central

    Farag, Mohamed A.; El Fishawy, Ahlam M.; El-Toumy, Sayed A.; Amer, Khadiga F.; Mansour, Ahmed M.; Taha, Hala E.

    2016-01-01

    Background: Panicum turgidum, desert grass, has not reported any detailed phytochemical or biological study as yet Objective: To establish P. turgidum secondary metabolite profile and to assess its antihepatotoxic effect Materials and Methods: Ultra-performance liquid chromatography (UPLC) coupled to quadrupole high-resolution time of flight mass spectrometry (qTOF-MS) was used for large-scale secondary metabolites profiling in P. turgidum extract, alongside assessing median lethal dose (LD50) and hepatoprotective effect against carbon tetrachloride (CCl4) intoxication Results: A total of 39 metabolites were identified with flavonoids as the major class present as O/C-glycosides of luteolin, apigenin, isorhamnetin and naringenin, most of which are first time to be reported in Panicum sp. Antihepatotoxic effect of P. turgidum crude extract was revealed via improving several biochemical marker levels and mitigation against oxidative stress in the serum and liver tissues, compared with CCl4 intoxicated group and further confirmed by histopathological examination. Conclusion: This study reveals that P. turgidum, enriched in C-flavonoids, presents a novel source of safe antihepatotoxic agents and further demonstrates the efficacy of UPLC-MS metabolomics in the field of natural products drug discovery. SUMMARY UPLC coupled to qTOF-MS was used for large scale secondary metabolites profiling in P. turgidum.A total of 39 metabolites were identified with flavonoids amounting as the major metabolite class.Anti-hepatotoxic effect of P. turgidum extract was revealed via several biochemical markers and histopathological examination.This study reveals that P. turgidum, enriched in C-flavonoids, present a novel source of antihepatotoxic agents. Abbreviations used: UPLC: Ultra-performance liquid chromatography (UPLC), LD50: median lethal dose, MDA: malondialdehyde, GSH: glutathione reductase, CAT: catalase, SOD: superoxide dismutase, ALT: alanine aminotransferase, AST: aspartate

  10. Development and validation of an UPLC-DAD-MS method for the determination of leonurine in Chinese motherwort (Leonurus japonicus).

    PubMed

    Chen, Zhe; Wu, Jian Bing; Liao, Xiao Juan; Yang, Wei; Song, Kang

    2010-11-01

    In the present study, an ultra-performance liquid chromatography method with diode array detection (UPLC-DAD) was developed for the analysis and determination of leonurine from motherwort (Leonurus japonicus), a traditional Chinese medicinal plant. This method was validated in terms of specificity, linearity (R(2) = 0.9995, linear range: 0.005 ~ 0.5 mg/mL), precision (< 5.0% RSD), and recovery (103.2%). The extracted amount of leonurine is 0.15 mg/g. Moreover, the target analyte was identified or tentatively characterized using UPLC coupled with electrospary tandem mass spectrometry (UPLC-ESI-MS).

  11. UPLC-MRM Mass Spectrometry Method for Measurement of the Coagulation Inhibitors Dabigatran and Rivaroxaban in Human Plasma and Its Comparison with Functional Assays

    PubMed Central

    Kuhn, Joachim; Gripp, Tatjana; Flieder, Tobias; Dittrich, Marcus; Hendig, Doris; Busse, Jessica; Knabbe, Cornelius; Birschmann, Ingvild

    2015-01-01

    Introduction The fast, precise, and accurate measurement of the new generation of oral anticoagulants such as dabigatran and rivaroxaban in patients’ plasma my provide important information in different clinical circumstances such as in the case of suspicion of overdose, when patients switch from existing oral anticoagulant, in patients with hepatic or renal impairment, by concomitant use of interaction drugs, or to assess anticoagulant concentration in patients’ blood before major surgery. Methods Here, we describe a quick and precise method to measure the coagulation inhibitors dabigatran and rivaroxaban using ultra-performance liquid chromatography electrospray ionization-tandem mass spectrometry in multiple reactions monitoring (MRM) mode (UPLC-MRM MS). Internal standards (ISs) were added to the sample and after protein precipitation; the sample was separated on a reverse phase column. After ionization of the analytes the ions were detected using electrospray ionization-tandem mass spectrometry. Run time was 2.5 minutes per injection. Ion suppression was characterized by means of post-column infusion. Results The calibration curves of dabigatran and rivaroxaban were linear over the working range between 0.8 and 800 μg/L (r >0.99). Limits of detection (LOD) in the plasma matrix were 0.21 μg/L for dabigatran and 0.34 μg/L for rivaroxaban, and lower limits of quantification (LLOQ) in the plasma matrix were 0.46 μg/L for dabigatran and 0.54 μg/L for rivaroxaban. The intraassay coefficients of variation (CVs) for dabigatran and rivaroxaban were < 4% and 6%; respectively, the interassay CVs were < 6% for dabigatran and < 9% for rivaroxaban. Inaccuracy was < 5% for both substances. The mean recovery was 104.5% (range 83.8–113.0%) for dabigatran and 87.0% (range 73.6–105.4%) for rivaroxaban. No significant ion suppressions were detected at the elution times of dabigatran or rivaroxaban. Both coagulation inhibitors were stable in citrate plasma at -20°C, 4

  12. Microminiature gas chromatographic column

    NASA Technical Reports Server (NTRS)

    Donaldson, R. W., Jr.

    1972-01-01

    Techniques commonly used for fabrication of integrated circuits are utilized to produce long capillary tubes for microminiature chromatographs. Method involves bonding of flat silicon plate to top of spirally grooved silicon chip to close groove and form capillary column.

  13. Distillation Column Flooding Predictor

    SciTech Connect

    2002-02-01

    This factsheet describes a research project whose goal is to develop the flooding predictor, an advanced process control strategy, into a universally useable tool that will maximize the separation yield of a distillation column.

  14. A method of analysis for T-2 toxin and neosolaniol by UPLC-MS/MS in apple fruit inoculated with Trichothecium roseum.

    PubMed

    Tang, Yamei; Xue, Huali; Bi, Yang; Li, Yongcai; Wang, Yi; Zhao, Ying; Shen, Keping

    2015-01-01

    Trichothecenes are one of the most important groups of mycotoxins produced by Trichothecium roseum, which causes core rot of apple. A reliable and sensitive method was developed and successfully applied for the rapid detection of trichothecenes including T-2 toxin and neosolaniol in harvested apple using UPLC-MS/MS. After the extraction of the two mycotoxins from the apple matrix with methanol/water (80/20, v/v), the concentrated extracts were cleaned-up by PriboFast M270 columns and then analysed by UPLC-MS/MS. T-2 toxin and neosolaniol were effectively separated as unique peaks. The validity of this method was established by its linearity (R(2) ≥ 0.9995), precision (relative standard deviation ≤ 3.6%), accuracy, selectivity, limit of detection of 2-5 μg kg(-1), limit of quantification of 5-10 μg kg(-1) and average recovery of 73-96%. Levels of T-2 toxin were found in the range 7.1-128.4 µg kg(-1) in the core rot lesion of three cultivars apple (cvs. Red Delicious, Fuji and Ralls). T-2 was detected not only in the lesion, but also in the tissue without any disease symptoms. However, neosolaniol was only detected in the lesion on 'Red Delicious' apples. In addition, the concentration of T-2 toxin in the susceptible cultivar (cv. Fuji) was significantly higher than that in the resistant one (cv. Ralls). This method proved to be suitable at detecting T-2 and neosolaniol simultaneously in apples infected with T. roseum.

  15. Towards Atomic Column-by-Column Spectroscopy

    SciTech Connect

    Pennycook, S.J.; Rafferty, B.

    1998-09-06

    The optical arrangement of the scanning transmission electron microscope (STEM) is ideally suited for performing analysis of individual atomic columns in materials. Using the incoherent Z-contrast image as a reference, and arranging incoherent conditions also for the spectroscopy, a precise correspondence is ensured between features in the inelastic image and elastic signals. In this way the exact probe position needed to maximise the inelastic signal from a selected column can be located and monitored during the analysis using the much higher intensity elastic signal. Although object functions for EELS are typically less than 1 {Angstrom} full width at half maximum, this is still an order of magnitude larger than the corresponding object functions for elastic (or diffuse) scattering used to form the Z-contrast image. Therefore the analysis is performed with an effective probe that is significantly broader than that used for the reference Z-contrast image. For a 2.2 {Angstrom} probe the effective probe is of the order of 2.5 {Angstrom}, while for a 1.3 {Angstrom} probe the effective probe is 1.6 {Angstrom}. Such increases in effective probe size can significantly reduce or even eliminate contrast between atomic columns that are visible in the image. However, this is only true if we consider circular collector apertures. Calculations based upon the theory of Maslen and Rossouw (Maslen and Rossouw 1984; Rossouw and Maslen 1984) show that employing an annular aperture can reduce the FWHM of the inelastic object function down to values close 0.1 {Angstrom}. With practical aperture sizes it should be possible to achieve this increased spatial resolution without loosing too much signal.

  16. Separation analysis of macrolide antibiotics with good performance on a positively charged C18HCE column.

    PubMed

    Wei, Jie; Shen, Aijin; Yan, Jingyu; Jin, Gaowa; Yang, Bingcheng; Guo, Zhimou; Zhang, Feifang; Liang, Xinmiao

    2016-03-01

    The separation of basic macrolide antibiotics suffers from peak tailing and poor efficiency on traditional silica-based reversed-phase liquid chromatography columns. In this work, a C18HCE column with positively charged surface was applied to the separation of macrolides. Compared with an Acquity BEH C18 column, the C18HCE column exhibited superior performance in the aspect of peak shape and separation efficiency. The screening of mobile phase additives including formic acid, acetic acid and ammonium formate indicated that formic acid was preferable for providing symmetrical peak shapes. Moreover, the influence of formic acid content was investigated. Analysis speed and mass spectrometry compatibility were also taken into account when optimizing the separation conditions for liquid chromatography coupled with tandem mass spectrometry. The developed method was successfully utilized for the determination of macrolide residues in a honey sample. Azithromycin was chosen as the internal standard for the quantitation of spiramycin and tilmicosin, while roxithromycin was used for erythromycin, tylosin, clarithromycin, josamycin and acetylisovaleryltylosin. Good correlation coefficients (r(2) > 0.9938) for all macrolides were obtained. The intra-day and inter-day recoveries were 73.7-134.7% and 80.7-119.7% with relative standard deviations of 2.5-8.0% and 3.9-16.1%, respectively. Outstanding sensitivity with limits of quantitation (S/N ≥ 10) of 0.02-1 μg/kg and limits of detection (S/N ≥ 3) of 0.01-0.5 μg/kg were achieved. PMID:26782089

  17. Ultrasound-assisted hydrolysis of conjugated parabens in human urine and their determination by UPLC-MS/MS and UPLC-HRMS.

    PubMed

    Schlittenbauer, Linda; Seiwert, Bettina; Reemtsma, Thorsten

    2016-02-01

    Parabens are preservatives widely used in personal care products, pharmaceutical formulations as well as in food, and they are considered endocrine disruptors. For application in biomonitoring studies we developed a method for the determination of eight parabens from human urine. Sample preparation was enhanced and simplified by the combination of ultrasound-assisted enzymatic hydrolysis of conjugates (glucuronide and sulfate) followed by an extraction-free cleanup step. Quantification, using deuterated parabens as internal standards, was performed by ultrahigh-performance liquid chromatography coupled to either triple-quadrupole (UPLC-QqQ) or time-of-flight (UPLC-QqTOF) mass spectrometry. Full chromatographic separation of three butyl paraben isomers was achieved. Limits of quantification for both mass analyzers ranged from 0.1 to 0.5 μg/L for methyl, ethyl, n-/isopropyl, n-/isobutyl, and benzyl paraben in 200 μL of urine sample. The method was tested for applicability and showed high precision (intra- and interday 0.9-14.5%) as well as high accuracy (relative recovery 95-132%). A total of 39 urine samples were analyzed by both mass analyzers. The results agreed well, with a trend to higher deviation at low concentrations (less than 10 μg/L). Methyl, ethyl, and n-propyl paraben were detected most frequently (in more than 87% of the samples) with median concentrations ranging from 0.8 to 16.6 μg/L. Female urine showed higher median concentrations for all parabens, which may indicate higher exposure due to lifestyle. This method permits accurate and high-throughput analysis of parabens for epidemiological studies. Further, the UPLC-QqTOF approach provides additional information on human exposure to other compounds by post-acquisition analysis. PMID:26753983

  18. Development and validation of a stability indicating UPLC method for determination of ticlopidine hydrochloride in its tablet formulation

    PubMed Central

    Ram, Vijay; Kher, Govind; Dubal, Kapil; Dodiya, Bhavesh; Joshi, Hitendra

    2011-01-01

    The objective of the current study was the development of a simple, precise and accurate isocratic reversed-phase stability indicating Ultra Performance Liquid Chromatography [UPLC] assay method and validated for determination of ticlopidine hydrochloride in solid pharmaceutical dosage forms. Isocratic separation was achieved on a Zorbax SB-C18 (50 mm × 4.6 mm, 1.8 μm) column using mobile phase of methanol–0.01 M ammonium acetate buffer, pH 5.0 (80:20, v/v) at a flow rate of 0.8 ml min−1, the injection volume was 4.0 μl and the detection was carried out at 235 nm by using photo-diode array detector. The drug was subjected to oxidation, hydrolysis, photolysis and heat to apply stress condition. The method was validated for specificity, linearity, precision, accuracy, robustness and solution stability. The method was linear in the drug concentration range of 62.5–375 μg ml−1 with a correlation coefficient of 0.9999. The precision (relative standard deviation – RSD) of six samples was 1.31% for repeatability and the intermediate precision [RSD] among six-sample preparation was 0.77%. The accuracy (recovery) was between 98.80% and 101.50%. Degradation products produced as a result of stress studies did not interfere with detection of ticlopidine hydrochloride and the assay can thus be considered stability indicating. PMID:23960754

  19. Eruption column physics

    SciTech Connect

    Valentine, G.A.

    1997-03-01

    In this paper the author focuses on the fluid dynamics of large-scale eruption columns. The dynamics of these columns are rooted in multiphase flow phenomena, so a major part of the paper sets up a foundation on that topic that allows one to quickly assess the inherent assumptions made in various theoretical and experimental approaches. The first part is centered on a set of complex differential equations that describe eruption columns, but the focus is on a general understanding of important physical processes rather than on the mathematics. The author discusses briefly the relative merits and weaknesses of different approaches, emphasizing that the largest advances in understanding are made by combining them. He then focuses on dynamics of steady eruption columns and then on transient phenomena. Finally he briefly reviews the effects of varying behavior of the ambient medium through which an eruption column moves. These final sections will emphasize concepts and a qualitative understanding of eruption dynamics. This paper relies on principles of continuum mechanics and transport processes but does not go into detail on the development of those principles. 36 refs., 36 figs., 3 tabs.

  20. Impact of the column hardware volume on resolution in very high pressure liquid chromatography non-invasive investigations.

    PubMed

    Gritti, Fabrice; McDonald, Thomas; Gilar, Martin

    2015-11-13

    The impact of the column hardware volume (≃ 1.7 μL) on the optimum reduced plate heights of a series of short 2.1 mm × 50 mm columns (hold-up volume ≃ 80-90 μL) packed with 1.8 μm HSS-T3, 1.7 μm BEH-C18, 1.7 μm CSH-C18, 1.6 μm CORTECS-C18+, and 1.7 μm BEH-C4 particles was investigated. A rapid and non-invasive method based on the reduction of the system dispersion (to only 0.15 μL(2)) of an I-class Acquity system and on the corrected plate heights (for system dispersion) of five weakly retained n-alkanophenones in RPLC was proposed. Evidence for sample dispersion through the column hardware volume was also revealed from the experimental plot of the peak capacities for smooth linear gradients versus the corrected efficiency of a weakly retained alkanophenone (isocratic runs). The plot is built for a constant gradient steepness irrespective of the applied flow rates (0.01-0.30 mL/min) and column lengths (2, 3, 5, and 10 cm). The volume variance caused by column endfittings and frits was estimated in between 0.1 and 0.7 μL(2) depending on the applied flow rate. After correction for system and hardware dispersion, the minimum reduced plate heights of short (5 cm) and narrow-bore (2.1mm i.d.) beds packed with sub-2 μm fully and superficially porous particles were found close to 1.5 and 0.7, respectively, instead of the classical h values of 2.0 and 1.4 for the whole column assembly.

  1. [Research on UPLC-PDA fingerprint of andrographis paniculata and quantitative determination of 4 major constituents].

    PubMed

    Huang, Jing-Yi; Liu, Xiao-Lin; Zhou, Shui-Ping; Tong, Ling; Ding, Li

    2014-11-01

    Andrographis paniculata from different parts and origins were analyzed by UPLC-PDA fingerprint to provide refererice for related preparation technology. Using the peak of andrographolide as reference, 27 common peaks were identified, and digitized UPLC-PDA fingerprints for 23 batches of andrographis paniculata were established in this research. Principal component analysis (PCA) was carried out after feature extraction. The contents of andrographolide, neoandrographolide, deoxyandrographolide, dehydroandrographolide were determined by external standard method. The Plackett-Burman design combined with pareto chart was used to analyze the factors influencing the robustness of the method. It was found that the medicinal part has a more remarkable influence on the quality of andrographis paniculata than the origin. The contents of the 4 lactones the differ greatly in the different parts of andrographis paniculata, and the pH of the mobile phase is an important factor that influenced the robustness of the method.

  2. Classification of illicit heroin by UPLC-Q-TOF analysis of acidic and neutral manufacturing impurities.

    PubMed

    Liu, Cuimei; Hua, Zhendong; Bai, Yanping

    2015-12-01

    The illicit manufacture of heroin results in the formation of trace levels of acidic and neutral manufacturing impurities that provide valuable information about the manufacturing process used. In this work, a new ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF) method; that features high resolution, mass accuracy and sensitivity for profiling neutral and acidic heroin manufacturing impurities was developed. After the UPLC-Q-TOF analysis, the retention times and m/z data pairs of acidic and neutral manufacturing impurities were detected, and 19 peaks were found to be evidently different between heroin samples from "Golden Triangle" and "Golden Crescent". Based on the data set of these 19 impurities in 150 authentic heroin samples, classification of heroin geographic origins was successfully achieved utilizing partial least squares discriminant analysis (PLS-DA). By analyzing another data set of 267 authentic heroin samples, the developed discrimiant model was validated and proved to be accurate and reliable.

  3. Metabolite Profiling of Justicia gendarussa Burm. f. Leaves Using UPLC-UHR-QTOF-MS

    PubMed Central

    Ningsih, Indah Yulia; Purwanti, Diah Intan; Wongso, Suwidji; Prajogo, Bambang E. W.; Indrayanto, Gunawan

    2015-01-01

    An ultra-performance liquid chromatography ultra-high-resolution quadrupole-time-of-flight-mass spectrometry (UPLC-UHR-QTOF-MS) metabolite profiling ofxs Justicia gendarussa Burm. f. leaves was performed. PCA and HCA analyses were applied to observe the clustering patterns and inter-sample relationships. It seemed that the concentrations of Ca, P, and Cu in the soil could affect the metabolite profiles of Justicia gendarussa. Six significant metabolites were proposed. PMID:26839833

  4. Metabolite Profiling of Justicia gendarussa Burm. f. Leaves Using UPLC-UHR-QTOF-MS.

    PubMed

    Ningsih, Indah Yulia; Purwanti, Diah Intan; Wongso, Suwidji; Prajogo, Bambang E W; Indrayanto, Gunawan

    2015-01-01

    An ultra-performance liquid chromatography ultra-high-resolution quadrupole-time-of-flight-mass spectrometry (UPLC-UHR-QTOF-MS) metabolite profiling ofxs Justicia gendarussa Burm. f. leaves was performed. PCA and HCA analyses were applied to observe the clustering patterns and inter-sample relationships. It seemed that the concentrations of Ca, P, and Cu in the soil could affect the metabolite profiles of Justicia gendarussa. Six significant metabolites were proposed. PMID:26839833

  5. Global Profiling of Various Metabolites in Platycodon grandiflorum by UPLC-QTOF/MS

    PubMed Central

    Lee, Jae Won; Ji, Seung-Heon; Kim, Geum-Soog; Song, Kyung-Sik; Um, Yurry; Kim, Ok Tae; Lee, Yi; Hong, Chang Pyo; Shin, Dong-Ho; Kim, Chang-Kug; Lee, Seung-Eun; Ahn, Young-Sup; Lee, Dae-Young

    2015-01-01

    In this study, a method of metabolite profiling based on UPLC-QTOF/MS was developed to analyze Platycodon grandiflorum. In the optimal UPLC, various metabolites, including major platycosides, were separated well in 15 min. The metabolite extraction protocols were also optimized by selecting a solvent for use in the study, the ratio of solvent to sample and sonication time. This method was used to profile two different parts of P. grandiflorum, i.e., the roots of P. grandiflorum (PR) and the stems and leaves of P. grandiflorum (PS), in the positive and negative ion modes. As a result, PR and PS showed qualitatively and quantitatively different metabolite profiles. Furthermore, their metabolite compositions differed according to individual plant samples. These results indicate that the UPLC-QTOF/MS-based profiling method is a good tool to analyze various metabolites in P. grandiflorum. This metabolomics approach can also be applied to evaluate the overall quality of P. grandiflorum, as well as to discriminate the cultivars for the medicinal plant industry. PMID:26569219

  6. UPLC-MS(E) application in disease biomarker discovery: the discoveries in proteomics to metabolomics.

    PubMed

    Zhao, Ying-Yong; Lin, Rui-Chao

    2014-05-25

    In the last decade, proteomics and metabolomics have contributed substantially to our understanding of different diseases. Proteomics and metabolomics aims to comprehensively identify proteins and metabolites to gain insight into the cellular signaling pathways underlying disease and to discover novel biomarkers for screening, early detection and diagnosis, as well as for determining prognoses and predicting responses to specific treatments. For comprehensive analysis of cellular proteins and metabolites, analytical methods of wider dynamic range higher resolution and good sensitivity are required. Ultra performance liquid chromatography-mass spectrometry(Elevated Energy) (UPLC-MS(E)) is currently one of the most versatile techniques. UPLC-MS(E) is an established technology in proteomics studies and is now expanding into metabolite research. MS(E) was used for simultaneous acquisition of precursor ion information and fragment ion data at low and high collision energy in one analytical run, providing similar information to conventional MS(2). In this review, UPLC-MS(E) application in proteomics and metabolomics was highlighted to assess protein and metabolite changes in different diseases, including cancer, neuropsychiatric pharmacology studies from clinical trials and animal models. In addition, the future prospects for complete proteomics and metabolomics are discussed.

  7. Global Profiling of Various Metabolites in Platycodon grandiflorum by UPLC-QTOF/MS.

    PubMed

    Lee, Jae Won; Ji, Seung-Heon; Kim, Geum-Soog; Song, Kyung-Sik; Um, Yurry; Kim, Ok Tae; Lee, Yi; Hong, Chang Pyo; Shin, Dong-Ho; Kim, Chang-Kug; Lee, Seung-Eun; Ahn, Young-Sup; Lee, Dae-Young

    2015-01-01

    In this study, a method of metabolite profiling based on UPLC-QTOF/MS was developed to analyze Platycodon grandiflorum. In the optimal UPLC, various metabolites, including major platycosides, were separated well in 15 min. The metabolite extraction protocols were also optimized by selecting a solvent for use in the study, the ratio of solvent to sample and sonication time. This method was used to profile two different parts of P. grandiflorum, i.e., the roots of P. grandiflorum (PR) and the stems and leaves of P. grandiflorum (PS), in the positive and negative ion modes. As a result, PR and PS showed qualitatively and quantitatively different metabolite profiles. Furthermore, their metabolite compositions differed according to individual plant samples. These results indicate that the UPLC-QTOF/MS-based profiling method is a good tool to analyze various metabolites in P. grandiflorum. This metabolomics approach can also be applied to evaluate the overall quality of P. grandiflorum, as well as to discriminate the cultivars for the medicinal plant industry. PMID:26569219

  8. Preparation and characterization of an immunoaffinity column for the selective extraction of aflatoxin B1 in 13 kinds of foodstuffs.

    PubMed

    Xie, Jie; Peng, Tao; He, Jian-Li; Shao, Yu; Fan, Chun-Lin; Chen, Ying; Jiang, Wen-Xiao; Chen, Min; Wang, Qi; Pei, Xing-Yao; Ding, Shuang-Yang; Jiang, Hai-Yang

    2015-08-15

    A rapid and reliable immunoaffinity column (IAC) clean-up based ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of aflatoxin B1 (AFB1) in cereals, peanuts, vegetable oils and Chinese traditional food products like sufu and lobster sauce. The immunoaffinity column of AFB1 (AFB1-IAC) was prepared by coupling CNBr-activated Sepharose-4B with the anti-AFB1 monoclonal antibody. The column capacity of IAC was over 260ng/mL gel. Samples were extracted with methanol-water (60:40, v/v) and the extracts were then purified on an AFB1-IAC before UPLC-MS/MS analysis. The average recoveries of AFB1 in spiked samples at levels of 1.0, 5.0 and 10.0μg/kg ranged from 72% to 98%, with the relative standard deviations of 1.2-9.3% (n=6). The limits of qualification ranged from 0.07 to 0.23μg/kg, which were below the MRLs of AFB1 in the matrices evaluated. In this work, the developed method was suitable for the determination of trace AFB1 residues in 13 kinds of foodstuffs. PMID:26160471

  9. Determination of a novel anticancer c-Met inhibitor LS-177 in rat plasma and tissues with a validated UPLC-MS/MS method: application to pharmacokinetics and tissue distribution study.

    PubMed

    Ju, Ping; Liu, Zhenzhen; Jiang, Yu; Zhao, Simin; Zhang, Lunhui; Zhang, Yuanyuan; Gu, Liqiang; Tang, Xing; Bi, Kaishun; Chen, Xiaohui

    2015-07-01

    LS-177 is a novel small-molecule kinase inhibitor employed to interrupt the c-Met signaling pathway. A rapid and sensitive ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for determination of LS-177 in rat plasma and tissues. The biosamples were extracted by liquid-liquid extraction with methyl tert-butyl ether and separated on a C18 column (50 × 4.6 mm, 2.6 µm) using a gradient elution mobile phase consisting of acetonitrile-0.1% formic acid water. Under the optimal conditions, the selectivity of the method was satisfactory with no endogenous interference. The intraday and interday precisions (relative standard deviation) were <10.5% and the accuracy (relative error) was from -12.5 to 12.5% at all quality control levels. Excellent recovery and negligible matrix effects were observed. Stability studies showed that LS-177 was stable during the preparation and analytical processes. The UPLC-MS/MS method was successfully applied to pharmacokinetic and tissue distribution studies. The results indicated that there was no significant drug accumulation after multiple-dose oral administration of LS-177. The tissue distribution study exhibited significant higher uptakes of LS-177 in stomach, intestine, lung and liver among all of the tissues. The results in pharmacokinetics and tissue distribution may provide a meaningful basis for clinical application.

  10. Determining trace amounts and the origin of formaldehyde impurity in Neisseria meningitidis A/C/Y/W-135-DT conjugate vaccine formulated in isotonic aqueous 1× PBS by improved C18-UPLC method.

    PubMed

    Gudlavalleti, Seshu K; Crawford, Erika N; Tran, Nhi N; Orten, Dana J; Harder, Jeffery D; Reddy, Jeeri R

    2015-03-25

    The ability to accurately measure and report trace amounts of residual formaldehyde impurity in a vaccine product is not only critical in the product release but also a regulatory requirement. In many bacterial or viral vaccine manufacturing procedures, formaldehyde is used either at a live culture inactivation step or at a protein de-toxification step or at both. Reported here is a validated and improved C18-UPLC method (developed based on previously published C-8 HPLC method) to determine the traces of formaldehyde process impurity in a liquid form Neisseria meningitidis A/C/Y/W-135-DT conjugate vaccine formulated in isotonic aqueous 1× PBS. UPLC C-18 column and the conditions described distinctly resolved the 2,4-DNPH-HCHO adduct from the un-reacted 2,4-DNPH as detected by TUV detector at 360 nm. This method was shown to be compatible with PBS formulation and extremely sensitive (with a quantitation limit of 0.05 ppm) and aided to determine formaldehyde contamination sources by evaluating the in-process materials as a track-down analysis. Final nanogram levels of formaldehyde in the formulated single dose vialed vaccine mainly originated from the diphtheria toxoid carrier protein used in the production of the conjugate vaccine, whereas relative contribution from polysaccharide API was minimal.

  11. UPLC-MS/MS determination of ephedrine, methylephedrine, amygdalin and glycyrrhizic acid in Beagle plasma and its application to a pharmacokinetic study after oral administration of Ma Huang Tang.

    PubMed

    Yan, Tianhua; Fu, Qiang; Wang, Jing; Ma, Shiping

    2015-02-01

    An ultra performance liquid chromatography-mass spectrometric (UPLC-MS) method was developed to investigate the pharmacokinetic properties of ephedrine, methylephedrine, amygdalin, and glycyrrhizic acid after oral gavage of Ma Huang Tang (MHT) in Beagles. Beagle plasma samples were pretreated using liquid-liquid extraction, and chromatographic separation was performed on a C18 column using a linear gradient of water-formic acid mixture (0.1%). The pharmacokinetic parameters of ephedrine, methylephedrine, amygdalin, and glycyrrhizic acid from MHT in Beagles were quantitatively determined by UPLC with tandem mass detector. The qualitative detection of the four compounds was accomplished by selected ion monitoring in negative/positive ion modes electrospray ionization-mass spectrometry (ESI-MS). Detection was based on multiple reaction monitoring with the precursor-to-product ion transitions m/z 166.096-116.983 (ephedrine), m/z 179.034-146.087 (methylephedrine), m/z 456.351-323.074 (amygdalin), and m/z 821.606-351.062 (glycyrrhizic acid). The selectivity, sensitivity, linearity, accuracy, precision, extraction recovery, ion suppression, and stability were within the acceptable ranges. The method described was successfully applied to reveal the pharmacokinetic properties of ephedrine, methylephedrine, amygdalin, and glycyrrhizic acid after oral gavage of MHT in Beagles.

  12. Columns in Clay

    ERIC Educational Resources Information Center

    Leenhouts, Robin

    2010-01-01

    This article describes a clay project for students studying Greece and Rome. It provides a wonderful way to learn slab construction techniques by making small clay column capitols. With this lesson, students learn architectural vocabulary and history, understand the importance of classical architectural forms and their influence on today's…

  13. A Column Dispersion Experiment.

    ERIC Educational Resources Information Center

    Corapcioglu, M. Y.; Koroglu, F.

    1982-01-01

    Crushed glass and a Rhodamine B solution are used in a one-dimensional optically scanned column experiment to study the dispersion phenomenon in porous media. Results indicate that the described model gave satisfactory results and that the dispersion process in this experiment is basically convective. (DC)

  14. 11. TIMBER COLUMN AND CAST IRON COLUMN CAP IN FIFTH ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    11. TIMBER COLUMN AND CAST IRON COLUMN CAP IN FIFTH FLOOR WAREHOUSE SPACE. VIEW TO SOUTHWEST. - Commercial & Industrial Buildings, Becker-Hazelton Company Warehouse, 280 Iowa Street, Dubuque, Dubuque County, IA

  15. Successfully downsize trayed columns

    SciTech Connect

    Sloley, A.W.; Fleming, B. )

    1994-03-01

    Techniques for the design and sizing of new trayed distillation columns are abundant in the literature. So, too, are the guidelines for modifying towers for operation beyond their original design range. Reducing capacity of distillation trays merits at least as much consideration. Indeed, lack of knowledge and experience in this area causes many tower failures and misdesigned columns. In this article, the authors present some practical design considerations, based on field experience, for tower trays operating at loadings dramatically lower than normal for a particular design. General considerations cover liquid and vapor hydraulics and flow behavior. Case studies are included for there typical units: a refinery vacuum crude still, a petrochemical superfractionator, and a steam stripper.

  16. Concurrent determination of olanzapine, risperidone and 9-hydroxyrisperidone in human plasma by ultra performance liquid chromatography with diode array detection method: application to pharmacokinetic study.

    PubMed

    Siva Selva Kumar, M; Ramanathan, M

    2016-02-01

    A simple and sensitive ultra-performance liquid chromatography (UPLC) method has been developed and validated for simultaneous estimation of olanzapine (OLZ), risperidone (RIS) and 9-hydroxyrisperidone (9-OHRIS) in human plasma in vitro. The sample preparation was performed by simple liquid-liquid extraction technique. The analytes were chromatographed on a Waters Acquity H class UPLC system using isocratic mobile phase conditions at a flow rate of 0.3 mL/min and Acquity UPLC BEH shield RP18 column maintained at 40°C. Quantification was performed on a photodiode array detector set at 277 nm and clozapine was used as internal standard (IS). OLZ, RIS, 9-OHRIS and IS retention times were found to be 0.9, 1.4, .1.8 and 3.1 min, respectively, and the total run time was 4 min. The method was validated for selectivity, specificity, recovery, linearity, accuracy, precision and sample stability. The calibration curve was linear over the concentration range 1-100 ng/mL for OLZ, RIS and 9-OHRIS. Intra- and inter-day precisions for OLZ, RIS and 9-OHRIS were found to be good with the coefficient of variation <6.96%, and the accuracy ranging from 97.55 to 105.41%, in human plasma. The validated UPLC method was successfully applied to the pharmacokinetic study of RIS and 9-OHRIS in human plasma.

  17. Column test-rig facility for column scanning studies

    NASA Astrophysics Data System (ADS)

    Zain, Rasif M.; Roslan, Y.

    2010-03-01

    Distillation columns are considered as one of the most critical components in oil and gas plants. The plant performance depends on the ability of these columns to function as intended. Defective columns may lead to serious consequences to the plant operation, and hence the quality of product. In order to perform any inspection techniques to distillation column for NDT practitioner, the best facility was designed when the adjustable defeats of distillation column test rig has been developed. The paper discussed the development and the function of this facility.

  18. Column test-rig facility for column scanning studies

    NASA Astrophysics Data System (ADS)

    Zain, Rasif M.; Roslan, Y.

    2009-12-01

    Distillation columns are considered as one of the most critical components in oil and gas plants. The plant performance depends on the ability of these columns to function as intended. Defective columns may lead to serious consequences to the plant operation, and hence the quality of product. In order to perform any inspection techniques to distillation column for NDT practitioner, the best facility was designed when the adjustable defeats of distillation column test rig has been developed. The paper discussed the development and the function of this facility.

  19. Quantitative and qualitative analysis of the novel antitumor 1,3,4-oxadiazole derivative (GLB) and its metabolites using HPLC-UV and UPLC-QTOF-MS

    PubMed Central

    Li, Pu; Wang, Xin; Li, Jian; Meng, Zhi-Yun; Li, Shu-Chun; Li, Zhong-Jun; Lu, Ying-Yuan; Ren, Hong; Lou, Ya-Qing; Lu, Chuang; Dou, Gui-Fang; Zhang, Guo-Liang

    2015-01-01

    Fructose-based 3-acetyl-2,3-dihydro-1,3,4-oxadiazole (GLB) is a novel antitumor agent and belongs to glycosylated spiro-heterocyclic oxadiazole scaffold derivative. This research first reported a simple, specific, sensitive and stable high performance liquid chromatography -ultraviolet detector (HPLC-UV) method for the quantitative determination of GLB in plasma. In this method, the chromatographic separation was achieved with a reversed phase C18 column. The calibration curve for GLB was linear at 300 nm. The lower limit of quantification was 10 ng/mL. The precision, accuracy and stability of the method were validated adequately. This method was successfully applied to the pharmacokinetic study in rats for detection of GLB after oral administration. Moreover, the structures of parent compound GLB and its two major metabolites M1 and M2 were identified in plasma using an ultra performance liquid chromatography- electrospray ionization-quadrupole-time of flight- mass spectrometry (UPLC-ESI-QTOF-MS) method. Our results indicated that the di-hydroxylation (M1) and hydroxylation (M2) of GLB are the major metabolites. In conclusion, the present study provided valuable information on an analytical method for the determination of GLB and its metabolites in rats, can be used to support further developing of this antitumor agent. PMID:26148672

  20. A novel UPLC-MS-MS method for simultaneous determination of seven uremic retention toxins with cardiovascular relevance in chronic kidney disease patients.

    PubMed

    Boelaert, Jente; Lynen, Frédéric; Glorieux, Griet; Eloot, Sunny; Van Landschoot, Maria; Waterloos, Marie-Anne; Sandra, Pat; Vanholder, Raymond

    2013-02-01

    Chronic kidney disease (CKD) is a devastating illness characterized by accumulation of uremic retention solutes in the body. The objective of this study was to develop and validate a simple, rapid, and robust UPLC-MS-MS method for simultaneous determination, in serum, of seven organic acid uremic retention toxins, namely uric acid (UA), hippuric acid (HA), indoxylsulfate (IS), p-cresylglucuronide (pCG), p-cresylsulfate (pCS), indole-3-acetic acid (IAA), and 3-carboxy-4-methyl-5-propyl-2-furanpropionic acid (CMPF). Isotopically labeled internal standards (d(5)-HA; 1,3-(15)N(2)-UA, and d(5)-IAA) were used to correct for variations in sample preparation and system performance. Separation on a C18 column was followed by negative electrospray ionization and tandem mass spectrometric detection. Accuracy was below the 15 % threshold. Within-day precision varied from 0.60 to 4.54 % and between-day precision was below 13.33 % for all compounds. The applicability of the method was evaluated by analyzing 78 serum samples originating both from healthy controls and from patients at different stages of CKD. These results were compared with those obtained by use of conventional HPLC-PDA-FLD methods. A good correlation was obtained between both methods for all compounds. PMID:23307120

  1. Ultrapressure liquid chromatography-tandem mass spectrometry assay using atmospheric pressure photoionization (UPLC-APPI-MS/MS) for quantification of 4-methoxydiphenylmethane in pharmacokinetic evaluation.

    PubMed

    Farhan, Nashid; Fitzpatrick, Sean; Shim, Yun M; Paige, Mikell; Chow, Diana Shu-Lian

    2016-09-01

    4-Methoxydiphenylmethane (4-MDM), a selective augmenter of Leukotriene A4 Hydrolase (LTA4H), is a new anti-inflammatory compound for potential treatment of chronic obstructive pulmonary disease (COPD). Currently, there is no liquid chromatography tandem mass spectrometric (LC-MS/MS) method for the quantification of 4-MDM. A major barrier for developing the LC-MS/MS method is the inability of electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) to ionize 4-MDM due to its hydrophobicity and lack of any functional group for ionization. With the advent of atmospheric pressure photoionization (APPI) technique, many hydrophobic compounds have been demonstrated to ionize by charge transfer reactions. In this study, a highly sensitive ultrapressure liquid chromatography tandem mass spectrometry assay using atmospheric pressure photoionization (UPLC-APPI-MS/MS) for the quantifications of 4-MDM in rat plasma has been developed and validated. 4-MDM was extracted from the plasma by solid phase extraction (SPE) and separated chromatographically using a reverse phase C8 column. The photoionization (PI) was achieved by introducing anisole as a dopant to promote the reaction of charge transfer. The assay with a linear range of 5 (LLOQ)-400ngmL(-1) met the regulatory requirements for accuracy, precision and stability. The validated assay was employed to quantify the plasma concentrations of 4-MDM after an oral dosing in Sprague Dawley (SD) rats.

  2. Simultaneous determination of 30 hormones illegally added to anti-ageing functional foods using UPLC-MS/MS coupled with SPE clean-up.

    PubMed

    He, Xiaoqin; Xi, Cunxian; Tang, Bobin; Wang, Guomin; Chen, Dongdong; Peng, Tao; Mu, Zhaode

    2014-01-01

    A novel analytical method employing solid-phase extraction (SPE) coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of 30 hormones in anti-ageing functional foods (capsules, powders and tablets). The analytes were extracted with acetic acid-acetonitrile (1-99 v/v), methanol and acetone, respectively. The extract was purified using a combined column, followed by analyte detection with electrospray ionisation in positive- or negative-ion modes. The results indicated that the 30 compounds had good linear correlations in the range of 1-1000 μg kg⁻¹, and the correlation coefficients were above 0.99. The limits of detection (LOD) and limits of quantification (LOQ) were 0.03-2 and 0.1-5 μg kg⁻¹, respectively. The average recovery of 30 compounds at the three spiked levels varied from 74.7% to 124.1%, and the relative standard deviation (RSD) was 2.4-15.0%. This method was applied to the analysis of hormones in 14 real samples of which seven hormones (such as estrone, dienestrol) were detected in four samples, but the remainder of the hormones were not detected. The developed method is sensitive, efficient, reliable and applicable to real samples.

  3. Time-resolved molecular characterization of organic aerosols by PILS + UPLC/ESI-Q-TOFMS

    NASA Astrophysics Data System (ADS)

    Zhang, X.; Dalleska, N. F.; Huang, D. D.; Bates, K. H.; Sorooshian, A.; Flagan, R. C.; Seinfeld, J. H.

    2016-04-01

    Real-time and quantitative measurement of particulate matter chemical composition represents one of the most challenging problems in the field of atmospheric chemistry. In the present study, we integrate the Particle-into-Liquid Sampler (PILS) with Ultra Performance Liquid Chromatography/Electrospray ionization Quadrupole Time-of-Flight High-Resolution/Mass Spectrometry (UPLC/ESI-Q-TOFMS) for the time-resolved molecular speciation of chamber-derived secondary organic aerosol (SOA). The unique aspect of the combination of these two well-proven techniques is to provide quantifiable molecular-level information of particle-phase organic compounds on timescales of minutes. We demonstrate that the application of the PILS + UPLC/ESI-Q-TOFMS method is not limited to water-soluble inorganic ions and organic carbon, but is extended to slightly water-soluble species through collection efficiency calibration together with sensitivity and linearity tests. By correlating the water solubility of individual species with their O:C ratio, a parameter that is available for aerosol ensembles as well, we define an average aerosol O:C ratio threshold of 0.3, above which the PILS overall particulate mass collection efficiency approaches ∼0.7. The PILS + UPLC/ESI-Q-TOFMS method can be potentially applied to probe the formation and evolution mechanism of a variety of biogenic and anthropogenic SOA systems in laboratory chamber experiments. We illustrate the application of this method to the reactive uptake of isoprene epoxydiols (IEPOX) on hydrated and acidic ammonium sulfate aerosols.

  4. [Analysis and identification of chemical constituents in Siwu decoction by UPLC-Q-TOF-MS(E)].

    PubMed

    Wang, Zhen-Fang; Zhao, Yang; Pang, Xu; Yu, He-Shui; Kang, Li-Ping; Gao, Yue; Ma, Bai-Ping

    2013-11-01

    This research analyzed the chemical constituents of Siwu decoction by UPLC-Q-TOF-MS(E). Base on the data of mass and related-literatures, 43 peaks were profiled and 25 compounds, which contain 8 monoterpene glycosides from Paeonia lactiflora and 13 phthalides from Rhizoma chuanxiong and Radix angelica sinensis mainly, were identified in both positive and negative mode respectively. Meanwhile, chemical constituents of water extract and 60% ethanol extract of Siwu decoction were compared by the principal constituent analysis with MarkerLynx software, which provides the basis for the active ingredients of Siwu decoction. PMID:24494558

  5. Simultaneous determination of four bioactive flavonoids from Polygonum orientale L. in dog plasma by UPLC-ESI-MS/MS and application of the technique to pharmacokinetic studies.

    PubMed

    Huang, Yong; Zhang, Peng; He, Feng; Zheng, Lin; Wang, Yong-lin; Wu, Ji-zhou

    2014-04-15

    The in vivo effects of traditional herbal medicines are generally mediated by multiple bioactive components. The main constituents of Polygonum orientale L. are flavonoids such as orientin, vitexin, cynaroside, and quercitrin. The aim of this study was to develop and validate a method for characterizing these flavonoids, in order to better understand the pharmacokinetics and pharmacodynamics of P. orientale L. We used ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) to analyze the flavonoids. After precipitation of the proteins with methanol, the flavonoids were separated on a BEH C18 column (50mm×2.1mm, i.d., 1.7μm) by using an elution gradient of acetonitrile. Flavonoid content was determined using the multiple reaction monitoring (MRM) mode at m/z 449.2→329.2 for orientin, m/z 433.2→313.0 for vitexin, m/z 449.2→287.1 for cynaroside, m/z 449.2→303.4 for quercitrin, and m/z 417.0→267.0 for the internal standard, puerarin. Pharmacokinetics was assessed after intravenous administration of P. orientale L. extracts (POE) in Beagle dogs at a dose of 22, 44, or 88mg/kg. Analysis of the standard curves by linear regression revealed high linearity over a 243-fold dynamic range for the four flavonoids (the lower limit of quantitation values were 4-21ng/mL). The relative standard deviations of intra- and inter-day measurements were less than 15.1%, and the method was accurate to within -8.7% to 7.2%; the extraction recoveries from dog plasma were 70.6-89.3%, 69.8-88.7%, 72.5-85.7%, and 71.0-79.1% for orientin, vitexin, cynaroside, and quercitrin, respectively. Our results suggest non-linear pharmacokinetic characteristics with rapid clearance of the flavonoids. In conclusion, UPLC-ESI-MS/MS is a rapid and sensitive method for simultaneous quantification of multiple flavonoids from POE in dog plasma and is suitable for pharmacokinetic studies of herbal medicines. PMID:24662144

  6. Quantification of lactose content in human and cow's milk using UPLC-tandem mass spectrometry.

    PubMed

    Fusch, Gerhard; Choi, Arum; Rochow, Niels; Fusch, Christoph

    2011-12-01

    A sensitive, accurate, and specific quantitative UPLC-MS/MS method was developed for lactose measurement of cow's and human milk and validated with cow's milk samples certified by an external laboratory. The new method employs only a dilution of raw cow's and human milk for simple preparation with no need to remove protein and fat prior to analysis with UPLC-MS/MS. It was operated in negative mode to detect lactose molecules and labeled (13)C(12)-lactose with the highest sensitivity. The principle advantages of the new LC-MS/MS method were: completed lactose determination in 5 min, absolute recovery of 97-107%, lower limit of detection <5 ng/L, and 99% linearity over the concentration range of 0.7-4.4 mg/L for both cow's and human milk. The mean lactose concentration of 51 human milk samples was measured as 56.8 ± 5.5 g/L ranging from 43 to 65 g/L. The described method represents validated lactose analysis with high accuracy and precision for a routine lactose determination in raw human milk.

  7. Comparative UPLC-QTOF-MS-based metabolomics and bioactivities analyses of Garcinia oblongifolia.

    PubMed

    Li, Ping; AnandhiSenthilkumar, Harini; Wu, Shi-biao; Liu, Bo; Guo, Zhi-yong; Fata, Jimmie E; Kennelly, Edward J; Long, Chun-lin

    2016-02-01

    Garcinia oblongifolia Champ. ex Benth. (Clusiaceae) is a well-known medicinal plant from southern China, with edible fruits. However, the phytochemistry and bioactivity of the different plant parts of G. oblongifolia have not been studied extensively. Comparative metabolic profiling and bioactivities of the leaf, branch, and fruit of G. oblongifolia were investigated. A total of 40 compounds such as biflavonoids, xanthones, and benzophenones were identified using UPLC-QTOF-MS and MS(E), including 15 compounds reported for the first time from this species. Heatmap analyses found that benzophenones, xanthones, and biflavonoids were predominately found in branches, with benzophenones present in relatively high concentrations in all three plant parts. Xanthones were found to have limited distribution in fruit while biflavonoids were present at only low levels in leaves. In addition, the cytotoxic (MCF-7 breast cancer cell line) and antioxidant (ABTS and DPPH chemical tests) activities of the crude extracts of G. oblongifolia indicate that the branch extract exhibits greater bioactivity than either the leaf or the fruit extracts. Orthogonal partial least squares discriminate analysis was used to find 12 marker compounds, mainly xanthones, from the branches, including well-known antioxidants and cytotoxic agents. These G. oblongifolia results revealed that the variation in metabolite profiles can be correlated to the differences in bioactivity of the three plant parts investigated. This UPLC-QTOF-MS strategy can be useful to identify bioactive constituents expressed differentially in the various plant parts of a single species. PMID:26773895

  8. UPLC-Q-TOF-MS analysis of non-volatile migrants from new active packaging materials.

    PubMed

    Aznar, M; Rodriguez-Lafuente, A; Alfaro, P; Nerin, C

    2012-10-01

    Ultra-performance liquid chromatography (UPLC) coupled to mass spectrometry (MS) is a useful tool in the analysis of non-volatile compounds, and the use of a quadrupole-time-of-flight (Q-TOF) mass analyzer allows a high sensitivity and accuracy when acquiring full fragment mode, providing a high assurance of correct identification of unknown compounds. In this work, UPLC-Q-TOF-MS technology has been applied to the analysis of non-volatile migrants from new active packaging materials. The materials tested were based on polypropylene (PP), ethylene-vinyl alcohol copolymer (EVOH), and poly(ethylene terephthalate) (PET). The active packaging materials studied were one PP film containing a natural antioxidant, and two PP/EVOH films, two PET/EVOH films and one coextruded PP/EVOH/PP film containing natural antimicrobials. The chemical structure of several compounds was unequivocally identified. The analysis revealed the migration of some of the active substances used in the manufacture of active packaging, such as caffeine (0.07 ± 0.01 μg/g), carvacrol (0.31 ± 0.03 μg/g) and citral (0.20 ± 0.01 μg/g). Unintentionally added substances were also found, such as citral reaction compounds, or citral impurities present in the raw materials. PMID:22836481

  9. Potentiometric detection in UPLC as an easy alternative to determine cocaine in biological samples.

    PubMed

    Daems, Devin; van Nuijs, Alexander L N; Covaci, Adrian; Hamidi-Asl, Ezat; Van Camp, Guy; Nagels, Luc J

    2015-07-01

    The analytical methods which are often used for the determination of cocaine in complex biological matrices are a prescreening immunoassay and confirmation by chromatography combined with mass spectrometry. We suggest an ultra-high-pressure liquid chromatography combined with a potentiometric detector, as a fast and practical method to detect and quantify cocaine in biological samples. An adsorption/desorption model was used to investigate the usefulness of the potentiometric detector to determine cocaine in complex matrices. Detection limits of 6.3 ng mL(-1) were obtained in plasma and urine, which is below the maximum residue limit (MRL) of 25 ng mL(-1). A set of seven plasma samples and 10 urine samples were classified identically by both methods as exceeding the MRL or being inferior to it. The results obtained with the UPLC/potentiometric detection method were compared with the results obtained with the UPLC/MS method for samples spiked with varying cocaine concentrations. The intraclass correlation coefficient was 0.997 for serum (n =7) and 0.977 for urine (n =8). As liquid chromatography is an established technique, and as potentiometry is very simple and cost-effective in terms of equipment, we believe that this method is potentially easy, inexpensive, fast and reliable.

  10. Comparative Metabolism of Cyclophosphamide and Ifosfamide in the Mouse Using UPLC-ESI-QTOFMS-Based Metabolomics

    PubMed Central

    Li, Fei; Patterson, Andrew D.; Höfer, Constance C.; Krausz, Kristopher W.; Gonzalez, Frank J.; Idle, Jeffrey R.

    2010-01-01

    Ifosfamide (IF) and cyclophosphamide (CP) are common chemotherapeutic agents. Interestingly, while the two drugs are isomers, only IF treatment is known to cause nephrotoxicity and neurotoxicity. Therefore, it was anticipated that a comparison of IF and CP drug metabolites in the mouse would reveal reasons for this selective toxicity. Drug metabolites were profiled by ultra-performance liquid chromatography-linked electrospray ionization quadrupole time-of-flight mass spectrometry (UPLC-ESI-QTOFMS), and the results analyzed by multivariate data analysis. Of the total 23 drug metabolites identified by UPLC-ESI-QTOFMS for both IF and CP, five were found to be novel. Ifosfamide preferentially underwent N-dechloroethylation, the pathway yielding 2-chloroacetaldehyde, while cyclophosphamide preferentially underwent ring-opening, the pathway yielding acrolein (AC). Additionally, S-carboxymethylcysteine and thiodiglycolic acid, two downstream IF and CP metabolites, were produced similarly in both IF- and CP-treated mice. This may suggest that other metabolites, perhaps precursors of thiodiglycolic acid, may be responsible for IF encephalopathy and nephropathy. PMID:20541539

  11. Classification of illicit heroin by UPLC-Q-TOF analysis of acidic and neutral manufacturing impurities.

    PubMed

    Liu, Cuimei; Hua, Zhendong; Bai, Yanping

    2015-12-01

    The illicit manufacture of heroin results in the formation of trace levels of acidic and neutral manufacturing impurities that provide valuable information about the manufacturing process used. In this work, a new ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF) method; that features high resolution, mass accuracy and sensitivity for profiling neutral and acidic heroin manufacturing impurities was developed. After the UPLC-Q-TOF analysis, the retention times and m/z data pairs of acidic and neutral manufacturing impurities were detected, and 19 peaks were found to be evidently different between heroin samples from "Golden Triangle" and "Golden Crescent". Based on the data set of these 19 impurities in 150 authentic heroin samples, classification of heroin geographic origins was successfully achieved utilizing partial least squares discriminant analysis (PLS-DA). By analyzing another data set of 267 authentic heroin samples, the developed discrimiant model was validated and proved to be accurate and reliable. PMID:26364155

  12. Identification and quantitation of new glutamic acid derivatives in soy sauce by UPLC/MS/MS.

    PubMed

    Frerot, Eric; Chen, Ting

    2013-10-01

    Glutamic acid is an abundant amino acid that lends a characteristic umami taste to foods. In fermented foods, glutamic acid can be found as a free amino acid formed by proteolysis or as a non-proteolytic derivative formed by microorganisms. The aim of the present study was to identify different structures of glutamic acid derivatives in a typical fermented protein-based food product, soy sauce. An acidic fraction was prepared with anion-exchange solid-phase extraction (SPE) and analyzed by UPLC/MS/MS and UPLC/TOF-MS. α-Glutamyl, γ-glutamyl, and pyroglutamyl dipeptides, as well as lactoyl amino acids, were identified in the acidic fraction of soy sauce. They were chemically synthesized for confirmation of their occurrence and quantified in the selected reaction monitoring (SRM) mode. Pyroglutamyl dipeptides accounted for 770 mg/kg of soy sauce, followed by lactoyl amino acids (135 mg/kg) and γ-glutamyl dipeptides (70 mg/kg). In addition, N-succinoylglutamic acid was identified for the first time in food as a minor compound in soy sauce (5 mg/kg).

  13. Analysis of Chemical Constituents in Wuzi-Yanzong-Wan by UPLC-ESI-LTQ-Orbitrap-MS.

    PubMed

    Zou, Dixin; Wang, Jinfeng; Zhang, Bo; Xie, Suhua; Wang, Qing; Xu, Kexin; Lin, Ruichao

    2015-12-01

    Wuzi-Yanzong-Wan (WZYZW), a classical traditional Chinese medicine (TCM) prescription containing Fructus Lych, Semen Cuscutae (fried), Fructus Rubi, Fructus Schisandrae chinensis (steamed) and Semen Plantaginis (fried with salt), is widely used to treat impotence, sterility, spermatorrhea, premature ejaculation, lumbago and post-micturation dribble. However, the chemical profile of WZYZW has not been established yet. In this work, a rapid and sensitive method for systematically screening and identifying the chemical constituents of WZYZW in both positive and negative ion modes using Ultra-Performance LC coupled with ESI-linear ion trap-Orbitrap tandem mass spectrometry (UPLC-ESI-LTQ-Orbitrap-MS) has been developed. Based on the chromatographic and spectrometric data, and referring to the literature, we could tentatively identify 106 compounds, including organic acids, flavonoids, phenylpropanoids, alkaloids and terpenoids. Fourteen ingredients from Fructus Lych were identified, while 10 ingredients were from Semen Cuscutae (fried), 33 ingredients were from Fructus Rubi, 37 ingredients were from Fructus Schisandrae chinensis (steamed), and 20 ingredients were from Semen Plantaginis (fried with salt). The results may provide essential data for further quality control, pharmacological research and clinical evaluation of WZYZW. Furthermore, this study indicates the developed approach based on UPLC-ESI-LTQ-Orbitrap-MS is suitable for characterizing the chemical profiles of TCM prescriptions. This is the first report to provide a comprehensive analysis of the chemical constituents of WZYZW.

  14. In vivo metabolite identification of bakuchiol in rats by UPLC/ESI-PDA-QTOF-MS.

    PubMed

    Hu, Chao; Liang, Qiande; Tang, Xianglin; Wang, Yuguang; Ma, Zengchun; Xiao, Chengrong; Tan, Hongling; Gao, Yue; Huang, Xianju

    2015-10-01

    Psoralea corylifolia L. is a traditional Chinese medicine for the treatment of various skin diseases such as psoriasis, vitiligo and chronic graft-versus-host. Bakuchiol, isolated from the seeds of P. corylifolia L., is one of the most important active compounds. To study the metabolic fate of bakuchiol in rats, an ultra performance liquid chromatography/electrospray ionization-photo diode array-quadrupole time of flight-mass spectrometry (UPLC/ESI-PDA-QTOF-MS) combined with MetaboLynx XS software was used, peak area-time curves of major metabolites in plasma from bakuchiol were determined. A total of 11 metabolites were identified after a single oral administration of bakuchiol, including 6 in plasma, 10 in bile, 8 in urine and 2 in feces, the metabolic transformation pathways of bakuchiol in rats included oxidation, hydroxylation, methylation, O-glucuronide conjugation and O-sulfate conjugation. In conclusion, this study expands our knowledge about the metabolism of bakuchiol which will be conducive to reveal its in vivo pharmacological and toxicological material basis, in addition, UPLC/ESI-PDA-QTOF-MS coupled with MetaboLynx XS software can be adopted as a useful tool for quick detection and identification of metabolites from medicine in vivo.

  15. Comparative study of three Plumbago L. species (Plumbaginaceae) by microscopy, UPLC-UV and HPTLC.

    PubMed

    Galal, Ahmed M; Raman, Vijayasankar; Avula, Bharathi; Wang, Yan-Hong; Rumalla, Chidananda Swamy; Weerasooriya, Aruna Dharmapriya; Khan, Ikhlas A

    2013-07-01

    This paper presents a comparative study of anatomy of leaves, stems and roots of three species of Plumbago, namely P. auriculata Lam., P. indica L. and P. zeylanica L. by light microscopy. The paper also provides qualitative and quantitative analysis of the naphthoquinone, plumbagin-a major constituent present in these species-using UPLC-UV. Microscopic examinations revealed the presence of distinctive differences in the anatomical features of the leaf, stem and root of the three species, and these can thus be used for identification and authentication of these species. UPLC-UV analysis showed the highest concentration of plumbagin in the roots of P. zeylanica (1.62% w/w) followed by the roots of P. indica (0.97% w/w) and then P. auriculata (0.33-0.53% w/w). In contrast, plumbagin was not detected in the stems and leaves of P. indica and in the leaves of P. auriculata, whereas very low concentrations (<0.02% w/w) of plumbagin were detected in the stems and leaves of P. zeylanica and in the stems of P. auriculata. HPTLC fingerprints of the leaf and root of the three species exhibited distinguishable profiles, while those of the stems were undifferentiated. PMID:23151906

  16. Determination of buprenorphine, fentanyl and LSD in whole blood by UPLC-MS-MS.

    PubMed

    Berg, Thomas; Jørgenrud, Benedicte; Strand, Dag Helge

    2013-04-01

    A sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method has been developed and validated for the quantification of buprenorphine, fentanyl and lysergic acid diethylamide (LSD) in whole blood. Sample preparation was performed by liquid-liquid extraction (LLE) with methyl tert-butyl ether. UPLC-MS-MS analysis was performed with a mobile phase consisting of ammonium formate (pH 10.2) and methanol. Positive electrospray ionization MS-MS detection was performed with two multiple reaction monitoring transitions for each of the analytes and the deuterium labeled internal standards. Limit of detection values of buprenorphine, fentanyl and LSD were 0.28, 0.044 and 0.0097 ng/mL and limit of quantification values were 0.94, 0.14 and 0.036 ng/mL, respectively. Most phospholipids were removed during LLE. No or only minor matrix effects were observed. The method has been routinely used at the Norwegian Institute of Public Health since September 2011 for qualitative and quantitative detections of buprenorphine, fentanyl and/or LSD in more than 400 whole blood samples with two replicates per sample.

  17. Pharmacokinetics of Dibutyl Phthalate (DBP) in the Rat Determined by UPLC-MS/MS

    PubMed Central

    Chang, Li-Wen; Hou, Mei-Ling; Tsai, Tung-Hu

    2013-01-01

    Dibutyl phthalate (DBP) is commonly used to increase the flexibility of plastics in industrial products. However, several plasticizers have been illegally used as clouding agents to increase dispersion of aqueous matrix in beverages. This study thus develops a rapid and validated analytical method by ultra-performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS) for the evaluation of pharmacokinetics of DBP in free moving rats. The UPLC-MS/MS system equipped with positive electrospray ionization (ESI) source in multiple reaction monitoring (MRM) mode was used to monitor m/z 279.25→148.93 transitions for DBP. The limit of quantification for DBP in rat plasma and feces was 0.05 μg/mL and 0.125 μg/g, respectively. The pharmacokinetic results demonstrate that DBP appeared to have a two-compartment model in the rats; the area under concentration versus time (AUC) was 57.8 ± 5.93 min μg/mL and the distribution and elimination half-life (t1/2,α and t1/2,β) were 5.77 ± 1.14 and 217 ± 131 min, respectively, after DBP administration (30 mg/kg, i.v.). About 0.18% of the administered dose was recovered from the feces within 48 h. The pharmacokinetic behavior demonstrated that DBP was quickly degraded within 2 h, suggesting a rapid metabolism low fecal cumulative excretion in the rat. PMID:23344044

  18. Determination of Glucocorticoids in UPLC-MS in Environmental Samples from an Occupational Setting

    PubMed Central

    Oddone, Enrico; Negri, Sara; Bellinzona, Massimo; Martino, Silvia; Di Tuccio, Marcello; Grignani, Elena; Cottica, Danilo; Imbriani, Marcello

    2015-01-01

    Occupational exposures to glucocorticoids are still a neglected issue in some work environments, including pharmaceutical plants. We developed an analytical method to quantify simultaneously 21 glucocorticoids using UPLC coupled with mass spectrometry to provide a basis to carry out environmental monitoring. Samples were taken from air, hand-washing tests, pad-tests and wipe-tests. This paper reports the contents of the analytical methodology, along with the results of this extensive environmental and personal monitoring of glucocorticoids. The method in UPLC-MS turned out to be suitable and effective for the aim of the study. Wipe-test and pad-test desorption was carried out using 50 mL syringes, a simple technique that saves time without adversely affecting analyte recovery. Results showed a widespread environmental pollution due to glucocorticoids. This is of particular concern. Evaluation of the dose absorbed by each worker and identification of a biomarker for occupational exposure will contribute to assessment and prevention of occupational exposure. PMID:25821468

  19. Rapid qualitative and quantitative analyses of proanthocyanidin oligomers and polymers by UPLC-MS/MS.

    PubMed

    Engström, Marica T; Pälijärvi, Maija; Fryganas, Christos; Grabber, John H; Mueller-Harvey, Irene; Salminen, Juha-Pekka

    2014-04-16

    This paper presents the development of a rapid method with ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the qualitative and quantitative analyses of plant proanthocyanidins directly from crude plant extracts. The method utilizes a range of cone voltages to achieve the depolymerization step in the ion source of both smaller oligomers and larger polymers. The formed depolymerization products are further fragmented in the collision cell to enable their selective detection. This UPLC-MS/MS method is able to separately quantitate the terminal and extension units of the most common proanthocyanidin subclasses, that is, procyanidins and prodelphinidins. The resulting data enable (1) quantitation of the total proanthocyanidin content, (2) quantitation of total procyanidins and prodelphinidins including the procyanidin/prodelphinidin ratio, (3) estimation of the mean degree of polymerization for the oligomers and polymers, and (4) estimation of how the different procyanidin and prodelphinidin types are distributed along the chromatographic hump typically produced by large proanthocyanidins. All of this is achieved within the 10 min period of analysis, which makes the presented method a significant addition to the chemistry tools currently available for the qualitative and quantitative analyses of complex proanthocyanidin mixtures from plant extracts.

  20. SPIRAL CONTACTOR FOR SOLVENT EXTRACTION COLUMN

    DOEpatents

    Cooley, C.R.

    1961-06-13

    The patented extraction apparatus includes a column, perforated plates extending across the column, liquid pulse means connected to the column, and an imperforate spiral ribbon along the length of the column.

  1. Why Hexagonal Basalt Columns?

    PubMed

    Hofmann, Martin; Anderssohn, Robert; Bahr, Hans-Achim; Weiß, Hans-Jürgen; Nellesen, Jens

    2015-10-01

    Basalt columns with their preferably hexagonal cross sections are a fascinating example of pattern formation by crack propagation. Junctions of three propagating crack faces rearrange such that the initial right angles between them tend to approach 120°, which enables the cracks to form a pattern of regular hexagons. To promote understanding of the path on which the ideal configuration can be reached, two periodically repeatable models are presented here involving linear elastic fracture mechanics and applying the principle of maximum energy release rate. They describe the evolution of the crack pattern as a transition from rectangular start configuration to the hexagonal pattern. This is done analytically and by means of three-dimensional finite element simulation. The latter technique reproduces the curved crack path involved in this transition.

  2. Why Hexagonal Basalt Columns?

    PubMed

    Hofmann, Martin; Anderssohn, Robert; Bahr, Hans-Achim; Weiß, Hans-Jürgen; Nellesen, Jens

    2015-10-01

    Basalt columns with their preferably hexagonal cross sections are a fascinating example of pattern formation by crack propagation. Junctions of three propagating crack faces rearrange such that the initial right angles between them tend to approach 120°, which enables the cracks to form a pattern of regular hexagons. To promote understanding of the path on which the ideal configuration can be reached, two periodically repeatable models are presented here involving linear elastic fracture mechanics and applying the principle of maximum energy release rate. They describe the evolution of the crack pattern as a transition from rectangular start configuration to the hexagonal pattern. This is done analytically and by means of three-dimensional finite element simulation. The latter technique reproduces the curved crack path involved in this transition. PMID:26550724

  3. Buckling of a holey column.

    PubMed

    Pihler-Puzović, D; Hazel, A L; Mullin, T

    2016-09-14

    We report the results from a combined experimental and numerical investigation of buckling in a novel variant of an elastic column under axial load. We find that including a regular line of centred holes in the column can prevent conventional, global, lateral buckling. Instead, the local microstructure introduced by the holes allows the column to buckle in an entirely different, internal, mode in which the holes are compressed in alternate directions, but the column maintains the lateral reflection symmetry about its centreline. The internal buckling mode can be accommodated within a smaller external space than the global one; and it is the preferred buckling mode over an intermediate range of column lengths for sufficiently large holes. For very short or sufficiently long columns a modification of the classical, global, lateral buckling is dominant. PMID:27501288

  4. Determination of sotolon content in South African white wines by two novel HPLC-UV and UPLC-MS methods.

    PubMed

    Gabrielli, Mario; Buica, Astrid; Fracassetti, Daniela; Stander, Marietjie; Tirelli, Antonio; du Toit, Wessel J

    2015-02-15

    Sotolon has been reported to play an important role in the atypical ageing and aroma character of many wines. A number of analytical techniques for sotolon analysis in wine have been reported, but these often require extensive sample preparation. In this work we report a HPLC-UV method and a novel UPLC-MS method to determine sotolon concentrations in white wines with little sample preparation applied for the first time for the evaluation of sotolon levels in South African wines. The validation showed that the instrumental methods had good accuracy, repeatability and linearity, but the UPLC-MS method proved more sensitive. For both methods, quantification limits were lower than the sotolon odour threshold in wine (10μg/L), 0.86μg/L and 0.013μg/L, for HPLC-UV and UPLC-MS methods, respectively. Sotolon levels in 65 South African white wines were often found to be lower than the reported odour threshold, with the highest concentration being 9.11μg/L. However, for low levels (<1μg/L), unknown interferences in certain wines led to sotolon not being quantified with the HPLC-UV method, which made the UPLC-MS method more suitable.

  5. Analytical methods for determination of alkaloids and saponins from roots of Caulophyllum thalictroids (L) Michx using UPLC HPLC and HPTLC

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A comparison study of analytical methods including HPLC, UPLC and HPTLC are presented in this paper for the determination of major alkaloid and triterpene saponins from the roots of Caulophyllum thalictroides (L.) Michx. (blue cohosh) and dietary supplements claiming to contain blue cohosh. The meth...

  6. DETERMINATION OF ECOLOGICALLY RELEVANT PHARMACEUTICALS AND THEIR SELECTED METABOLITES IN EFFLUENT AND SURFACE WATER USING UPLC/MS/MS

    EPA Science Inventory

    Objective is to develop analytical methods including SPE and UPLC/MS/MS needed to analyze over 60 human prescription pharamceuticals and metabolites belonging to a multitude of different classes in surface waters and wastewater effluent. The methods will be used in future studies...

  7. Compact electron beam focusing column

    SciTech Connect

    Persaud, Arun; Leung, Ka-Ngo; Reijonen, Jani

    2001-07-13

    A novel design for an electron beam focusing column has been developed at LBNL. The design is based on a low-energy spread multicusp plasma source which is used as a cathode for electron beam production. The focusing column is 10 mm in length. The electron beam is focused by means of electrostatic fields. The column is designed for a maximum voltage of 50 kV. Simulations of the electron trajectories have been performed by using the 2-D simulation code IGUN and EGUN. The electron temperature has also been incorporated into the simulations. The electron beam simulations, column design and fabrication will be discussed in this presentation.

  8. 45. MAIN MEETING ROOM COLUMNS. Ends of gallery columns identified ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    45. MAIN MEETING ROOM COLUMNS. Ends of gallery columns identified at the time of removal for transfer to the George School for re-erection. The stamp reads, 'REMOVED FROM 12th ST. MTG HSE PHILA 1972'. - Twelfth Street Meeting House, 20 South Twelfth Street, Philadelphia, Philadelphia County, PA

  9. UPLC and LC-MS studies on degradation behavior of irinotecan hydrochloride and development of a validated stability-indicating ultra-performance liquid chromatographic method for determination of irinotecan hydrochloride and its impurities in pharmaceutical dosage forms.

    PubMed

    Kumar, Navneet; Sangeetha, Dhanaraj; Reddy, Sunil P

    2012-10-01

    The objective of the current investigation was to study the degradation behavior of irinotecan hydrochloride under different International Conference on Harmonization (ICH) recommended stress conditions using ultra-performance liquid chromatography and liquid chromatography-mass spectrometry and to establish a validated stability-indicating reverse-phase ultra-performance liquid chromatographic method for the quantitative determination of irinotecan hydrochloride and its seven impurities and degradation products in pharmaceutical dosage forms. Irinotecan hydrochloride was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Irinotecan hydrochloride was found to degrade significantly in oxidative and base hydrolysis and photolytic degradation conditions. The degradation products were well resolved from the main peak and its impurities, thus proving the stability-indicating power of the method. Chromatographic separation was achieved on a Waters Acquity BEH C8 (100 × 2.1 mm) 1.7-µm column with a mobile phase containing a gradient mixture of solvent A (0.02M KH(2)PO(4) buffer, pH 3.4) and solvent B (a mixture of acetonitrile and methanol in the ratio of 62:38 v/v). The mobile phase was delivered at a flow rate of 0.3 mL/min with ultraviolet detection at 220 nm. The run time was 8 min, within which irinotecan and its seven impurities and degradation products were satisfactorily separated. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness. This method was also suitable for the assay determination of irinotecan hydrochloride in pharmaceutical dosage forms.

  10. Determination of a selection of anti-epileptic drugs and two active metabolites in whole blood by reversed phase UPLC-MS/MS and some examples of application of the method in forensic toxicology cases.

    PubMed

    Karinen, Ritva; Vindenes, Vigdis; Hasvold, Inger; Olsen, Kirsten Midtbøen; Christophersen, Asbjørg S; Øiestad, Elisabeth

    2015-07-01

    Quantitative determination of anti-epileptic drug concentrations is of great importance in forensic toxicology cases. Although the drugs are not usually abused, they are important post-mortem cases where the question of both lack of compliance and accidental or deliberate poisoning might be raised. In addition these drugs can be relevant for driving under the influence cases. A reversed phase ultra-performance liquid chromatography-tandem mass spectrometry method has been developed for the quantitative analysis of the anti-epileptic compounds carbamazepine, carbamazepine-10,11-epoxide, gabapentin, lamotrigine, levetiracetam, oxcarbazepine, 10-OH-carbazepine, phenobarbital, phenytoin, pregabalin, and topiramate in whole blood, using 0.1 mL sample volume with methaqualone as internal standard. Sample preparation was a simple protein precipitation with acetonitrile and methanol. The diluted supernatant was directly injected into the chromatographic system. Separation was performed on an Acquity UPLC® BEH Phenyl column with gradient elution and a mildly alkaline mobile phase. The mass spectrometric detection was performed in positive ion mode, except for phenobarbital, and multiple reaction monitoring was used for drug quantification. The limits of quantification for the different anti-epileptic drugs varied from 0.064 to 1.26 mg/L in blood, within-day and day-to-day relative standard deviations from 2.2 to 14.7% except for phenobarbital. Between-day variation for phenobarbital was 20.4% at the concentration level of 3.5 mg/L. The biases for all compounds were within ±17.5%. The recoveries ranged between 85 and 120%. The corrected matrix effects were 88-106% and 84-110% in ante-mortem and post-mortem whole blood samples, respectively.

  11. A UPLC-MS Method for Simultaneous Determination of Geniposidic Acid, Two Lignans and Phenolics in Rat Plasma and its Application to Pharmacokinetic Studies of Eucommia ulmoides Extract in Rats.

    PubMed

    Li, Yongjun; Gong, Zipeng; Cao, Xu; Wang, Yonglin; Wang, Aimin; Zheng, Lin; Huang, Yong; Lan, Yanyu

    2016-10-01

    The bark of Eucommia ulmoides is a well-known Chinese herbal medicine that is used to regulate blood pressure and reduce blood sugar and fats, as well as an antioxidant and antimicrobial agent. Here we describe the development of a sensitive ultrahigh performance liquid chromatography-tandem mass spectrum method for the simultaneous determination of five major active ingredients of E. ulmoides bark extract, namely, geniposidic acid (GA), protocatechuic acid (PCA), chlorogenic acid (CA), (+)-pinoresinol di-O-β-D-glucopyranoside (PDG) and (+)-pinoresinol 4'-O-β-D-glucopyranoside (PG), in rat plasma. The preliminary steps in the plasma analysis were the addition of an internal standard and acidification (0.1 % formic acid), followed by protein precipitation with methanol. Separation of the active ingredients was performed on an ACQUITY UPLC® BEH C18 column (2.1 × 50 mm; internal diameter 1.7 µm) at a flow rate of 0.35 mL/min, with acetonitrile/water containing 0.1 % formic acid as the mobile phase. Detection was performed on a triple quadrupole tandem mass spectrometer via electrospray ionization source with positive and negative ionization modes. All calibration curves showed good linearity (r ≥ 0.997) over the concentration range with the low limit of quantification between 4.45 and 54.9 ng/mL. Precision was evaluated by intra- and inter-day assays, and the percentages of the relative standard deviation were all within 15 %. Extraction efficiency and matrix effect were 84.3-102.4 % and 98.1-112.2 %, respectively. The validated method was successfully applied to the pharmacokinetic study in rats after oral administration of E. ulmoides extract. The results indicate that the pharmacokinetic properties of GA differ from those of PCA, CA, PDG and PG, respectively.

  12. Identification and Quantitation of Anthocyanins in Purple-Fleshed Sweet Potatoes Cultivated in China by UPLC-PDA and UPLC-QTOF-MS/MS.

    PubMed

    He, Wei; Zeng, Maomao; Chen, Jie; Jiao, Yuzhi; Niu, Fuxiang; Tao, Guanjun; Zhang, Shuang; Qin, Fang; He, Zhiyong

    2016-01-13

    The identification and quantitation of the anthocyanins in 12 purple-fleshed sweet potato (PFSP) cultivars ('Jihei 1', 'Xuzi 3', 'Xuzi 6', 'Zhezi 4', 'Ningzi 1', 'Ningzi 2', 'Ningzi 3', 'Ning 2-2', 'Ning 6-8', 'Guangzi 1', 'Ziluolan', and 'Qinzi 1') in China were carried out using a combination of ultraperformance liquid chromatography-photodiode array (UPLC-PDA), quadrupole-time-of-flight mass spectrometry (QTOF-MS), and tandem mass spectrometry (MS/MS) analyses. Thirteen acylated anthocyanins were tentatively characterized, including two new PFSP anthocyanins, cyanidin 3-caffeoyl-vanilloyl sophoroside-5-glucoside and peonidin 3-caffeoyl-vanilloyl sophoroside-5-glucoside. The quantitative analyses of these anthocyanins were conducted using cyanidin 3-O-glucoside as a standard. The total anthocyanin content of the PFSPs depended on the cultivar. The five PFSP cultivars with the highest content of anthocyanins were 'Jihei 1', 'Xuzi 3', 'Zhezi 4', 'Ziluolan', and 'Qinzi 1'. This is the first report of the 'Ningzi 2', 'Ningzi 3', and 'Ning 2-2' PFSP cultivars containing only diacylated anthocyanins and of the 'Xuzi 6' cultivar containing single anthocyanidin-based anthocyanins.

  13. Identification and Quantitation of Anthocyanins in Purple-Fleshed Sweet Potatoes Cultivated in China by UPLC-PDA and UPLC-QTOF-MS/MS.

    PubMed

    He, Wei; Zeng, Maomao; Chen, Jie; Jiao, Yuzhi; Niu, Fuxiang; Tao, Guanjun; Zhang, Shuang; Qin, Fang; He, Zhiyong

    2016-01-13

    The identification and quantitation of the anthocyanins in 12 purple-fleshed sweet potato (PFSP) cultivars ('Jihei 1', 'Xuzi 3', 'Xuzi 6', 'Zhezi 4', 'Ningzi 1', 'Ningzi 2', 'Ningzi 3', 'Ning 2-2', 'Ning 6-8', 'Guangzi 1', 'Ziluolan', and 'Qinzi 1') in China were carried out using a combination of ultraperformance liquid chromatography-photodiode array (UPLC-PDA), quadrupole-time-of-flight mass spectrometry (QTOF-MS), and tandem mass spectrometry (MS/MS) analyses. Thirteen acylated anthocyanins were tentatively characterized, including two new PFSP anthocyanins, cyanidin 3-caffeoyl-vanilloyl sophoroside-5-glucoside and peonidin 3-caffeoyl-vanilloyl sophoroside-5-glucoside. The quantitative analyses of these anthocyanins were conducted using cyanidin 3-O-glucoside as a standard. The total anthocyanin content of the PFSPs depended on the cultivar. The five PFSP cultivars with the highest content of anthocyanins were 'Jihei 1', 'Xuzi 3', 'Zhezi 4', 'Ziluolan', and 'Qinzi 1'. This is the first report of the 'Ningzi 2', 'Ningzi 3', and 'Ning 2-2' PFSP cultivars containing only diacylated anthocyanins and of the 'Xuzi 6' cultivar containing single anthocyanidin-based anthocyanins. PMID:26687974

  14. Dorsal column stimulator applications

    PubMed Central

    Yampolsky, Claudio; Hem, Santiago; Bendersky, Damián

    2012-01-01

    Background: Spinal cord stimulation (SCS) has been used to treat neuropathic pain since 1967. Following that, technological progress, among other advances, helped SCS become an effective tool to reduce pain. Methods: This article is a non-systematic review of the mechanism of action, indications, results, programming parameters, complications, and cost-effectiveness of SCS. Results: In spite of the existence of several studies that try to prove the mechanism of action of SCS, it still remains unknown. The mechanism of action of SCS would be based on the antidromic activation of the dorsal column fibers, which activate the inhibitory interneurons within the dorsal horn. At present, the indications of SCS are being revised constantly, while new applications are being proposed and researched worldwide. Failed back surgery syndrome (FBSS) is the most common indication for SCS, whereas, the complex regional pain syndrome (CRPS) is the second one. Also, this technique is useful in patients with refractory angina and critical limb ischemia, in whom surgical or endovascular treatment cannot be performed. Further indications may be phantom limb pain, chronic intractable pain located in the head, face, neck, or upper extremities, spinal lumbar stenosis in patients who are not surgical candidates, and others. Conclusion: Spinal cord stimulation is a useful tool for neuromodulation, if an accurate patient selection is carried out prior, which should include a trial period. Undoubtedly, this proper selection and a better knowledge of its underlying mechanisms of action, will allow this cutting edge technique to be more acceptable among pain physicians. PMID:23230533

  15. An Undergraduate Column Chromatography Experiment.

    ERIC Educational Resources Information Center

    Danot, M.; And Others

    1984-01-01

    Background information, list of materials needed, and procedures used are provided for an experiment designed to introduce undergraduate students to the theoretical and technical aspects of column chromatography. The experiment can also be shortened to serve as a demonstration of the column chromatography technique. (JN)

  16. Analyze distillation columns with thermodynamics

    SciTech Connect

    Ognisty, T.P. )

    1995-02-01

    In a distillation column, heat supplies the work for separating the components of a feed stream into products. Distillation columns consume some 95% of the total energy used in separations. This amounts to roughly 3% of the energy consumed in the US. Since distillation is so energy intensive and requires significant capital outlays, an endless quest to improve the economics has continued since the beginning of the industry. By analyzing the thermodynamics of a distillation column, an engineer can quantify the thermodynamic efficiency of the process, identify the regions where energy can be better utilized, and define the minimum targets for energy consumption. This article reviews the principles of distillation column thermodynamics and outlines the analysis of lost work profiles and column heat profiles. It then illustrates these concepts through three examples.

  17. Mush Column Magma Chambers

    NASA Astrophysics Data System (ADS)

    Marsh, B. D.

    2002-12-01

    Magma chambers are a necessary concept in understanding the chemical and physical evolution of magma. The concept may well be similar to a transfer function in circuit or time series analysis. It does what needs to be done to transform source magma into eruptible magma. In gravity and geodetic interpretations the causative body is (usually of necessity) geometrically simple and of limited vertical extent; it is clearly difficult to `see' through the uppermost manifestation of the concentrated magma. The presence of plutons in the upper crust has reinforced the view that magma chambers are large pots of magma, but as in the physical representation of a transfer function, actual magma chambers are clearly distinct from virtual magma chambers. Two key features to understanding magmatic systems are that they are vertically integrated over large distances (e.g., 30-100 km), and that all local magmatic processes are controlled by solidification fronts. Heat transfer considerations show that any viable volcanic system must be supported by a vertically extensive plumbing system. Field and geophysical studies point to a common theme of an interconnected stack of sill-like structures extending to great depth. This is a magmatic Mush Column. The large-scale (10s of km) structure resembles the vertical structure inferred at large volcanic centers like Hawaii (e.g., Ryan et al.), and the fine scale (10s to 100s of m) structure is exemplified by ophiolites and deeply eroded sill complexes like the Ferrar dolerites of the McMurdo Dry Valleys, Antarctica. The local length scales of the sill reservoirs and interconnecting conduits produce a rich spectrum of crystallization environments with distinct solidification time scales. Extensive horizontal and vertical mushy walls provide conditions conducive to specific processes of differentiation from solidification front instability to sidewall porous flow and wall rock slumping. The size, strength, and time series of eruptive behavior

  18. Rapid analysis of avenacosides in grain and husks of oats by UPLC-TQ-MS.

    PubMed

    Pecio, Łukasz; Wawrzyniak-Szołkowska, Aleksandra; Oleszek, Wiesław; Stochmal, Anna

    2013-12-01

    Avenacosides A (AA) and B (AB) as well as 26-desglucoavenacoside A (26dAA) were quantified in oats using rapid and sensitive method utilising UPLC-TQ-MS. In the grain, AA and AB were revealed as the primary saponins, whereas in the husks, dAA was predominant. Inconsistent with the published data, observed concentrations of AA and AB in the grain were very similar. Presumably, this is due to higher sensitivity and better selectivity of the mass spectrometry-based quantification method, thus allowing for more precise measurements. Elevated level of an active fungicidal form of saponin, dAA in the husks possibly indicates they are more prone to fungal attacks.

  19. Metabolites profiling of Chrysanthemum pacificum Nakai parts using UPLC-PDA-MS coupled to chemometrics.

    PubMed

    Farag, Nermeen F; Farag, Mohamed A; Abdelrahman, Enas H; Azzam, Shadia M; El-Kashoury, El-Sayeda A

    2015-01-01

    Methanol-soluble constituents from the flowers, non-flowering aerial parts and roots of Chrysanthemum pacificum Nakai were analysed via high resolution UPLC-PDA-qTOF-MS followed by chemometrics. Forty-seven chromatographic peaks belonging to various metabolite classes were detected. Most metabolite classes showed qualitative and quantitative differences across parts, with luteolin conjugates being mostly enriched in flowers whereas non-flowering aerial parts contained mostly quercetin and methoxylated flavone conjugates. Root sample ranked the lowest for all flavones and dicaffeoylquinic acids. In contrast, 1,5-di-caffeoylquinic acid levels were found at high levels in flowers and aerial parts reaching 3145 and 1390 μg/g, respectively, suggesting that C. pacificum could serve as a natural resource of this well-recognised anti-hepatotoxic phenolic. Principal component analysis was further used for organs classification in an untargeted manner. This study provides the first map of secondary metabolites distribution in C. pacificum Nakai organs.

  20. Novel identification strategy for ground coffee adulteration based on UPLC-HRMS oligosaccharide profiling.

    PubMed

    Cai, Tie; Ting, Hu; Jin-Lan, Zhang

    2016-01-01

    Coffee is one of the most common and most valuable beverages. According to International Coffee Organization (ICO) reports, the adulteration of coffee for financial reasons is regarded as the most serious threat to the sustainable development of the coffee market. In this work, a novel strategy for adulteration identification in ground coffee was developed based on UPLC-HRMS oligosaccharide profiling. Along with integrated statistical analysis, 17 oligosaccharide composition were identified as markers for the identification of soybeans and rice in ground coffee. This strategy, validated by manual mixtures, optimized both the reliability and authority of adulteration identification. Rice and soybean adulterants present in ground coffee in amounts as low as 5% were identified and evaluated. Some commercial ground coffees were also successfully tested using this strategy.

  1. Novel identification strategy for ground coffee adulteration based on UPLC-HRMS oligosaccharide profiling.

    PubMed

    Cai, Tie; Ting, Hu; Jin-Lan, Zhang

    2016-01-01

    Coffee is one of the most common and most valuable beverages. According to International Coffee Organization (ICO) reports, the adulteration of coffee for financial reasons is regarded as the most serious threat to the sustainable development of the coffee market. In this work, a novel strategy for adulteration identification in ground coffee was developed based on UPLC-HRMS oligosaccharide profiling. Along with integrated statistical analysis, 17 oligosaccharide composition were identified as markers for the identification of soybeans and rice in ground coffee. This strategy, validated by manual mixtures, optimized both the reliability and authority of adulteration identification. Rice and soybean adulterants present in ground coffee in amounts as low as 5% were identified and evaluated. Some commercial ground coffees were also successfully tested using this strategy. PMID:26213074

  2. Free amino acid profiling in the giant puffball mushroom (Calvatia gigantea) using UPLC-MS/MS.

    PubMed

    Kıvrak, İbrahim; Kıvrak, Şeyda; Harmandar, Mansur

    2014-09-01

    Wild edible and medicinal mushroom, Calvatia gigantea, was quantitatively analyzed for the determination of its free amino acids using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The concentrations of total free amino acids, essential and non-essential amino acids were 199.65 mg/100 g, 113.69 mg/100 g, and 85.96 mg/100 g in C. gigantea, respectively. This study showed that C. gigantea, so called a giant puffball mushroom, has free amino acids content. The essential amino acids: tryptophan, isoleucine, valine, phenylalanine, leucine, threonine, lysine, histidine, methionine, and the non-essential amino acids: tyrosine, 4-hyrdroxy proline, arginine, proline, glycine, serine, alanine, glutamine, glutamic acid, aspargine, aspartic acid were detected.

  3. [Characterization and comparison of interferon reference standards using UPLC-MS].

    PubMed

    Tao, Lei; Pei, De-ning; Han, Chun-mei; Chen, Wei; Rao, Chun-ming; Wang, Jun-zhi

    2015-01-01

    The study aims to characterize and compare interferon reference standards from 5 manufacturers. By testing molecular mass and trypsin-digested peptide mass mapping, the amino acid sequence was verified and post-translational modifications such as disulfide bond were identified. Results show that the molecular mass and amino acid sequence were consistent with theory; the disulfide bonds of 4 lots of interferon were Cys1-Cys98/Cys29-Cys138, 1 lot was Cys29-Cys139/Cys86-Cys99; N-terminal "+Met", acetyl N-terminal and Met oxidation were identified in part of the sample. UPLC-MS can be used to characterize and compare interferon reference standards from different manufacturers.

  4. Assessment of fruit juice authenticity using UPLC-QToF MS: a metabolomics approach.

    PubMed

    Jandrić, Z; Roberts, D; Rathor, M N; Abrahim, A; Islam, M; Cannavan, A

    2014-04-01

    In recent years, with the growing complexity of global food supply chains and trade, food fraud, including adulteration of high value foods with cheaper substitutes, has become an increasingly important issue. A metabolomics approach can be applied to discover biomarkers that can be used to trace food adulteration. A study was undertaken to discover novel, potential biomarkers for the rapid detection of the adulteration of fruit juices with cheaper alternatives. Pineapple, orange, grapefruit, apple, clementine, and pomelo were investigated. Untargeted metabolite fingerprinting was performed by UPLC-QToF MS with multivariate data analysis. Twenty-one differential metabolites were selected, contributing to the separation between pineapple, orange and grapefruit juices, and their admixtures down to 1% adulteration level. A targeted metabolomics method was then optimised and adulteration could be detected at 1%. The results demonstrate that metabolomics has potential as a screening tool for the rapid detection of food adulteration.

  5. Rapid screening of mycotoxins in liquid milk and milk powder by automated size-exclusion SPE-UPLC-MS/MS and quantification of matrix effects over the whole chromatographic run.

    PubMed

    Wang, Xiupin; Li, Peiwu

    2015-04-15

    An automated, size-exclusion solid phase extraction (SPE)-UPLC-MS/MS protocol without pre-treatment of samples was developed to screen for four mycotoxins (OTA, ZEN, AFB1, and AFM1) in liquid milk and milk powder. Firstly, a mixed macropore-silica gel cartridge was established as a size-exclusion SPE column. The proposed methodology could be a candidate in green analytical chemistry because it saves on manpower and organic solvent. Permanent post-column infusion of mycotoxin standards was used to quantify matrix effects throughout the chromatographic run. Matrix-matched calibration could effectively compensate for matrix effects, which may be caused by liquid milk or milk powder matrix. Recovery of the four mycotoxins in fortified liquid milk was in the range 89-120% and RSD 2-9%. The LOD for the four mycotoxins in liquid milk and milk powder were 0.05-2 ng L(-1) and 0.25-10 ng kg(-1), respectively. The LOQ for the four mycotoxins in liquid milk and milk powder were 0.1-5 ng L(-1) and 0.5-25 ng kg(-1), respectively.

  6. Microbial activity in weathering columns.

    PubMed

    García, C; Ballester, A; González, F; Blázquez, M L

    2007-03-22

    The aim of the present work was to evaluate the metabolic activity of the microbial population associated with a pyritic tailing after a column-weathering test. For this purpose, a column 150cm high and 15cm diameter was used. The solid was a tailing with 63.4% pyrite and with minor amounts of Cu, Pb and Zn sulfides (1.4, 0.5 and 0.8%, respectively). The column model was the habitual one for weathering tests: distilled water was added at the top of the column; the water flowed down through tailings and finally was collected at the bottom for chemical and microbiological analysis. Weathering was maintained for 36 weeks. The results showed a significant presence of microbial life that was distributed selectively over the column: sulfur- and iron-oxidizing aerobic bacteria were in the more oxygenated zone; anaerobic sulfur-reducing bacteria were isolated from the samples taken from the anoxic part of the column. Activity testing showed that (oxidizing and reducing) bacteria populations were active at the end of the weathering test. The quality of the water draining from the column was thus the final product of biological oxidation and reduction promoted by the bacteria consortia.

  7. Post column derivatisation analyses review. Is post-column derivatisation incompatible with modern HPLC columns?

    PubMed

    Jones, Andrew; Pravadali-Cekic, Sercan; Dennis, Gary R; Shalliker, R Andrew

    2015-08-19

    Post Column derivatisation (PCD) coupled with high performance liquid chromatography or ultra-high performance liquid chromatography is a powerful tool in the modern analytical laboratory, or at least it should be. One drawback with PCD techniques is the extra post-column dead volume due to reaction coils used to enable adequate reaction time and the mixing of reagents which causes peak broadening, hence a loss of separation power. This loss of efficiency is counter-productive to modern HPLC technologies, -such as UHPLC. We reviewed 87 PCD methods published from 2009 to 2014. We restricted our review to methods published between 2009 and 2014, because we were interested in the uptake of PCD methods in UHPLC environments. Our review focused on a range of system parameters including: column dimensions, stationary phase and particle size, as well as the geometry of the reaction loop. The most commonly used column in the methods investigated was not in fact a modern UHPLC version with sub-2-micron, (or even sub-3-micron) particles, but rather, work-house columns, such as, 250 × 4.6 mm i.d. columns packed with 5 μm C18 particles. Reaction loops were varied, even within the same type of analysis, but the majority of methods employed loop systems with volumes greater than 500 μL. A second part of this review illustrated briefly the effect of dead volume on column performance. The experiment evaluated the change in resolution and separation efficiency of some weak to moderately retained solutes on a 250 × 4.6 mm i.d. column packed with 5 μm particles. The data showed that reaction loops beyond 100 μL resulted in a very serious loss of performance. Our study concluded that practitioners of PCD methods largely avoid the use of UHPLC-type column formats, so yes, very much, PCD is incompatible with the modern HPLC column. PMID:26343427

  8. Optimal design of thermally coupled distillation columns

    SciTech Connect

    Duennebier, G.; Pantelides, C.C.

    1999-01-01

    This paper considers the optimal design of thermally coupled distillation columns and dividing wall columns using detailed column models and mathematical optimization. The column model used is capable of describing both conventional and thermally coupled columns, which allows comparisons of different structural alternatives to be made. Possible savings in both operating and capital costs of up to 30% are illustrated using two case studies.

  9. Simultaneous determination of four furostanol glycosides in rat plasma by UPLC-MS/MS and its application to PK study after oral administration of Dioscorea nipponica extracts.

    PubMed

    Liao, Min; Dai, Cong; Liu, Mengping; Chen, Jiefeng; Chen, Zuanguang; Xie, Zhiyong; Yao, Meicun

    2016-01-01

    A novel, sensitive and rapid ultra-performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method for simultaneous quantification of four furostanol glycosides in rat plasma was established and validated. Ginsenoside Rb1 was used as an internal standard. Plasma samples were pretreated by liquid-liquid extraction with n-butanol and chromatographed on a C18 column (2.1×50 mm i.d., 2.6 μm) using a gradient elution program consisting of acetonitrile and water (containing 0.03% formic acid and 0.1 mM lithium acetate) at a flow rate of 0.4 mL/min. Lithium adduct ions were employed to enhance the response of the analytes in electrospray positive ionization mode and multiple reaction monitoring transitions were performed for detection. All calibration curves exhibited good linearity (r>0.999) over the range of 10-20,000 ng/mL for protodioscin and 2-4000 ng/mL for protogracillin, pseudoprotodioscin and pseudoprotogracillin. The recoveries of the whole analytes were more than 80.3% and exhibited no severe matrix effect. Meanwhile, the intra- and inter-day precisions were all less than 10.7% and accuracies were within the range of -8.1-12.9%. The four saponins showed rapid excretion and relative high plasma concentrations when the validated method was applied to the PK study of Dioscorea nipponica extracts by intragastric administration at low, medium and high dose to rats. Moreover, the T(1/2) and AUC(0-t) of each compound turned out to behave in a dose-dependent pattern by comparing them at different dose levels.

  10. Inhibitive activities detection of monoamine oxidases (MAO) A and B inhibitors in human liver MAO incubations by UPLC-ESI-MS/MS.

    PubMed

    Jiang, Bo; Li, Shuping; Liu, Wei; Yang, Yadi; Chen, Wenxia; He, Dandan; Cheng, Xuemei; Wang, Zhengtao; Chen, Wansheng; Wang, Changhong

    2015-11-10

    A sensitive UPLC-ESI-MS/MS method was developed for determining and screening of inhibitors of monoamine oxidase (MAO) by using mix MAO enzymes prepared from human liver. 5-Hydroxytryptamine (5-HT) and 2-phenethylamine (2-PEA) were used as substrates for MAO-A and MAO-B in incubations, and 5-hydroxyindole-3-acetic acid (5-HIAA) and phenylacetic acid (PAA) resulting from 5-HT and 2-PEA were used as markers to evaluate inhibitive activities of test compounds on MAO-A and MAO-B. Proper separation was achieved for positive multiple reaction monitoring of 5-HIAA (m/z 192.1→146.1) and negative multiple reaction monitoring PAA (m/z 135.0→91.0) via isocratic elution (0.1% fromic acid:acetonitrile=60:40) on a HSS T3 column following a simple precipitation of proteins for sample treatment. The relative standard deviations of intra- and inter-day precisions were ranged from 1.74% to 6.76% and 0.77% to 9.35%. The mean accuracies for the quality control samples were 101.37±6.60% and 101.39±2.85%, respectively. This method exhibited characteristics of small total reaction volume (100μl), short analysis time (3.5min), highly sensitivity, low cost and without matrix effect (103.56±2.33% to 112.63±8.57% for 5-HIAA and 105.68±8.75% to 112.76±4.67% for PAA). The developed method was successfully applied for detection of the MAO-A and MAO-B inhibitive activities by model drugs, including pargyline, clorgyline, as well as β-carboline alkaloids from Peganum harmala.

  11. Development and validation of an UPLC-MS/MS method for the quantification of ethoxzolamide in plasma and bioequivalent buffers: Applications to absorption, brain distribution, and pharmacokinetic studies

    PubMed Central

    Gao, Song; Zhao, Jing; Yin, Taijun; Ma, Yong; Xu, Beibei; Moore, Anthony N.; Dash, Pramod K.; Hu, Ming

    2015-01-01

    The purpose of this study is to develop and validate an UPLC-MS/MS method to quantify ethoxzolamide in plasma (EZ) and apply the method to absorption, brain distribution, as well as pharmacokinetic studies. A C18 column was used with 0.1% of formic acid in acetonitrile and 0.1% of formic acid in water as the mobile phases to resolve EZ. The mass analysis was performed in a triple quadrupole mass spectrometer using multiple reaction monitoring (MRM) with positive scan mode. The results show that the linear range of EZ is 4.88–10,000.00 nM. The intra-day variance is less than 12.43 % and the accuracy is between 88.88–08.00 %. The inter-day variance is less than 12.87 % and accuracy is between 89.27–115.89 %. Protein precipitation was performed using methanol to extract EZ from plasma and brain tissues. Only 40 µL of plasma is needed for analysis due to the high sensitivity of this method, which could be completed in less than three minutes. This method was used to study the pharmacokinetics of EZ in SD rats, and the transport of EZ in Caco-2 and MDCK-MDR1 overexpressing cell culture models. Our data show that EZ is not a substrate for p-glycoprotein (P-gp) and its entry into the brain may not limited by the blood-brain barrier. PMID:25706567

  12. A selective and sensitive method based on UPLC-MS/MS for quantification of momordin Ic in rat plasma: application to a pharmacokinetic study.

    PubMed

    Yan, Huiyu; Song, Yanqing; Zhou, Wei; Zhang, Sixi

    2015-11-10

    A selective and sensitive method was developed and validated based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). This method was applied to quantify momordin Ic in rat plasma. Chromatographic separation was performed on a Hypersil GOLD HPLC C18 column (150mm×4.6mm, 5μm) using an isocratic mobile phase of acetonitrile/water (80:20, v/v) at a flow rate of 0.6mL/min. An electrospray ionization source was applied and operated in negative ion mode; selected reaction monitoring (SRM) mode was used for quantification by monitoring the precursor-to-product ion transitions of m/z 763.4→m/z 455.3 for momordin Ic, and m/z 649.4→m/z 487.3 for IS. Calibration curves showed good linearity over the range of 22.0-2200ng/mL for momordin Ic in rat plasma. The developed method was applied to a pharmacokinetic study of momordin Ic in rats after single intravenous doses at 0.52, 1.56, and 4.67mg/kg. The elimination half-life (t1/2) values were 1.22±0.39, 1.14±0.10, and 1.83±0.39h, respectively. The plasma concentration at 2min (C2min) and area under the curve (AUC) for the intravenous doses of momordin Ic were approximately dose proportional. PMID:26218506

  13. Self-regenerating column chromatography

    DOEpatents

    Park, Woo K.

    1995-05-30

    The present invention provides a process for treating both cations and anions by using a self-regenerating, multi-ionic exchange resin column system which requires no separate regeneration steps. The process involves alternating ion-exchange chromatography for cations and anions in a multi-ionic exchange column packed with a mixture of cation and anion exchange resins. The multi-ionic mixed-charge resin column works as a multi-function column, capable of independently processing either cationic or anionic exchange, or simultaneously processing both cationic and anionic exchanges. The major advantage offered by the alternating multi-function ion exchange process is the self-regeneration of the resins.

  14. LIQUID-LIQUID EXTRACTION COLUMNS

    DOEpatents

    Thornton, J.D.

    1957-12-31

    This patent relates to liquid-liquid extraction columns having a means for pulsing the liquid in the column to give it an oscillatory up and down movement, and consists of a packed column, an inlet pipe for the dispersed liquid phase and an outlet pipe for the continuous liquid phase located in the direct communication with the liquid in the lower part of said column, an inlet pipe for the continuous liquid phase and an outlet pipe for the dispersed liquid phase located in direct communication with the liquid in the upper part of said column, a tube having one end communicating with liquid in the lower part of said column and having its upper end located above the level of said outlet pipe for the dispersed phase, and a piston and cylinder connected to the upper end of said tube for applying a pulsating pneumatic pressure to the surface of the liquid in said tube so that said surface rises and falls in said tube.

  15. Determination of Curcuminoids in Curcuma longa Linn. by UPLC/Q-TOF-MS: An Application in Turmeric Cultivation.

    PubMed

    Ashraf, Kamran; Mujeeb, Mohd; Ahmad, Altaf; Ahmad, Niyaz; Amir, Mohd

    2015-09-01

    Cucuma longa Linn. (Fam-Zingiberaceae) is a valued medicinal plant contains curcuminoids (curcumin, demethoxycurcumin and bisdemethoxycurcumin) as major bioactive constituents. Previously reported analytical methods for analysis of curcuminoids were found to suffer from low resolution, lower sensitivity and longer analytical times. In this study, a rapid, sensitive, selective high-throughput ultra high performance liquid chromatography-tandem mass spectrometry (UPLC/Q-TOF-MS) method was developed and validated for the quantification of curcuminoids with an aim to reduce analysis time and enhance efficiency. UPLC/Q-TOF-MS analysis showed large variation (1.408-5.027% w/w) of curcuminoids among different samples with respect to their occurrence of metabolite and their concentration. The results showed that Erode (south province) contains highest quantity of curcuminoids and concluded to be the superior varieties. The results obtained here could be valuable for devising strategies for cultivating this medicinal plant. PMID:25838167

  16. Glycosylation characterization of Human IgA1 with differential deglycosylation by UPLC-ESI TOF MS.

    PubMed

    Klapoetke, Song C; Zhang, Jian; Becht, Steven

    2011-11-01

    Differential deglycosylation was introduced as an effective technique to characterize glycosylation in glycoprotein containing both N-linked and O-linked glycans at both protein and peptide levels. Human IgA1 was used as a model glycoprotein to demonstrate this technique. The glycans attached to Human IgA1 were removed from their attachment sites by an array of enzymes. After reduction by DTT, the resulting deglycoproteins were analyzed by UPLC-ESI TOF MS to estimate the numbers of N-glycan and O-glycan sites through differential masses. The deglycoproteins and unmodified glycoprotein were further digested to deglycopeptide through trypsin digestion. The glycopeptides and deglycopeptides were identified by UPLC-ESI TOF MS. Two N-glycan and four O-glycan sites were identified and confirmed at peptide levels. These results matched those from deglycoproteins. The N-glycosylation site and N-glycan sequence confirmation were also demonstrated in this study.

  17. Simultaneous determination of mequindox, quinocetone, and their major metabolites in chicken and pork by UPLC-MS/MS.

    PubMed

    Li, Yanshen; Liu, Kaili; Beier, Ross C; Cao, Xingyuan; Shen, Jianzhong; Zhang, Suxia

    2014-10-01

    This report presents a UPLC-MS/MS method for determination of mequindox (MEQ), quinocetone (QCT) and their 11 metabolites in chicken and pork samples. Following extraction process with acetonitrile-ethyl acetate, acidulation, and re-extraction with ethyl acetate in turn, target analytes were further purified using C18 solid phase extraction (SPE) cartridges for UPLC-MS/MS analysis. Validation was processed with mean recoveries from 69.1% to 113.3% with intra-day relative standard deviation (RSD) <14.7%, inter-day RSD <19.2%, and limit of detection between 0.05 and 1.0 μg/kg for each analytes. The verified method was successfully applied to the quantitative determination of commercial samples. This developed procedure will help to control food animal products with MEQ and QCT residues, and facilitate further pharmacokinetic and residue studies of similar quinoxaline-1,4-dioxide veterinary drugs. PMID:24799224

  18. Determination of Curcuminoids in Curcuma longa Linn. by UPLC/Q-TOF-MS: An Application in Turmeric Cultivation.

    PubMed

    Ashraf, Kamran; Mujeeb, Mohd; Ahmad, Altaf; Ahmad, Niyaz; Amir, Mohd

    2015-09-01

    Cucuma longa Linn. (Fam-Zingiberaceae) is a valued medicinal plant contains curcuminoids (curcumin, demethoxycurcumin and bisdemethoxycurcumin) as major bioactive constituents. Previously reported analytical methods for analysis of curcuminoids were found to suffer from low resolution, lower sensitivity and longer analytical times. In this study, a rapid, sensitive, selective high-throughput ultra high performance liquid chromatography-tandem mass spectrometry (UPLC/Q-TOF-MS) method was developed and validated for the quantification of curcuminoids with an aim to reduce analysis time and enhance efficiency. UPLC/Q-TOF-MS analysis showed large variation (1.408-5.027% w/w) of curcuminoids among different samples with respect to their occurrence of metabolite and their concentration. The results showed that Erode (south province) contains highest quantity of curcuminoids and concluded to be the superior varieties. The results obtained here could be valuable for devising strategies for cultivating this medicinal plant.

  19. Quantification of patulin in fruit leathers by ultra-high-performance liquid chromatography-photodiode array (UPLC-PDA).

    PubMed

    Maragos, Chris M; Busman, Mark; Ma, Liang; Bobell, John

    2015-01-01

    Patulin is a mycotoxin commonly found in certain fruit and fruit products. For this reason many countries have established regulatory limits pertaining to, in particular, apple juice and apple products. Fruit leathers are produced by dehydrating fruit puree, leaving a sweet product that has a leathery texture. A recent report in the literature described the detection of patulin at substantial levels in fruit leathers. To investigate this further, an ultra-high-performance liquid chromatography-photodiode array (UPLC-PDA) method was developed for the sensitive detection of patulin in fruit leathers. Investigations were also made of the suitability of direct analysis in real time-mass spectrometry (DART-MS) for detection of patulin from the surface of fruit leathers. Results indicated DART-MS was insufficiently sensitive for quantification from the surface of home-style apple leathers, although patulin spiked onto the surface of leather or peel could be detected. The UPLC-PDA method was used to determine the fate of patulin during the preparation of home-made fruit leathers. Interestingly, when a home-style process was used, the patulin was not destroyed, but rather increased in concentration as the puree was dehydrated. The UPLC-PDA method was also used to screen for patulin in commercial fruit leathers. Of the 36 products tested, 14 were above the limit of detection (3.5 μg kg(-1)) and nine were above the limit of quantification (12 μg kg(-1)). Positive samples were confirmed by UPLC-MS/MS. Only one sample was found above the US regulatory limit for single-strength apple juice products (50 μg kg(-1)). These results suggest patulin can be concentrated during preparation and can be found in fruit leathers. The limited survey suggests that patulin is fairly prevalent in such commercial products, but that the levels are usually low.

  20. Large Scale Non-targeted Metabolomic Profiling of Serum by Ultra Performance Liquid Chromatography-Mass Spectrometry (UPLC-MS)

    PubMed Central

    Broeckling, Corey D.; Heuberger, Adam L.; Prenni, Jessica E.

    2013-01-01

    Non-targeted metabolite profiling by ultra performance liquid chromatography coupled with mass spectrometry (UPLC-MS) is a powerful technique to investigate metabolism. The approach offers an unbiased and in-depth analysis that can enable the development of diagnostic tests, novel therapies, and further our understanding of disease processes. The inherent chemical diversity of the metabolome creates significant analytical challenges and there is no single experimental approach that can detect all metabolites. Additionally, the biological variation in individual metabolism and the dependence of metabolism on environmental factors necessitates large sample numbers to achieve the appropriate statistical power required for meaningful biological interpretation. To address these challenges, this tutorial outlines an analytical workflow for large scale non-targeted metabolite profiling of serum by UPLC-MS. The procedure includes guidelines for sample organization and preparation, data acquisition, quality control, and metabolite identification and will enable reliable acquisition of data for large experiments and provide a starting point for laboratories new to non-targeted metabolite profiling by UPLC-MS. PMID:23524330

  1. Metabolomic approach for discrimination of processed ginseng genus (Panax ginseng and Panax quinquefolius) using UPLC-QTOF MS.

    PubMed

    Park, Hee-Won; In, Gyo; Kim, Jeong-Han; Cho, Byung-Goo; Han, Gyeong-Ho; Chang, Il-Moo

    2014-01-01

    Discriminating between two herbal medicines (Panax ginseng and Panax quinquefolius), with similar chemical and physical properties but different therapeutic effects, is a very serious and difficult problem. Differentiation between two processed ginseng genera is even more difficult because the characteristics of their appearance are very similar. An ultraperformance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF MS)-based metabolomic technique was applied for the metabolite profiling of 40 processed P. ginseng and processed P. quinquefolius. Currently known biomarkers such as ginsenoside Rf and F11 have been used for the analysis using the UPLC-photodiode array detector. However, this method was not able to fully discriminate between the two processed ginseng genera. Thus, an optimized UPLC-QTOF-based metabolic profiling method was adapted for the analysis and evaluation of two processed ginseng genera. As a result, all known biomarkers were identified by the proposed metabolomics, and additional potential biomarkers were extracted from the huge amounts of global analysis data. Therefore, it is expected that such metabolomics techniques would be widely applied to the ginseng research field.

  2. Metabonomics evaluation of urine from rats given acute and chronic doses of acetaminophen using NMR and UPLC/MS.

    PubMed

    Sun, Jinchun; Schnackenberg, Laura K; Holland, Ricky D; Schmitt, Thomas C; Cantor, Glenn H; Dragan, Yvonne P; Beger, Richard D

    2008-08-15

    Urinary metabolic perturbations associated with acute and chronic acetaminophen-induced hepatotoxicity were investigated using nuclear magnetic resonance (NMR) spectroscopy and ultra performance liquid chromatography/mass spectrometry (UPLC/MS) metabonomics approaches to determine biomarkers of hepatotoxicity. Acute and chronic doses of acetaminophen (APAP) were administered to male Sprague-Dawley rats. NMR and UPLC/MS were able to detect both drug metabolites and endogenous metabolites simultaneously. The principal component analysis (PCA) of NMR or UPLC/MS spectra showed that metabolic changes observed in both acute and chronic dosing of acetaminophen were similar. Histopathology and clinical chemistry studies were performed and correlated well with the PCA analysis and magnitude of metabolite changes. Depletion of antioxidants (e.g. ferulic acid), trigonelline, S-adenosyl-L-methionine, and energy-related metabolites indicated that oxidative stress was caused by acute and chronic acetaminophen administration. Similar patterns of metabolic changes in response to acute or chronic dosing suggest similar detoxification and recovery mechanisms following APAP administration.

  3. UPLC-QTOFMS(E)-Guided Dereplication of the Endangered Chinese Species Garcinia paucinervis to Identify Additional Benzophenone Derivatives.

    PubMed

    Li, Ping; Anandhi Senthilkumar, Harini; Figueroa, Mario; Wu, Shi-Biao; Fata, Jimmie E; Kennelly, Edward J; Long, Chunlin

    2016-06-24

    A number of Garcinia species accumulate benzophenone derivatives that may be useful for the treatment of breast cancer. The dereplication of new benzophenone derivatives from Garcinia species is challenging due to the occurrence of multiple isomers and the known compounds found in their extracts. In the current study, a strategy is described using the UPLC-QTOFMS(E) technique to identify tentatively the known and uncharacterized benzophenones of interest based upon the characteristic fragmentation ions. Several UPLC-QTOFMS peaks (a-ee) appeared to contain benzophenone derivatives, and 12 of these peaks contained compounds with MS ionization profiles not consistent with previously identified compounds from the seeds of Garcinia paucinervis, an endangered Chinese species. The targeted isolation of unidentified compounds of interest afforded five new benzophenones, paucinones E-I (1-5), which were determined by MS and NMR analysis and ECD spectroscopy. These compounds were evaluated for cytotoxicity against three breast cancer cell lines inclusive of MDA-MB-231, SKBR3, and MCF-7. These results indicate that the UPLC-QTOFMS(E)-guided isolation procedure is an efficient strategy for isolating new benzophenones from Garcinia species. PMID:27266714

  4. UPLC-QTOFMS(E)-Guided Dereplication of the Endangered Chinese Species Garcinia paucinervis to Identify Additional Benzophenone Derivatives.

    PubMed

    Li, Ping; Anandhi Senthilkumar, Harini; Figueroa, Mario; Wu, Shi-Biao; Fata, Jimmie E; Kennelly, Edward J; Long, Chunlin

    2016-06-24

    A number of Garcinia species accumulate benzophenone derivatives that may be useful for the treatment of breast cancer. The dereplication of new benzophenone derivatives from Garcinia species is challenging due to the occurrence of multiple isomers and the known compounds found in their extracts. In the current study, a strategy is described using the UPLC-QTOFMS(E) technique to identify tentatively the known and uncharacterized benzophenones of interest based upon the characteristic fragmentation ions. Several UPLC-QTOFMS peaks (a-ee) appeared to contain benzophenone derivatives, and 12 of these peaks contained compounds with MS ionization profiles not consistent with previously identified compounds from the seeds of Garcinia paucinervis, an endangered Chinese species. The targeted isolation of unidentified compounds of interest afforded five new benzophenones, paucinones E-I (1-5), which were determined by MS and NMR analysis and ECD spectroscopy. These compounds were evaluated for cytotoxicity against three breast cancer cell lines inclusive of MDA-MB-231, SKBR3, and MCF-7. These results indicate that the UPLC-QTOFMS(E)-guided isolation procedure is an efficient strategy for isolating new benzophenones from Garcinia species.

  5. Validation of a method for the determination of chloramphenicol in poultry and swine liver by ultra-performance liquid chromatography coupled with tandem mass spectrometry.

    PubMed

    Xia, Xi; Li, Xiaowei; Ding, Shuangyang; Shen, Jianzhong

    2010-01-01

    A sensitive and reliable method has been developed and validated for the determination of chloramphenicol in poultry and swine liver using SPE and ultra-performance liquid chromatography (UPLC)/MS/MS. The liver samples were extracted with ethyl acetate, defatted with n-hexane, and further cleaned up using SPE cartridges with polymeric sorbent. An Acquity BEH C18 column was used for gradient UPLC separation, with water and acetonitrile as the mobile phase. The multiple reaction monitoring mode was used for two precursor-product ion transitions for chloramphenicol and one for the internal standard. The method was validated at 0.1, 0.3, and 1.0 microg/kg. Mean recoveries from fortified samples ranged from 95.5 to 106.7% with an RSD of 12.2%. The method LOD was < 0.02 microg/kg. PMID:21140679

  6. [Simultaneous determination of artificial sweeteners in beverage by ultra performance liquid chromatography].

    PubMed

    Ji, Chao; Sun, Yanyan; Li, Xiuqin; Chu, Xiaogang; Chen, Zhengxing

    2009-01-01

    An ultra performance liquid chromatographic (UPLC) method for the simultaneous separation and determination of four artificial sweeteners (sodium saccharin, aspartame, acesulfame and neotame) in a single injection was developed. The separation was performed on an ACQUITY UPLC BEH C18 column with gradient program and detection at 220 nm. The good linearities between the concentrations of all analytes and peak area responses were achieved over the range from 0.5 to 20.0 mg/L. The average recoveries in samples were 80.5% - 95.2% with the relative standard deviations of 0.50% - 8.7%. The method has been successfully applied to the determination of the four sweeteners in drinks and powdered tabletop sweeteners.

  7. Quantification of flavonol glycosides in Camellia sinensis by MRM mode of UPLC-QQQ-MS/MS.

    PubMed

    Wu, Yahui; Jiang, Xiaolan; Zhang, Shuxiang; Dai, Xinlong; Liu, Yajun; Tan, Huarong; Gao, Liping; Xia, Tao

    2016-04-01

    Phenolic compounds are major components of tea flavour, in which catechins and flavonol glycosides play important roles in the astringent taste of tea infusion. However, the flavonol glycosides are difficult to quantify because of the large variety, as well as the inefficient seperation on chromatography. In this paper, a total of 15 flavonol glycosides in the tea plant (Camellia sinensis) were identified by the high performance liquid chromatography (HPLC) coupled to a time-of-flight mass spectrometer (TOF-MS), and a quantitative method was established based on multiple reaction monitoring (MRM) mode of ultra-high performance liquid chromatography (UPLC) coupled to a triple quadrupole mass spectrometer (QQQ-MS/MS). It provided the limit of detection and quantification to the order of picogram, which was more sensitive than the HPLC detection of the order of nanogram. The relative standard deviations of the intra- and inter-day variations in retention time and signal intensity (peak area) of six analytes were less than 0.26% and 4%, respectively. The flavonol glycosides of four tea cultivars were relatively quantified using the signal intensity (peak area) of product ion, in which six flavonol glycosides were quantified by the authentic standards. The results showed that the flavonol mono-, di- and tri-glycoside mostly accumulated in young leaves of the four tea cultivars. Notably, the myricetin 3-O-galactoside was the major component among the six flavonol glycosides detected.

  8. Chemical Profiling Using Uplc Q-Tof/Ms and Antioxidant Activities of Fortunella Fruits.

    PubMed

    Tan, Si; Zhao, Xijuan; Yang, Ying; Ke, Zunli; Zhou, Zhiqin

    2016-07-01

    The fruits of Fortunella Swingle are widely consumed as fresh fruits and traditional medicine in China. China is the origin center and has the largest cultivated area of the genus Fortunella. In this study, the chemical compositions of ethanol extracts of the major Fortunella cultivated types including Fortunella japonica Swingle, Fortunella margarita Swingle, Fortunella crassifolia Swingle 1 (Lanshang) and Fortunella crassifolia Swingle 2 (Liuyang) were determined using ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC Q-TOF/MS) method, and their antioxidant activities were evaluated. 12 compounds were identified and 5 compounds were tentatively characterized. The results showed that the chemical compositions of the ethanol extracts of 4 Fortunella cultivated types were largely the same. 3', 5'-di-C-glucopyranosylphloretin was the predominant flavonoid in Fortunella fruits, and Fortunella margarita Swingle had higher contents of flavonoids than other species. In addition, the data demonstrated high antioxidant activities of Fortunella fruits. The developed method could be available to rapidly analyze the chemical compounds in Fortunella fruits and its products. This study will provide information for further quality assessment and utilization of Fortunella resources. PMID:27243926

  9. UPLC-ESI-TOF MS-Based Metabolite Profiling of the Antioxidative Food Supplement Garcinia buchananii.

    PubMed

    Stark, Timo D; Lösch, Sofie; Wakamatsu, Junichiro; Balemba, Onesmo B; Frank, Oliver; Hofmann, Thomas

    2015-08-19

    Comparative antioxidative analyses of aqueous ethanolic extracts from leaf, root, and stem of Garcinia buchananii revealed high activity of all three organs. To investigate the metabolite composition of the different parts of G. buchananii, an untargeted metabolomics approach using UPLC-ESI-TOF MS with simultaneous acquisition of low- and high-collision energy mass spectra (MS(e)) was performed. Unsupervised statistics (PCA) highlighted clear differences in the metabolomes of the three organs. OPLS-DA revealed (2R,3S,2″R,3″R)-GB-1, (2R,3S)-morelloflavone, and (2R,3S)-volkensiflavone as the most decisive marker compounds discriminating leaf from root and stem extract. Leaves represent the best source to isolate GB-1, morelloflavone, and volkensiflavone. Root extract is the best organ to isolate xanthones and stem bark extract the best source to isolate (2R,3S,2″R,3″R)-manniflavanone; the identified polyisoprenylated benzophenones are characteristic compounds for the leaf organ. Morelloflavone, volkensiflavone, and garcicowin C were isolated for the first time from G. buchananii, identified via MS, NMR, and CD spectroscopy, and showed in H2O2 scavenging, H/L-TEAC, and H/L-ORAC assays moderate to strong in vitro antioxidative activities. PMID:26226176

  10. UPLC-TOF-MS Characterization and Identification of Bioactive Iridoids in Cornus mas Fruit

    PubMed Central

    West, Brett J.; Jensen, C. Jarakae

    2013-01-01

    Cornus mas L. is indigenous to Europe and parts of Asia. Although Cornus is widely considered to be an iridoid rich genera, only two iridoids have been previously found in this plant. The lack of information on taxonomically and biologically active iridoids prompted us to develop and optimize an analytical method for characterization of additional phytochemicals in C. mas fruit. An ultra performance liquid chromatography (UPLC) coupled with photodiode array spectrophotometry (PDA) and electrospray time-of-flight mass spectrometry (ESI-TOF-MS) was employed and mass parameters were optimized. Identification was made by elucidating the mass spectral data and further confirmed by comparing retention times and UV spectra of target peaks with those of reference compounds. Primary DNA damage and antigenotoxicity tests in E. coli PQ37 were used to screen the iridoids for biological activity. As a result, ten phytochemicals were identified, including iridoids loganic acid, loganin, sweroside, and cornuside. Nine of these were reported for the first time from C. mas fruit. The iridoids did not induce SOS repair of DNA, indicating a lack of genotoxic activity in E. coli PQ37. However, loganin, sweroside, and cornuside did reduce the amount of DNA damage caused by 4-nitroquinoline 1-oxide, suggesting potential antigenotoxic activity. PMID:24228188

  11. UPLC-ESI-TOF MS-Based Metabolite Profiling of the Antioxidative Food Supplement Garcinia buchananii.

    PubMed

    Stark, Timo D; Lösch, Sofie; Wakamatsu, Junichiro; Balemba, Onesmo B; Frank, Oliver; Hofmann, Thomas

    2015-08-19

    Comparative antioxidative analyses of aqueous ethanolic extracts from leaf, root, and stem of Garcinia buchananii revealed high activity of all three organs. To investigate the metabolite composition of the different parts of G. buchananii, an untargeted metabolomics approach using UPLC-ESI-TOF MS with simultaneous acquisition of low- and high-collision energy mass spectra (MS(e)) was performed. Unsupervised statistics (PCA) highlighted clear differences in the metabolomes of the three organs. OPLS-DA revealed (2R,3S,2″R,3″R)-GB-1, (2R,3S)-morelloflavone, and (2R,3S)-volkensiflavone as the most decisive marker compounds discriminating leaf from root and stem extract. Leaves represent the best source to isolate GB-1, morelloflavone, and volkensiflavone. Root extract is the best organ to isolate xanthones and stem bark extract the best source to isolate (2R,3S,2″R,3″R)-manniflavanone; the identified polyisoprenylated benzophenones are characteristic compounds for the leaf organ. Morelloflavone, volkensiflavone, and garcicowin C were isolated for the first time from G. buchananii, identified via MS, NMR, and CD spectroscopy, and showed in H2O2 scavenging, H/L-TEAC, and H/L-ORAC assays moderate to strong in vitro antioxidative activities.

  12. Alkaloids in Erythrina by UPLC-ESI-MS and In Vivo Hypotensive Potential of Extractive Preparations

    PubMed Central

    Merlugo, Liara; Santos, Marí C.; Sant'Anna, Liane S.; Cordeiro, Everson W. F.; Batista, Luiz A. C.; Miotto, Silvia T. S.; Garcia, Cássia V.; Moreira, Cleci M.; Mendez, Andreas S. L.

    2015-01-01

    Erythrina species are used in popular medicine as sedative, anxiolytic, anti-inflammatory, and antihypertensive. In this work, we investigated the chemical composition of extracts obtained from leaves of E. falcata and E. crista-galli. The hypotensive potential of E. falcata and the mechanism of action were also studied. The extracts were obtained by maceration and infusion. The total content of phenolic compounds and flavonoids was estimated by spectrophotometric methods. The chemical constituents were studied performing a chromatographic analysis by UPLC-ESI-MS. For in vivo protocols, blood pressure and heart rate were measured by the invasive hemodynamic monitoring method. Different concentrations of extracts and drugs such as L-NAME, losartan, hexamethonium, and propranolol were administrated i.v. The results of total phenolic contents for E. falcata and E. crista-galli were 1.3193–1.4989 mgGAE/mL for maceration and 0.8771–0.9506 mgGAE/mL for infusion. In total flavonoids, the content was 7.7829–8.1976 mg RE/g for maceration and 9.3471–10.4765 RE mg/g for infusion. The chemical composition was based on alkaloids, suggesting the presence of erythristemine, 11β-methoxyglucoerysodine, erysothiopine, 11β-hydroxyerysodine-glucose, and 11-hydroxyerysotinone-rhamnoside. A potent dose-dependent hypotensive effect was observed for E. falcata, which may be related to the route of β-adrenergic receptors. PMID:26356581

  13. Comparative analysis of diosgenin in Dioscorea species and related medicinal plants by UPLC-DAD-MS

    PubMed Central

    2014-01-01

    Background Dioscorea is a genus of flowering plants, and some Dioscorea species are known and used as a source for the steroidal sapogenin diosgenin. To screen potential resource from Dioscorea species and related medicinal plants for diosgenin extraction, a rapid method to compare the contents of diosgenin in various plants is crucial. Results An ultra-performance liquid chromatography (UPLC) coupled with diode array detection (DAD) and electrospray ionization mass spectrometry (ESI-MS) method was developed for identification and determination of diosgenin in various plants. A comprehensive validation of the developed method was conducted. Twenty-four batches of plant samples from four Dioscorea species, one Smilax species and two Heterosmilax species were analyzed by using the developed method. The present method presented good sensitivity, precision and accuracy. Diosgenin was found in three Dioscorea species and one Heterosmilax species, namely D. zingiberensis, D. septemloba, D. collettii and H. yunnanensis. Conclusion The method is suitable for the screening of diosgenin resources from plants. D. zingiberensis is an important resource for diosgenin harvesting. PMID:25107333

  14. FRACTIONATING COLUMN PRODUCT COLLECTOR CONTROL

    DOEpatents

    Paxson, G.D. Jr.

    1964-03-10

    Means for detecting minute fluid products from a chemical separation column and for advancing a collector tube rack in order to automatically separate and collect successive fractionated products are described. A charge is imposed on the forming drops at the column orifice to create an electric field as the drop falls in the vicinity of a sensing plate. The field is detected by an electrometer tube coupled to the plate causing an output signal to actuate rotation of a collector turntable rack, thereby positioning new collectors under the orifice. The invention provides reliable automatic collection independent of drop size, rate of fall, or chemical composition. (AEC)

  15. A UPLC-MS/MS method for simultaneous determination of danshensu, protocatechuic aldehyde, rosmarinic acid, and ligustrazine in rat plasma, and its application to pharmacokinetic studies of Shenxiong glucose injection in rats.

    PubMed

    Zheng, Lin; Gong, Zipeng; Lu, Yuan; Xie, Yumin; Huang, Yong; Liu, Yue; Lan, Yanyu; Wang, Aimin; Wang, Yonglin

    2015-08-01

    A rapid and sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of the four major active ingredients, danshensu, protocatechuic aldehyde, rosmarinic acid, and ligustrazine, in the traditional Chinese medicine Shenxiong glucose injection in rat plasma. Acidified and alkalized plasma samples were extracted using ethyl acetate, and separated on a Waters C18 column (2.1mm×50mm, 1.7μm) by using a gradient mobile phase system of acetonitrile-water containing 0.1% formic acid and luteoloside as an internal standard. Electrospray ionization in the positive-ion mode and multiple reaction monitoring were used to identify and quantitate the active components. All calibration curves showed good linearity (r>0.994) over the concentration range, with a lower limit of quantification (LLOQ) between 0.02 and 0.21μg/mL. The precision of the in vivo study was evaluated by intra- and inter-day assays, and the percentage of relative standard deviation was within 15%. Moreover, satisfactory extraction efficiency was obtained (between 83.94 and 117.81%) by liquid-liquid extraction. The validated method was successfully applied in a pharmacokinetic study in rats after intravenous administration of Shenxiong glucose injection. The results showed that the four bioactive ingredients in Shenxiong glucose injection have linear pharmacokinetic properties in rats after intravenous injection within the administered dose range and partially different ones compared to single ingredient.

  16. QuEChERS-based purification method coupled to ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to determine six quaternary ammonium compounds (QACs) in dairy products.

    PubMed

    Xian, Yanping; Dong, Hao; Wu, Yuluan; Guo, Xindong; Hou, Xiangchang; Wang, Bin

    2016-12-01

    QuEChERS-based purification coupled with UPLC-MS/MS method, was developed for six quaternary ammonium compounds (QACs) determination in dairy products. Powder samples were firstly dispersed by water. Protein in liquid milk was precipitated and sample solution was extracted by acetonitrile. QuEChERS-based purification was used to purify the solution. QACs were finally separated by HILIC column and detected in MRM mode of MS/MS under ESI(+). The stable isotope benzyl-2,3,4,5,6-d5-dimethyltetradecylammonium bromide (C14-BAC-d5) was used as an internal standard. This method was validated in terms of linearity, sensitivity, precision, accuracy. Linear relations were favorable for QACs over the selected concentration ranges of 0.2-50μg/L, with correlation coefficients greater than 0.999. The limits of detection (LODs) were in the range of 0.4-14.5μg/kg. Recoveries were between 91.2% and 115% with RSDs of 2.8-7.5% for intra-day precision and 3.7-6.7% for inter-day precision. This validated method was successfully applied to determine the QACs concentrations in dairy products. PMID:27374511

  17. A picture of polar iodinated disinfection byproducts in drinking water by (UPLC/)ESI-tqMS.

    PubMed

    Ding, Guoyu; Zhang, Xiangru

    2009-12-15

    Iodinated disinfection byproducts (DBPs) are generally more toxic than their chlorinated and brominated analogues. Up to date, only a few iodinated DBPs in drinking water have been identified by gas chromatography/mass spectrometry. In this work, a method for fast selective detection of polar iodinated DBPs was developed using an electrospray ionization-triple quadrupole mass spectrometer (ESI-tqMS) by conducting precursor ion scan of iodide at m/z 126.9. With such a method, pictures of polar iodinated DBPs in chlorinated, chloraminated, and chlorine-ammonia treated water samples were achieved. By coupling state-of-the-art ultra performance liquid chromatography (UPLC) to the ESI-tqMS, structures of 17 iodinated DBPs were tentatively proposed. The results fully demonstrate that, with respect to the DBP number/levels among the three disinfection processes, chloramination generally generated the most/highest iodinated DBPs, chlorination generally produced the fewest/lowest iodinated DBPs, and chlorine-ammonia sequential treatment formed iodinated DBPs lying in between; the numbers of iodinated DBPs in chloraminated Suwannee River Fulvic Acid (SRFA) and Humic Acid (SRHA) were nearly the same, but the levels of aliphatic iodinated DBPs were higher in the chloraminated SRFA while the levels of aromatic iodinated DBPs were higher in the chloraminated SRHA; a couple of nitrogenous iodinated DBPs were found in chloramination and chlorine-ammonia treatment. The ratio of total organic iodine levels in chlorine-ammonia sequential treatment and chloramination could be expressed as a function of the lag time of ammonia addition.

  18. Identification of in vitro and in vivo metabolites of alantolactone by UPLC-TOF-MS/MS.

    PubMed

    Yao, Donggui; Li, Zhe; Huo, Changhong; Wang, Yufang; Wu, Yibing; Zhang, Manli; Li, Ligeng; Shi, Qingwen; Kiyota, Hiromasa; Shi, Xiaowei

    2016-10-15

    Alantolactone (AL), an active sesquiterpene originating from Inula helenium, is a potential anticancer and anti-inflammatory agent. However so far, studies on AL metabolism have not been reported. In the present study, we have investigated for the first time the in vivo and in vitro metabolites of AL using ultra performance liquid chromatography combined with time of flight mass spectrometry (UPLC-TOF-MS/MS). A unique on-line information-dependent acquisition (IDA) method multiple mass defect filter (MMDF) combined with dynamic background subtraction (DBS) was applied to trace all of the probable metabolites of AL. Five MMDF templates were set according to the core structure of AL and the general metabolite biotransformation patterns, and other five sulfur-containing dimer filter templates were first established on the basis of structural elucidation of AL metabolites obtained from rat intestinal bacteria biotransformation. As a result, 44 metabolites were characterized: 41 metabolites from rat urine, bile and feces after oral administration of AL, and 13 metabolites from AL biotransformation by rat intestinal bacteria. Particularly, 26 metabolites were identified as novel sulfur-containing products. The results indicated that addition of double bond at Δ((11,13)) and oxidization were the main metabolic reactions of AL. A new metabolism pathway to produce addition products of H2S to AL and further generate a series of sulfur-containing dimers of AL was revealed. This study significantly enriched our knowledge about AL metabolism, which will lead to a better understanding of the safety and efficacy of AL. At the same time, the established methodology can be widely applied for the structural determination of the metabolites of other sesquiterpene containing α-methylene-γ-lactone moiety. PMID:27571685

  19. Comprehensive analysis of serum metabolites in gestational diabetes mellitus by UPLC/Q-TOF-MS.

    PubMed

    Liu, Tianhu; Li, Jiaxun; Xu, Fengcheng; Wang, Mengni; Ding, Shijia; Xu, Hongbing; Dong, Fang

    2016-02-01

    Gestational diabetes mellitus (GDM) refers to the first sign or onset of diabetes mellitus during pregnancy rather than progestation. In recent decades, more and more research has focused on the etiology and pathogenesis of GDM in order to further understand GDM progress and recovery. Using an advanced metabolomics platform based on ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF-MS), we explored the changes in serum metabolites between women with GDM and healthy controls during and after pregnancy. Some significant differences were discovered using multivariate analysis including partial least-squares discriminant analysis (PLS-DA) and orthogonal PLS-DA (OPLS-DA). The dysregulated metabolites were further compared and verified in several databases to understand how these compounds might function as potential biomarkers. Analyses of the metabolic pathways associated with these potential biomarkers were subsequently explored. A total of 35 metabolites were identified, contributing to GDM progress to some extent. The identified biomarkers were involved in some important metabolic pathways including glycine, serine, and threonine metabolism; steroid hormone biosynthesis; tyrosine metabolism; glycerophospholipid metabolism; and fatty acid metabolism. The above mentioned metabolic pathways mainly participate in three major metabolic cycles in humans, including lipid metabolism, carbohydrate metabolism, and amino acid metabolism. In this pilot study, the valuable comprehensive analysis gave us further insight into the etiology and pathophysiology of GDM, which might benefit the feasibility of a rapid, accurate diagnosis and reasonable treatment as soon as possible but also prevent GDM and its related short- and long-term complications. PMID:26677023

  20. [Metabolites and metabolic pathways of mesaconitine in rat liver microsomal investigated by using UPLC-MS/MS method in vitro].

    PubMed

    Bi, Yun-Feng; Liu, Shu; Zhang, Rui-Xing; Song, Feng-Rui; Liu, Zhi-Qiang

    2013-12-01

    Mesaconitine was incubated with rat liver microsomes in vitro. The metabolites of mesaconitine in rat liver microsomes were identified by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method with high resolution power. A typical reaction mixture of 100 mol L-1 Tris-HCI buffer (pH 7.4) containing 0.5 gL-1 microsomal protein and 50 micro molL-1 mesaconitine was prepared. The above reaction mixture was divided into six groups, and the volume of each group was 200 micro L. The incubation mixture was pre-incubated at 37 degrees C for 2 min and the reactions were initiated by adding NADPH generating system. After 90 min incubation at 37 degrees C, 200 micro L of acetonitrile was added to each group to stop the reaction. The metabolites of mesaconitine were investigated by UPLC-MS/MS method. Mesaconitine and 6 metabolites M1-M6 were found in the incubation system. The structures were characterized according to the data from MS/MS spectra and literatures. The metabolic reactions of mesaconitine in rat liver microsomes included the demethylation, deacetylation, dehydrogenation and hydroxylation. The major metabolic pathways of mesaconitine in rat liver microsomes were determined by UPLC-MS/MS on multiple reaction monitoring (MRM) mode combined with specific inhibitors of cytochrome P450 (CYP) isoforms, including alpha-naphthoflavone (CYP1A2), quinine (CYP2D), diethyldithiocarbamate (CYP2E1), ketoconazole (CYP3A) and sulfaphenazole (CYP2C), separately. Mesaconitine was mainly metabolized by CYP3A. CYP2C and CYP2D were also more important CYP isoforms for the metabolism reactions of mesaconitine, but CYP1A2 and CYP2E1 haven't any contribution to MA metabolism in rat liver microsomes. PMID:24689241

  1. Beam Studies with Electron Columns

    SciTech Connect

    Shiltsev, V.; Valishev, A.; Kuznetsov, G.; Kamerdzhiev, V.; Romanov, A.; /Novosibirsk, IYF

    2009-04-01

    We report preliminary results of experimental studies of 'electron columns' in the Tevatron and in a specialized test setup. In the Tevatron, a beam of 150 GeV protons ionizes residual gas and ionization electrons are stored in an electrostatic trap immersed into strong longitudinal magnetic field. Shifts of proton betatron frequencies are observed. In the test setup, we observe effects pointing to accumulation and escape of ionization electrons.

  2. Quantitation of the Oral Anticoagulants Dabigatran, Rivaroxaban, Apixaban, and Warfarin in Plasma Using Ultra-Performance Liquid Chromatography with Tandem Mass Spectrometry (UPLC-MS/MS).

    PubMed

    Noguez, Jaime H; Ritchie, James C

    2016-01-01

    This chapter describes a method to measure the oral anticoagulants dabigatran, rivaroxaban, apixaban, and warfarin in plasma samples using ultra-performance liquid chromatography combined with tandem mass spectrometry (UPLC-MS/MS). The instrument is operated in multiple reaction monitoring (MRM) mode with an electrospray ionization (ESI) source in positive ionization mode. Samples are extracted with a 90:10 methanol/0.1 N hydrochloric acid solution containing stable isotope-labeled internal standards for each analyte. After centrifugation the supernatant is transferred to a mass spectrometry vial, injected onto the UPLC-ESI-MS/MS, and quantified using an eight-point calibration curve.

  3. Temperature programmable microfabricated gas chromatography column

    DOEpatents

    Manginell, Ronald P.; Frye-Mason, Gregory C.

    2003-12-23

    A temperature programmable microfabricated gas chromatography column enables more efficient chemical separation of chemical analytes in a gas mixture by the integration of a resistive heating element and temperature sensing on the microfabricated column. Additionally, means are provided to thermally isolate the heated column from their surroundings. The small heat capacity and thermal isolation of the microfabricated column improves the thermal time response and power consumption, both important factors for portable microanalytical systems.

  4. Development and validation of an UPLC-MS/MS method for the quantification of irinotecan, SN-38 and SN-38 glucuronide in plasma, urine, feces, liver and kidney: Application to a pharmacokinetic study of irinotecan in rats.

    PubMed

    Basu, Sumit; Zeng, Min; Yin, Taijun; Gao, Song; Hu, Ming

    2016-03-15

    The objective of this research is to develop and validate a sensitive and reproducible UPLC-MS/MS method to quantify irinotecan, its active metabolite SN-38 and SN-38 glucuronide (phase II metabolite of SN-38) simultaneously in different bio-matrices (plasma, urine, feces), tissues (liver and kidney) and to use the method to investigate its pharmacokinetic behavior in rats. Irinotecan, SN-38 and SN-38 glucuronide has been resolved and separated by C18 column using acetonitrile and 0.1% formic acid in water used as the mobile phases. Triple quadruple mass spectrometer using multiple reaction monitoring (MRM) with positive scan mode were employed to perform mass analysis. The results showed that the linear response range of irinotecan and SN-38 in plasma, feces, liver and kidney is 4.88-10000 nM, 39-5000 nM, 48.8-6250 nM and 48.8-6250 nM, respectively (R(2)>0.99). In case of SN-38 glucuronide, the standard curves were linear in the concentration range of 6.25-2000 nM, 4.88-1250 nM, 9.8-1250 nM and 9.8-1250 nM in plasma, feces, liver and kidney homogenates, respectively. The lower limit of detection (LLOD) of irinotecan, SN-38 and SN-38 glucuronide was determined to be less than 25 nM in all bio-matrices as well as tissue homogenates. Recoveries of irinotecan, SN-38 and SN-38 glucuronide at three different concentrations (low, medium and high) were not less than 85% at three different concentrations in plasma and feces. The percentage matrix factors in different bio-matrices and tissues were within 20%. The UPLC-MS/MS method was validated with intra-day and inter-day precision of less than 15% in plasma, feces, liver and kidney. Owing to the high sensitivity of this method, only 20 μl of plasma, urine and homogenates of liver, kidney and feces is needed. The validated method has been successfully employed for pharmacokinetic evaluation of irinotecan in male wistar rats to quantify irinotecan, SN-38 and SN-38 glucuronide in plasma, feces, and urine samples. PMID

  5. Validation of a novel in vitro assay using ultra performance liquid chromatography-mass spectrometry (UPLC/MS) to detect and quantify hydroxylated metabolites of BDE-99 in rat liver microsomes.

    PubMed

    Erratico, Claudio A; Szeitz, András; Bandiera, Stelvio M

    2010-06-01

    The purpose of this study was to develop and validate an ultra performance liquid chromatography-mass spectrometry (UPLC/MS) method to investigate the hepatic oxidative metabolism of 2,2',4,4',5-pentabromodiphenyl ether (BDE-99), a widely used flame retardant and ubiquitous environmental contaminant. Hydroxylated metabolites were extracted using liquid-to-liquid extraction, resolved on a C18 column with gradient elution and detected by mass spectrometry in single ion recording mode using electrospray negative ionization. The assay was validated for linearity, accuracy, precision, limit of quantification, range and recovery. Calibration curves were linear (R2 > or = 0.98) over a concentration range of 0.010-1.0 microM for 4-OH-2,2',3,4',5-pentabromodiphenyl ether (4-OH-BDE-90), 5'-OH-2,2',4,4',5-pentabromodiphenyl ether (5'-OH-BDE-99) and 6'-OH-2,2',4,4',5-pentabromodiphenyl ether (6'-OH-BDE-99), and a concentration range of 0.0625-12.5 microM for 2,4,5-tribromophenol (2,4,5-TBP). Inter- and intra-day accuracy values ranged from -2.0% to 6.0% and from -7.7% to 7.3%, respectively, and inter- and intra-day precision values ranged from 2.0% to 8.5% and from 2.2% to 8.6% (n=6), respectively. The limits of quantification were 0.010 microM for 4-OH-BDE-90, 5'-OH-BDE-99 and 6'-OH-BDE-99, and 0.0625 microM for 2,4,5-TBP. Recovery values ranged between 85 and 100% for the four analytes. The validated analytical method was applied to identify and quantify hydroxy BDE-99 metabolites formed in vitro. Incubation of BDE-99 with rat liver microsomes yielded 4-OH-BDE-90 and 6'-OH-BDE-99 as major metabolites and 5'-OH-BDE-99 and 2,4,5-TBP as minor metabolites. To our knowledge, this is the first validated UPLC/MS method to quantify hydroxylated metabolites of PBDEs without the need of derivatization. PMID:20451473

  6. 29 CFR 1926.755 - Column anchorage.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ...) General requirements for erection stability. (1) All columns shall be anchored by a minimum of 4 anchor rods (anchor bolts). (2) Each column anchor rod (anchor bolt) assembly, including the column-to-base... of anchor rods (anchor bolts). (1) Anchor rods (anchor bolts) shall not be repaired, replaced...

  7. 29 CFR 1926.755 - Column anchorage.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 29 Labor 8 2011-07-01 2011-07-01 false Column anchorage. 1926.755 Section 1926.755 Labor... (CONTINUED) SAFETY AND HEALTH REGULATIONS FOR CONSTRUCTION Steel Erection § 1926.755 Column anchorage. (a) General requirements for erection stability. (1) All columns shall be anchored by a minimum of 4...

  8. Coumarin and furanocoumarin quantitation in citrus peel via ultraperformance liquid chromatography coupled with mass spectrometry (UPLC-MS).

    PubMed

    Dugrand, Audray; Olry, Alexandre; Duval, Thibault; Hehn, Alain; Froelicher, Yann; Bourgaud, Frédéric

    2013-11-13

    Coumarins and furanocoumarins are secondary metabolites commonly found in citrus plants. These molecules are allelochemical compounds in plants that have controversial effects on humans, such as phototoxicity and the commonly described interactions with drugs, referred to as the "grapefruit juice effect". Thus, it is important to develop a reliable method to identify and quantitate the coumarins and furanocoumarins in citrus extracts. For this purpose, we herein describe an ultraperformance liquid chromatography coupled with mass spectrometry (UPLC-MS)-based method. We first developed a rapid UPLC method (20 min) to separate the isomers of each furanocoumarin. A subsequent single ion monitoring MS detection method was performed to distinguish between the molecules, which were possibly coeluting but had different molecular weights. The method was successfully used to separate and quantitate 6 coumarins and 21 furanocoumarins in variable amounts within peel extracts (flavedo and albedo) of 6 varieties of Citrus (sweet orange, lemon, grapefruit, bergamot, pummelo, and clementine). This method combines high selectivity and sensitivity in a rapid analysis and is useful for fingerprinting Citrus species via their coumarin and furanocoumarin contents.

  9. A Pharmaco-Metabonomic Study on Chronic Kidney Disease and Therapeutic Effect of Ergone by UPLC-QTOF/HDMS

    PubMed Central

    Zhao, Ying-Yong; Chen, Hua; Tian, Ting; Chen, Dan-Qian; Bai, Xu; Wei, Feng

    2014-01-01

    Chronic kidney disease (CKD) is an important public health problem. Ergone has been proved to prevent the progression of CKD. UPLC-QTOF/HDMS was employed for metabolic profiling of adenine-induced CKD and to investigate the nephroprotective effects of ergone. Pharmacology parameters including blood biochemistry, histopathological evaluation and Western blot analysis were performed concurrently. The UPLC-MS data were analyzed by partial least squares-discriminate analysis, correlation analysis, heatmap analysis and mapped to KEGG pathways. Blood and serum biochemistry were observed to be significantly different in the CKD group than in the control group. In conjunction with biochemistry, histopathology and protein expression results, identified metabolites indicated perturbations in fatty acid metabolism, purine metabolism and amino acid metabolism as changes associated with adenine-induced CKD and the interventions of ergone. Upregulated expression of TGF-β1, ED-1, CTGF, bFGF and collagen I was observed in the CKD group. However, downregulated expression of these proteins was observed after oral administration of ergone. These results suggest that expression changes in these proteins had implications for fatty acid metabolism, purine metabolism and amino acid metabolism in the development of CKD and that ergone treatment could delay the development of CKD by normalizing or blocking abnormal changes in biomarker metabolites and protein expression in the CKD group. PMID:25535749

  10. Metabolomic fingerprint classification of Brachychiton acerifolius organs via UPLC-qTOF-PDA-MS analysis and chemometrics.

    PubMed

    Farag, Mohamed A; Abou Zeid, Aisha H; Hamed, Manal A; Kandeel, Zeinab; El-Rafie, Hanaa M; El-Akad, Radwa H

    2015-01-01

    Brachychiton acerifolius, or Sterculia acerifolia as formerly known, is a member of a genus reported for a myriad of bioactive compounds. Metabolome analysis of B. acerifolius--leaves, flowers and seeds--and quantification of its major compounds are demonstrated in this study. Metabolites were analysed via UPLC-PDA-qTOF-(±) ESI-MS and UPLC/ITMS, with a total of 56 metabolites characterised including 30 flavonoids, 2 anthocyanins, 6 phenolic acids (i.e. citric and hydroxycitric acid conjugates) and 8 fatty acids (FAs). Multivariate data analyses (i.e. principle component analysis and orthogonal partial least square-discriminate analysis) were applied to identify metabolite markers for each organ. Pelargonidin-O-glucoside and naringenin-O-glucuronide were found exclusively in flowers versus flavone enrichment in leaves (i.e. luteolin-O-glucuronide and apigenin-O-rhamnosyl glucuronide). Gas chromatography/mass spectrometry analysis revealed the presence of toxic cyclopropene FAs in seeds which may restrict its use. Antioxidant activity assessment for the three organs was performed in comparison with vitamin C as positive control. Leaves showed the highest activity (IC50 0.015 mg/mL). PMID:25296242

  11. Secondary metabolite profiling of Curcuma species grown at different locations using GC/TOF and UPLC/Q-TOF MS.

    PubMed

    Lee, Jueun; Jung, Youngae; Shin, Jeoung-Hwa; Kim, Ho Kyoung; Moon, Byeong Cheol; Ryu, Do Hyun; Hwang, Geum-Sook

    2014-07-04

    Curcuma, a genus of rhizomatous herbaceous species, has been used as a spice, traditional medicine, and natural dye. In this study, the metabolite profile of Curcuma extracts was determined using gas chromatography-time of flight mass spectrometry (GC/TOF MS) and ultrahigh-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF MS) to characterize differences between Curcuma aromatica and Curcuma longa grown on the Jeju-do or Jin-do islands, South Korea. Previous studies have performed primary metabolite profiling of Curcuma species grown in different regions using NMR-based metabolomics. This study focused on profiling of secondary metabolites from the hexane extract of Curcuma species. Principal component analysis (PCA) and partial least-squares discriminant analysis (PLS-DA) plots showed significant differences between the C. aromatica and C. longa metabolite profiles, whereas geographical location had little effect. A t-test was performed to identify statistically significant metabolites, such as terpenoids. Additionally, targeted profiling using UPLC/Q-TOF MS showed that the concentration of curcuminoids differed depending on the plant origin. Based on these results, a combination of GC- and LC-MS allowed us to analyze curcuminoids and terpenoids, the typical bioactive compounds of Curcuma, which can be used to discriminate Curcuma samples according to species or geographical origin.

  12. Tissue distribution model and pharmacokinetics of nuciferine based on UPLC-MS/MS and BP-ANN.

    PubMed

    Xu, Yanyan; Bao, Shihui; Tian, Weiqiang; Wen, Congcong; Hu, Lufeng; Lin, Chongliang

    2015-01-01

    Nuciferine has shown remarkable biological activities and been considered as a promising drug. In this study, a sensitive and selective ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for determination of nuciferine in tissue and plasma. An electrospray ionization source was applied and operated in positive ion mode; multiple reactions monitoring (MRM) mode was used for quantification using target fragment ions m/z 296.0→265.1 for nuciferine, and m/z 322.0→307.0 for berberrubine internal standard (IS). Based on the UPLC-MS/MS method, the tissue distribution profile of nuciferine in mice and plasma pharmacokinetics in rat were studied. The results showed nuciferine was absorbed through intestinal tract and distributed into tissues rapidly. The bioavailability of nuciferine was identified at 17.9%. It can across through blood brain barrier, the concentrations in liver and kidney are highest, then followed by spleen, lung heart and brain. Nuciferine is eliminated quickly in the tissues and plasma, the t1/2 within 5 hour. The concentrations in these tissues are correlated to each other, and can be predicted by a back-propagation artificial neural network model. PMID:26770351

  13. Tissue distribution model and pharmacokinetics of nuciferine based on UPLC-MS/MS and BP-ANN

    PubMed Central

    Xu, Yanyan; Bao, Shihui; Tian, Weiqiang; Wen, Congcong; Hu, Lufeng; Lin, Chongliang

    2015-01-01

    Nuciferine has shown remarkable biological activities and been considered as a promising drug. In this study, a sensitive and selective ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for determination of nuciferine in tissue and plasma. An electrospray ionization source was applied and operated in positive ion mode; multiple reactions monitoring (MRM) mode was used for quantification using target fragment ions m/z 296.0→265.1 for nuciferine, and m/z 322.0→307.0 for berberrubine internal standard (IS). Based on the UPLC-MS/MS method, the tissue distribution profile of nuciferine in mice and plasma pharmacokinetics in rat were studied. The results showed nuciferine was absorbed through intestinal tract and distributed into tissues rapidly. The bioavailability of nuciferine was identified at 17.9%. It can across through blood brain barrier, the concentrations in liver and kidney are highest, then followed by spleen, lung heart and brain. Nuciferine is eliminated quickly in the tissues and plasma, the t1/2 within 5 hour. The concentrations in these tissues are correlated to each other, and can be predicted by a back-propagation artificial neural network model. PMID:26770351

  14. Rapid screening and identification of phenolic antioxidants in Hydrocotyle sibthorpioides Lam. by UPLC-ESI-MS/MS.

    PubMed

    Kumari, Sima; Elancheran, R; Kotoky, Jibon; Devi, Rajlakshmi

    2016-07-15

    The aim of the study was to identify the phenolic compounds present in Hydrocotyle sibthorpioides (HS), Centella asiatica (CA) and Amaranthus viridis (AV) extracts and investigate their respective antioxidant activities. Herein, an ultra-high pressure liquid chromatography-mass spectrometer (UPLC-MS/MS) analytical method has been developed for the separation, and systematic characterization of the phenolic compounds in HS, CA and AV extracts and was compared along with ten standard phenolic compounds. Additionally, in vitro antioxidant activity of the phenolic compounds was also determined. The HS extract revealed excellent antioxidant activity such as 1,1-diphenyl-2-picrylhydrazyl radical scavenging activity (IC50=19.7 ± 1.2 μg/mL), total reduction capability (0.169 ± 0.003 at 100 μg/mL), nitric oxide radical scavenging activity (IC50=39.33 ± 3.2 μg/mL), metal chelating activity (IC50=56.51 ± 3.6 μg/mL) and inhibition of lipid peroxidation (IC50=12.34 ± 2.3 μg/mL) as compared to CA and AV extracts. Furthermore, catechin, epicatechin, quercetin and chlorogenic acid were found to be the major components responsible for the antioxidant activity of the HS extract as evidenced from UPLC-MS/MS. Taken together, this study demonstrates the promising antioxidant properties of the HS extract, which can further be utilized in various pharmaceutical, food, and agricultural applications. PMID:26948646

  15. Varietal classification and antioxidant activity prediction of Osmanthus fragrans Lour. flowers using UPLC-PDA/QTOF-MS and multivariable analysis.

    PubMed

    Zhou, Fei; Peng, Jiyu; Zhao, Yajing; Huang, Weisu; Jiang, Yirong; Li, Maiquan; Wu, Xiaodan; Lu, Baiyi

    2017-02-15

    This study was aimed to classify the varieties and predict the antioxidant activity of Osmanthus fragrans flowers by UPLC-PDA/QTOF-MS and multivariable analysis. The PLS-DA model successfully classified the four varieties based on both the 21 identified compounds and the effective compounds. For the antioxidant activity prediction, PLS performed well to predict the antioxidant activity of O. fragrans flowers. Furthermore, acteoside, suspensaside A, ligustroside, forsythoside A, phillygenin and caffeic acid were selected as effective compounds by UVE-SPA for prediction. On the basis of effective compounds, PLS, MLR and PCR were applied to establish the calibration models. The UVE-SPA-MLR model was the optimal method to predict the antioxidant activity values with Rp of 0.9200, 0.9010 and 0.8905 for DPPH, ABTS and FRAP assays, respectively. The results revealed that the UPLC-PDA/QTOF-MS combined with chemometrics could be a new method to classify the varieties and predict the antioxidant activity of O. fragrans flowers. PMID:27664663

  16. Separation and identification of diarylheptanoids in supercritical fluid extract of Alpinia officinarum by UPLC-MS-MS.

    PubMed

    Luo, Jingchao; Rui, Wen; Jiang, Miaomiao; Tian, Qinglong; Ji, Xing; Feng, Yifan

    2010-11-01

    In the present study, ultra-performance liquid chromatography (UPLC) coupled to electrospray ionization (ESI(+)) tandem mass spectrometry (MS) was developed to identify and characterize the diarylheptanoids in the supercritical fluid extract (SFE) of Alpinia officinarum. The method established provides good reproducibility of UPLC and shows high precision with all the mass accuracy of less than 5 ppm. The ESI-MS-MS fragmentation behavior of every group and their appropriate characteristic pathways were proposed. On the basis of analyzing the fragmentation pathways, elemental composition provided by software Masslynx, mass data of the standard compounds and the information regarding polarity obtained from retention time data, in all, 23 diarylheptanods were characterized. All of them have been reported in Alpinia officinarum. They were classified into six distinct groups (homologous series). Compared to the references, the fragmentation pathways of the first and second group were detailed much more and complementary. Further more, the fragmentation pathways of the last four groups were firstly discussed. The fragmentation rules deduced and the data provided could aid in the characterization of other diarylheptanoids of these types and would be useful for the further research of diarylheptanoids in Alpinia officinarum or the other plants.

  17. Optimization and evaluation of metabolite extraction protocols for untargeted metabolic profiling of liver samples by UPLC-MS.

    PubMed

    Masson, Perrine; Alves, Alexessander Couto; Ebbels, Timothy M D; Nicholson, Jeremy K; Want, Elizabeth J

    2010-09-15

    A series of six protocols were evaluated for UPLC-MS based untargeted metabolic profiling of liver extracts in terms of reproducibility and number of metabolite features obtained. These protocols, designed to extract both polar and nonpolar metabolites, were based on (i) a two stage extraction approach or (ii) a simultaneous extraction in a biphasic mixture, employing different volumes and combinations of extraction and resuspension solvents. A multivariate statistical strategy was developed to allow comparison of the multidimensional variation between the methods. The optimal protocol for profiling both polar and nonpolar metabolites was found to be an aqueous extraction with methanol/water followed by an organic extraction with dichloromethane/methanol, with resuspension of the dried extracts in methanol/water before UPLC-MS analysis. This protocol resulted in a median CV of feature intensities among experimental replicates of <20% for aqueous extracts and <30% for organic extracts. These data demonstrate the robustness of the proposed protocol for extracting metabolites from liver samples and make it well suited for untargeted liver profiling in studies exploring xenobiotic hepatotoxicity and clinical investigations of liver disease. The generic nature of this protocol facilitates its application to other tissues, for example, brain or lung, enhancing its utility in clinical and toxicological studies. PMID:20715759

  18. Pharmacokinetics screening for multi-components absorbed in the rat plasma after oral administration of traditional Chinese medicine Flos Lonicerae Japonicae-Fructus Forsythiae herb couple by sequential negative and positive ionization ultra-high-performance liquid chromatography/tandem triple quadrupole mass spectrometric detection.

    PubMed

    Zhou, Wei; Tam, Kin Y; Meng, Minxin; Shan, Jinjun; Wang, Shouchuan; Ju, Wenzheng; Cai, Baochang; Di, Liuqing

    2015-01-01

    The current study aims to investigate the pharmacokinetics of multi-components (caffeic acid, quinic acid, genistein, luteolin, quercetin, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, arctigenin, genistin, luteoloside, astragalin, hyperoside, isoquercitrin, 3,5-dicaffeoylquinic acid, 3,4-dicaffeoylquinic acid, rutin, loganin, pinoresinol-β-d-glucoside, phillyrin, isoforsythoside, forsythoside A and forsythoside B) following oral administration of Flos Lonicerae Japonicae-Fructus Forsythiae herb couple in rats. A rapid and sensitive UPLC-ESI-MS/MS with sequential positive and negative ionization modes was developed to determine the 23 absorbed ingredients using one sample preparation combined with three chromatographic conditions in rat plasma. After mixing with internal standard (IS) (tinidazole and chloramphenicol), samples were pretreated by liquid-liquid extraction (LLE) with n-butyl alcohol/ethyl acetate (1:1, v/v). The separations for pinoresinol-β-d-glucoside, phillyrin, isoforsythoside, forsythoside A and forsythoside B were performed on an ACQUITY UPLC BEH C18 column (100mm×2.1mm, 1.7μm) with acetonitrile/methanol (4:1, v/v)-water as mobile phase. For analyzing quinic acid, an ACQUITY UPLC HSS T3 column (100mm×2.1mm, 1.8μm) was applied with acetonitrile/methanol (4:1, v/v)-0.01% formic acid as mobile phase after dilution up to 25-fold. The same column was applied to the other components with acetonitrile/methanol (4:1, v/v)-0.4% formic acid as mobile phase. The method validation results demonstrated that the proposed method was sensitive, specific and reliable, which was successfully applied to the pharmacokinetic study of the multi-components after oral administration of Flos Lonicerae Japonicae-Fructus Forsythiae herb couple.

  19. Pharmacokinetics screening for multi-components absorbed in the rat plasma after oral administration of traditional Chinese medicine Flos Lonicerae Japonicae-Fructus Forsythiae herb couple by sequential negative and positive ionization ultra-high-performance liquid chromatography/tandem triple quadrupole mass spectrometric detection.

    PubMed

    Zhou, Wei; Tam, Kin Y; Meng, Minxin; Shan, Jinjun; Wang, Shouchuan; Ju, Wenzheng; Cai, Baochang; Di, Liuqing

    2015-01-01

    The current study aims to investigate the pharmacokinetics of multi-components (caffeic acid, quinic acid, genistein, luteolin, quercetin, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, arctigenin, genistin, luteoloside, astragalin, hyperoside, isoquercitrin, 3,5-dicaffeoylquinic acid, 3,4-dicaffeoylquinic acid, rutin, loganin, pinoresinol-β-d-glucoside, phillyrin, isoforsythoside, forsythoside A and forsythoside B) following oral administration of Flos Lonicerae Japonicae-Fructus Forsythiae herb couple in rats. A rapid and sensitive UPLC-ESI-MS/MS with sequential positive and negative ionization modes was developed to determine the 23 absorbed ingredients using one sample preparation combined with three chromatographic conditions in rat plasma. After mixing with internal standard (IS) (tinidazole and chloramphenicol), samples were pretreated by liquid-liquid extraction (LLE) with n-butyl alcohol/ethyl acetate (1:1, v/v). The separations for pinoresinol-β-d-glucoside, phillyrin, isoforsythoside, forsythoside A and forsythoside B were performed on an ACQUITY UPLC BEH C18 column (100mm×2.1mm, 1.7μm) with acetonitrile/methanol (4:1, v/v)-water as mobile phase. For analyzing quinic acid, an ACQUITY UPLC HSS T3 column (100mm×2.1mm, 1.8μm) was applied with acetonitrile/methanol (4:1, v/v)-0.01% formic acid as mobile phase after dilution up to 25-fold. The same column was applied to the other components with acetonitrile/methanol (4:1, v/v)-0.4% formic acid as mobile phase. The method validation results demonstrated that the proposed method was sensitive, specific and reliable, which was successfully applied to the pharmacokinetic study of the multi-components after oral administration of Flos Lonicerae Japonicae-Fructus Forsythiae herb couple. PMID:25533397

  20. Metabolomics driven analysis of six Nigella species seeds via UPLC-qTOF-MS and GC-MS coupled to chemometrics.

    PubMed

    Farag, Mohamed A; Gad, Haidy A; Heiss, Andreas G; Wessjohann, Ludger A

    2014-05-15

    Nigella sativa, commonly known as black cumin seed, is a popular herbal supplement that contains numerous phytochemicals including terpenoids, saponins, flavonoids, alkaloids. Only a few of the ca. 15 species in the genus Nigella have been characterized in terms of phytochemical or pharmacological properties. Here, large scale metabolic profiling including UPLC-PDA-MS and GC-MS with further multivariate analysis was utilized to classify 6 Nigella species. Under optimized conditions, we were able to annotate 52 metabolites including 8 saponins, 10 flavonoids, 6 phenolics, 10 alkaloids, and 18 fatty acids. Major peaks in UPLC-MS spectra contributing to the discrimination among species were assigned as kaempferol glycosidic conjugates, with kaempferol-3-O-[glucopyranosyl-(1→2)-galactopyranosyl-(1→2)-glucopyranoside, identified as potential taxonomic marker for N. sativa. Compared with GC-MS, UPLC-MS was found much more efficient in Nigella sample classification based on genetic and geographical origin. Nevertheless, both GC-MS and UPLC-MS support the remote position of Nigella nigellastrum in relation to the other taxa.

  1. Assessment of cosmetic ingredients in the in vitro reconstructed human epidermis test method EpiSkin™ using HPLC/UPLC-spectrophotometry in the MTT-reduction assay.

    PubMed

    Alépée, N; Hibatallah, J; Klaric, M; Mewes, K R; Pfannenbecker, U; McNamee, P

    2016-06-01

    Cosmetics Europe recently established HPLC/UPLC-spectrophotometry as a suitable alternative endpoint detection system for measurement of formazan in the MTT-reduction assay of reconstructed human tissue test methods irrespective of the test system involved. This addressed a known limitation for such test methods that use optical density for measurement of formazan and may be incompatible for evaluation of strong MTT reducer and/or coloured chemicals. To build on the original project, Cosmetics Europe has undertaken a second study that focuses on evaluation of chemicals with functionalities relevant to cosmetic products. Such chemicals were primarily identified from the Scientific Committee on Consumer Safety (SCCS) 2010 memorandum (addendum) on the in vitro test EpiSkin™ for skin irritation testing. Fifty test items were evaluated in which both standard photometry and HPLC/UPLC-spectrophotometry were used for endpoint detection. The results obtained in this study: 1) provide further support for Within Laboratory Reproducibility of HPLC-UPLC-spectrophotometry for measurement of formazan; 2) demonstrate, through use a case study with Basazol C Blue pr. 8056, that HPLC/UPLC-spectrophotometry enables determination of an in vitro classification even when this is not possible using standard photometry and 3) addresses the question raised by SCCS in their 2010 memorandum (addendum) to consider an endpoint detection system not involving optical density quantification in in vitro reconstructed human epidermis skin irritation test methods. PMID:26891813

  2. Development of an UPLC-MS/MS Sulfonamide Multi-residue Method and It's Application to Water, Manure Slurry, and Soils from Swine Rearing Facilities

    Technology Transfer Automated Retrieval System (TEKTRAN)

    An analytical method was developed using ultra performance liquid chromatography-triple quadrupole-tandem mass spectrophotometry (UPLC-TQ-MS/MS) to simultaneously analyze 14 sulfonamides (SA) in six minutes. The instrumental detection limit based on signal-to-noise ratio (S/N) > 3, was below 1 pg/µL...

  3. Quantitative determination of curcuminoids from the Roots of Curcuma longa, Curcuma species and dietary supplements using an UPLC-UV-MS method

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A simple, fast UPLC-UV-MS method was developed for the determination of curcuminoids from roots of Curcuma longa L., Curcuma species (C. zedoaria, C. phaecaulis, C. wenyujin and C. kwangsiensis) and dietary supplements claiming to contain C. longa. The total content of curcuminoids (curcumin, desmet...

  4. Simultaneous determination of alkaloids and flavonoids from aerial parts of Passiflora species and dietary supplements using UPLC-UV-MS and HPTLC

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A rapid UPLC method was developed for the simultaneous analysis of five indole alkaloids (harmalol, harmol, harmane, harmaline and harmine) and four flavonoids (orientin, isoorientin, vitexin, and isovitexin) from the aerial parts of Passiflora incarnata L. (Passifloracea), different species of Pass...

  5. Metabolomics driven analysis of six Nigella species seeds via UPLC-qTOF-MS and GC-MS coupled to chemometrics.

    PubMed

    Farag, Mohamed A; Gad, Haidy A; Heiss, Andreas G; Wessjohann, Ludger A

    2014-05-15

    Nigella sativa, commonly known as black cumin seed, is a popular herbal supplement that contains numerous phytochemicals including terpenoids, saponins, flavonoids, alkaloids. Only a few of the ca. 15 species in the genus Nigella have been characterized in terms of phytochemical or pharmacological properties. Here, large scale metabolic profiling including UPLC-PDA-MS and GC-MS with further multivariate analysis was utilized to classify 6 Nigella species. Under optimized conditions, we were able to annotate 52 metabolites including 8 saponins, 10 flavonoids, 6 phenolics, 10 alkaloids, and 18 fatty acids. Major peaks in UPLC-MS spectra contributing to the discrimination among species were assigned as kaempferol glycosidic conjugates, with kaempferol-3-O-[glucopyranosyl-(1→2)-galactopyranosyl-(1→2)-glucopyranoside, identified as potential taxonomic marker for N. sativa. Compared with GC-MS, UPLC-MS was found much more efficient in Nigella sample classification based on genetic and geographical origin. Nevertheless, both GC-MS and UPLC-MS support the remote position of Nigella nigellastrum in relation to the other taxa. PMID:24423541

  6. Assessment of cosmetic ingredients in the in vitro reconstructed human epidermis test method EpiSkin™ using HPLC/UPLC-spectrophotometry in the MTT-reduction assay.

    PubMed

    Alépée, N; Hibatallah, J; Klaric, M; Mewes, K R; Pfannenbecker, U; McNamee, P

    2016-06-01

    Cosmetics Europe recently established HPLC/UPLC-spectrophotometry as a suitable alternative endpoint detection system for measurement of formazan in the MTT-reduction assay of reconstructed human tissue test methods irrespective of the test system involved. This addressed a known limitation for such test methods that use optical density for measurement of formazan and may be incompatible for evaluation of strong MTT reducer and/or coloured chemicals. To build on the original project, Cosmetics Europe has undertaken a second study that focuses on evaluation of chemicals with functionalities relevant to cosmetic products. Such chemicals were primarily identified from the Scientific Committee on Consumer Safety (SCCS) 2010 memorandum (addendum) on the in vitro test EpiSkin™ for skin irritation testing. Fifty test items were evaluated in which both standard photometry and HPLC/UPLC-spectrophotometry were used for endpoint detection. The results obtained in this study: 1) provide further support for Within Laboratory Reproducibility of HPLC-UPLC-spectrophotometry for measurement of formazan; 2) demonstrate, through use a case study with Basazol C Blue pr. 8056, that HPLC/UPLC-spectrophotometry enables determination of an in vitro classification even when this is not possible using standard photometry and 3) addresses the question raised by SCCS in their 2010 memorandum (addendum) to consider an endpoint detection system not involving optical density quantification in in vitro reconstructed human epidermis skin irritation test methods.

  7. Ultra performance liquid chromatography PDA method for determination of tigecycline in human plasma.

    PubMed

    D'Avolio, Antonio; Peila, Emanuela; Simiele, Marco; Pensi, Debora; Baietto, Lorena; Cusato, Jessica; Cinnirella, Giacoma; De Rosa, Francesco; Di Perri, Giovanni

    2013-12-01

    : A simple ultra performance liquid chromatography with photodiode array method for the quantification of human plasma concentrations of tigecycline was developed and validated. Quinaxoline, used as an internal standard, was added to 500 μL of plasma before adding 1 mL of protein precipitation solution. The extracts were dried in a vacuum centrifuge system at 60°C and reconstituted with 60 μL of water and acetonitrile (95:5, vol/vol), and 5 μL was injected onto an ACQUITY UPLC H-Class system. Chromatographic separation was performed on a C18 ACQUITY UPLC HSS T3 column using a gradient of potassium phosphate buffer (pH 3.2) and acetonitrile. Detection was performed using a photodiode array detector at 350 nm. Relative error at 3 quality control concentrations ranged from -2.49% to -8.74%. Intraday and interday (percent relative standard error) precision ranged from 3.93% to 12.27% and from 9.53% to 13.32%, respectively. Limit of quantification and limit of detection were 0.024 and 0.006 μg/mL, respectively. Mean recovery was 95%. The calibration curve was linear up to 6 μg/mL. This concentration range proved to be adequate to measure tigecycline concentrations in patients treated with the drug, therefore this method would be suitable for therapeutic drug monitoring.

  8. A validated LC-MS-MS method for simultaneous identification and quantitation of rodenticides in blood.

    PubMed

    Bidny, Sergei; Gago, Kim; David, Mark; Duong, Thanh; Albertyn, Desdemona; Gunja, Naren

    2015-04-01

    A rapid, highly sensitive and specific analytical method for the extraction, identification and quantification of nine rodenticides from whole blood has been developed and validated. Commercially available rodenticides in Australia include coumatetralyl, warfarin, brodifacoum, bromadiolone, difenacoum, flocoumafen, difethialone, diphacinone and chlorophacinone. A Waters ACQUITY UPLC TQD system operating in multiple reaction monitoring mode was used to conduct the analysis. Two different ionization techniques, ES+ and ES-, were examined to achieve optimal sensitivity and selectivity resulting in detection by MS-MS using electrospray ionization in positive mode for difenacoum and brodifacoum and in negative mode for all other analytes. All analytes were extracted from 200 µL of whole blood with ethylacetate and separated on a Waters ACQUITY UPLC BEH-C18 column using gradient elution. Ammonium acetate (10 mM, pH 7.5) and methanol were used as mobile phases with a total run time of 8 min. Recoveries were between 70 and 105% with limits of detection ranging from 0.5 to 1 ng/mL. The limit of quantitation was 2 ng/mL for all analytes. Calibration curves were linear within the range 2-200 ng/mL for all analytes with the coefficient of determination ≥0.98. The application of the proposed method using liquid-liquid extraction in a series of clinical investigations and forensic toxicological analyses was successful. PMID:25595137

  9. Stage-frit: A straightforward sub-2 μm nano-liquid chromatography column fabrication for proteomic analysis.

    PubMed

    Hsieh, Ming-Yueh; Hsiao, He-Hsuan

    2015-07-30

    In this work we demonstrated a facile method for the fabrication of C18 coordination polymer gel in a capillary, called stage-frit, which was efficiently applied to pack sub-2 μm C18 beads into the capillary by a high pressure bomb for the online separation of proteolytic peptides. The back pressure of the column with 10 cm × 75 μm i.d. is regularly lower than 170 bar at a flow rate of 300 nl/min, which could be operated on a common nanoLC system instead of nanoUPLC system due to the good permeability, low back pressure and high mechanical stress of the frit that will totally reduce the cost for the purchase of instrument. The stage-frit allows long-term continuous flow of the solvent and no significant beads loss or pressure instability was observed during the period. The repeatability of retention time for fifteen BSA tryptic peaks was found to be less than 1.08% (RSD) in six time nanoLC-ESI-MS/MS experiments. The average full width at half maximum (FWHM) of peptide peaks is 5.87 s. The sub-2 μm stage-frit nanoLC column showed better sensitivity than the commercial available for large scale proteomic analysis of total tissue proteins from human spleen. The number of identified peptides is approximately 0.4-fold and 0.2-fold higher than that obtained by utilizing commercial columns packed with 3 μm and 1.8 μm C18 materials, respectively. In the field of analytical chemistry, particularly the use of nanoLC systems, stage-frit nanoLC column offers a great potential for the separation of complex mixtures. PMID:26320654

  10. Stage-frit: A straightforward sub-2 μm nano-liquid chromatography column fabrication for proteomic analysis.

    PubMed

    Hsieh, Ming-Yueh; Hsiao, He-Hsuan

    2015-07-30

    In this work we demonstrated a facile method for the fabrication of C18 coordination polymer gel in a capillary, called stage-frit, which was efficiently applied to pack sub-2 μm C18 beads into the capillary by a high pressure bomb for the online separation of proteolytic peptides. The back pressure of the column with 10 cm × 75 μm i.d. is regularly lower than 170 bar at a flow rate of 300 nl/min, which could be operated on a common nanoLC system instead of nanoUPLC system due to the good permeability, low back pressure and high mechanical stress of the frit that will totally reduce the cost for the purchase of instrument. The stage-frit allows long-term continuous flow of the solvent and no significant beads loss or pressure instability was observed during the period. The repeatability of retention time for fifteen BSA tryptic peaks was found to be less than 1.08% (RSD) in six time nanoLC-ESI-MS/MS experiments. The average full width at half maximum (FWHM) of peptide peaks is 5.87 s. The sub-2 μm stage-frit nanoLC column showed better sensitivity than the commercial available for large scale proteomic analysis of total tissue proteins from human spleen. The number of identified peptides is approximately 0.4-fold and 0.2-fold higher than that obtained by utilizing commercial columns packed with 3 μm and 1.8 μm C18 materials, respectively. In the field of analytical chemistry, particularly the use of nanoLC systems, stage-frit nanoLC column offers a great potential for the separation of complex mixtures.

  11. Determination of multicomponent contents in Calculus bovis by ultra-performance liquid chromatography-evaporative light scattering detection and its application for quality control.

    PubMed

    Kong, Weijun; Jin, Cheng; Xiao, Xiaohe; Zhao, Yanling; Liu, Wei; Li, Zulun; Zhang, Ping

    2010-06-01

    A fast ultra-performance liquid chromatography-evaporative light scattering detection (UPLC-ELSD) method was established for simultaneous quantification of seven components in natural Calculus bovis (C. bovis) and its substitutes or spurious breeds. On a Waters Acquity UPLC BEH C(18) column, seven analytes were efficiently separated using 0.2% aqueous formic acid-acetonitrile as the mobile phase in a gradient program. The evaporator tube temperature of ELSD was set at 100 degrees C with the nebulizing gas flow-rate of 1.9 L/min. The results showed that this established UPLC-ELSD method was validated to be sensitive, precise and accurate with the LODs of seven analytes at 2-11 ng, and the overall intra-day and inter-day variations less than 3.0%. The recovery of the method was in the range of 97.8-101.6%, with RSD less than 3.0%. Further results of PCA on the contents of seven investigated analytes suggested that compounds of cholic acid, deoxycholic acid and chenodeoxycholic acid or cholesterol should be added as chemical markers to UPLC analysis of C. bovis samples for quality control and to discriminate natural C. bovis sample and its substitutes or some spurious breeds, then normalize the use of natural C. bovis and ensure its clinical efficacy. PMID:20155752

  12. Oscillating water column structural model

    SciTech Connect

    Copeland, Guild; Bull, Diana L; Jepsen, Richard Alan; Gordon, Margaret Ellen

    2014-09-01

    An oscillating water column (OWC) wave energy converter is a structure with an opening to the ocean below the free surface, i.e. a structure with a moonpool. Two structural models for a non-axisymmetric terminator design OWC, the Backward Bent Duct Buoy (BBDB) are discussed in this report. The results of this structural model design study are intended to inform experiments and modeling underway in support of the U.S. Department of Energy (DOE) initiated Reference Model Project (RMP). A detailed design developed by Re Vision Consulting used stiffeners and girders to stabilize the structure against the hydrostatic loads experienced by a BBDB device. Additional support plates were added to this structure to account for loads arising from the mooring line attachment points. A simplified structure was designed in a modular fashion. This simplified design allows easy alterations to the buoyancy chambers and uncomplicated analysis of resulting changes in buoyancy.

  13. Characterization of polyacrylamide based monolithic columns.

    PubMed

    Plieva, Fatima M; Andersson, Jonatan; Galaev, Igor Yu; Mattiasson, Bo

    2004-07-01

    Supermacroporous monolithic polyacrylamide (pAAm)-based columns have been prepared by radical cryo-copolymerization (copolymerization in the moderately frozen system) of acrylamide with functional co-monomer, allyl glycidyl ether (AGE), and cross-linker N,N'-methylene-bis-acrylamide (MBAAm) directly in glass columns (ID 10 mm). The monolithic columns have uniform supermacroporous sponge-like structure with interconnected supermacropores of pore size 5-100 microm. The monoliths can be dried and stored in the dry state. High mechanical stability of the monoliths allowed sterilization by autoclaving. Column-to-column reproducibility of pAAm-monoliths was demonstrated on 5 monolithic columns from different batches prepared under the same cryostructuration conditions.

  14. Characterization of polyacrylamide based monolithic columns.

    PubMed

    Plieva, Fatima M; Andersson, Jonatan; Galaev, Igor Yu; Mattiasson, Bo

    2004-07-01

    Supermacroporous monolithic polyacrylamide (pAAm)-based columns have been prepared by radical cryo-copolymerization (copolymerization in the moderately frozen system) of acrylamide with functional co-monomer, allyl glycidyl ether (AGE), and cross-linker N,N'-methylene-bis-acrylamide (MBAAm) directly in glass columns (ID 10 mm). The monolithic columns have uniform supermacroporous sponge-like structure with interconnected supermacropores of pore size 5-100 microm. The monoliths can be dried and stored in the dry state. High mechanical stability of the monoliths allowed sterilization by autoclaving. Column-to-column reproducibility of pAAm-monoliths was demonstrated on 5 monolithic columns from different batches prepared under the same cryostructuration conditions. PMID:15354560

  15. REDISTRIBUTOR FOR LIQUID-LIQUID EXTRACTION COLUMNS

    DOEpatents

    Bradley, J.G.

    1957-10-29

    An improved baffle plate construction to intimately mix immiscible liquid solvents for solvent extraction processes in a liquid-liquid pulse column is described. To prevent the light and heavy liquids from forming separate continuous homogeneous vertical channels through sections of the column, a baffle having radially placed rectangular louvers with deflection plates opening upon alternate sides of the baffle is placed in the column, normal to the axis. This improvement substantially completely reduces strippiig losses due to poor mixing.

  16. Distillation of light hydrocarbons in packed columns

    SciTech Connect

    Strigle, R.F.

    1985-04-01

    Newly developed design procedures have led to a wider acceptance of packed columns for distillation operations, especially those operating at atmospheric or higher pressures. Based on these new design methods, modern IMTP packing has been used in a wide variety of services to revamp over 300 distillation columns previously equipped with trays. A few of these columns are listed. These revamps were justified by capacity increase and by greater product recovery. In addition, energy savings were realized from reduction of reflux ratio.

  17. Differentiating Milk and Non-milk Proteins by UPLC Amino Acid Fingerprints Combined with Chemometric Data Analysis Techniques.

    PubMed

    Lu, Weiying; Lv, Xiaxia; Gao, Boyan; Shi, Haiming; Yu, Liangli Lucy

    2015-04-22

    Amino acid fingerprinting combined with chemometric data analysis was used to differentiate milk and non-milk proteins in this study. Microwave-assisted hydrolysis and ultraperformance liquid chromatography (UPLC) were used to obtain the amino acid fingerprints. Both univariate and multivariate chemometrics methods were applied for differentiation. The confidence boundary of amino acid concentration, principal component analysis (PCA), and partial least-squares-discriminant analysis (PLS-DA) of the amino acid fingerprints demonstrated that there were significant differences between milk proteins and inexpensive non-milk protein powders from other biological sources including whey, peanut, corn, soy, fish, egg yolk, beef extract, collagen, and cattle bone. The results indicate that the amino acid compositions with the chemometric techniques could be applied for the detection of potential protein adulterants in milk.

  18. Myoglobin as marker in meat adulteration: a UPLC method for determining the presence of pork meat in raw beef burger.

    PubMed

    Giaretta, Nicola; Di Giuseppe, Antonella M A; Lippert, Martina; Parente, Augusto; Di Maro, Antimo

    2013-12-01

    The identification of meat animal species used in raw burgers is very important with respect to economic and religious considerations. Therefore, international supervisory bodies have implemented procedures to control the employed meat species. In this paper we propose myoglobin as a powerful molecular marker to evaluate the presence of non-declared meat addition in raw beef burgers by using ultra-performance liquid chromatography (UPLC) for the separation and identification of edible animal species (beef, chicken, horse, ostrich, pig and water buffalo). Meat samples were pre-treated with sodium nitrite to transform oxymyoglobin and deoxymyoglobin to the more stable metmyoglobin. The developed method was validated, preparing mixtures with different percentages of pork and beef minced meat. The obtained results show that using myoglobin as marker, 5% (25 mg/500 mg) of pork or beef meat can be detected in premixed minced meat samples.

  19. An improved UPLC method for the detection of undeclared horse meat addition by using myoglobin as molecular marker.

    PubMed

    Di Giuseppe, Antonella M A; Giarretta, Nicola; Lippert, Martina; Severino, Valeria; Di Maro, Antimo

    2015-02-15

    In 2013, following the scandal of the presence of undeclared horse meat in various processed beef products across the Europe, several researches have been undertaken for the safety of consumer health. In this framework, an improved UPLC separation method has been developed to detect the presence of horse myoglobin in raw meat samples. The separation of both horse and beef myoglobins was achieved in only seven minutes. The methodology was improved by preparing mixtures with different composition percentages of horse and beef meat. By using myoglobin as marker, low amounts (0.50mg/0.50g, w/w; ∼0.1%) of horse meat can be detected and quantified in minced raw meat samples with high reproducibility and sensitivity, thus offering a valid alternative to conventional PCR techniques.

  20. Analysis of steroidal alkaloids and saponins in Solanaceae plant extracts using UPLC-qTOF mass spectrometry.

    PubMed

    Heinig, Uwe; Aharoni, Asaph

    2014-01-01

    Plants of the Solanaceae family are renowned for the production of cholesterol-derived steroidal glycosides, including the nitrogen containing glycoalkaloids and steroidal saponins. In this chapter we describe the use of UPLC (Ultra Performance Liquid Chromatography) coupled with qTOF (Quadrupole Time-of-Flight) mass spectrometry for profiling of these two large classes of semipolar metabolites. The presented method includes an optimized sample preparation protocol, a procedure for high resolution chromatographic separation and metabolite detection using the TOF mass spectrometer which provides high resolution and mass accuracy. A detailed description for non-targeted data analysis and a strategy for putative identification of steroidal glycosides from complex extracts based on interpretation of mass fragmentation patterns is also provided. The described methodology allows profiling and putative identification of multiple steroidal glycoside compounds from the assortment of Solanaceae species producing these molecules.

  1. [Analysis on component difference in Citrus reticulata before and after being processed with salt by UPLC-Q-TOF/MS].

    PubMed

    Zeng, Rui; Fu, Juan; Wu, La-Bin; Huang, Lin-Fang

    2013-07-01

    To analyze components of Citrus reticulata and salt-processed C. reticulata by ultra-performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF/MS), and compared the changes in components before and after being processed with salt. Principal component analysis (PCA) and partial least squares discriminant analysis (OPLS-DA) were adopted to analyze the difference in fingerprint between crude and processed C. reticulata, showing increased content of eriocitrin, limonin, nomilin and obacunone increase in salt-processed C. reticulata. Potential chemical markers were identified as limonin, obacunone and nomilin, which could be used for distinguishing index components of crude and processed C. reticulata. PMID:24199563

  2. Interstitial gas effect on vibrated granular columns

    NASA Astrophysics Data System (ADS)

    Pastenes, Javier C.; Géminard, Jean-Christophe; Melo, Francisco

    2014-06-01

    Vibrated granular materials have been intensively used to investigate particle segregation, convection, and heaping. We report on the behavior of a column of heavy grains bouncing on an oscillating solid surface. Measurements indicate that, for weak effects of the interstitial gas, the temporal variations of the pressure at the base of the column are satisfactorily described by considering that the column, despite the observed dilation, behaves like a porous solid. In addition, direct observation of the column dynamics shows that the grains of the upper and lower surfaces are in free fall in the gravitational field and that the dilation is due to a small delay between their takeoff times.

  3. Soil column leaching of pesticides.

    PubMed

    Katagi, Toshiyuki

    2013-01-01

    In this review, I address the practical and theoretical aspects of pesticide soil mobility.I also address the methods used to measure mobility, and the factors that influence it, and I summarize the data that have been published on the column leaching of pesticides.Pesticides that enter the unsaturated soil profile are transported downwards by the water flux, and are adsorbed, desorbed, and/or degraded as they pass through the soil. The rate of passage of a pesticide through the soil depends on the properties of the pesticide, the properties of the soil and the prevailing environmental conditions.Because large amounts of many different pesticides are used around the world, they and their degradates may sometimes contaminate groundwater at unacceptable levels.It is for this reason that assessing the transport behavior and soil mobility of pesticides before they are sold into commerce is important and is one indispensable element that regulators use to assess probable pesticide safety. Both elementary soil column leaching and sophisticated outdoor lysimeter studies are performed to measure the leaching potential for pesticides; the latter approach more reliably reflects probable field behavior, but the former is useful to initially profile a pesticide for soil mobility potential.Soil is physically heterogeneous. The structure of soil varies both vertically and laterally, and this variability affects the complex flow of water through the soil profile, making it difficult to predict with accuracy. In addition, macropores exist in soils and further add to the complexity of how water flow occurs. The degree to which soil is tilled, the density of vegetation on the surface, and the type and amounts of organic soil amendments that are added to soil further affect the movement rate of water through soil, the character of soil adsorption sites and the microbial populations that exist in the soil. Parameters that most influence the rate of pesticide mobility in soil are

  4. Effect of column dimension on observed column efficiency in very high pressure liquid chromatography.

    PubMed

    Wu, Naijun; Bradley, Ashley C

    2012-10-26

    The effect of extra-column volume on observed linear velocity was investigated for columns of various internal diameters in very high pressure liquid chromatography. The results showed that the observed linear velocities were approximately 4.5, 9.5, 16.8, and 39.5% lower than the linear velocities corrected for the extra-column volume contribution for 4.6, 3.0, 2.1, and 1.0mm internal diameter columns, respectively. An empirical relationship between extra-column band broadening and extra-column volume was obtained using 50 cm long tubings of various internal diameters. The peak variance from the extra-column volume is near linearly proportional to the square of the extra-column volume for tubings with 0.0635-0.178 mm (0.025-0.07 in.) i.d. using a 50/50 acetonitrile/water mobile phase at flow rates greater than 0.3 mL/min. The effect of column internal diameter and column length on observed efficiency was studied using 50mm columns with four different column internal diameters and 2.1mm i.d columns with three different lengths. The results showed that the observed column efficiencies for 3.0, 2.1, and 1.0mm internal diameter columns were 18, 33, and 73% lower than that for a 4.6mm internal diameter column for benzophenone (k=5.5), respectively. An approximate 20% decrease in theoretical plate number was observed for propiophenone (k=3.3) using a 50 mm × 2.1 mm column packed with 1.7 μm particles compared to a 150 mm × 2.1 mm column packed with 5.0 μm particles, while the former column provided 9 fold faster separation. It is the column to extra column volume ratio instead of absolute extra-column volume that determines the degree of extra-column band-broadening in VHPLC.

  5. Ultra performance liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry for high-sensitivity and high-throughput analysis of U.S. Environmental Protection Agency 16 priority pollutants polynuclear aromatic hydrocarbons.

    PubMed

    Cai, Sheng-Suan; Syage, Jack A; Hanold, Karl A; Balogh, Michael P

    2009-03-15

    In this work, we demonstrate the utility of ultra performance liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry (UPLC-APPI-MS/MS) for high-sensitivity and high-throughput analysis of United States Environmental Protection Agency (U.S. EPA) 16 priority pollutants polycyclic aromatic hydrocarbons (PAHs). Analyses were performed on a Waters Acquity-TQD equipped with Syagen's PhotoMate APPI source. All 16 PAHs were analyzed on column in approximately 3.5 min with excellent chromatographic separation for all PAH isomers and with low picogram detection limits on column for all analytes using chlorobenzene as a dopant. Dynamic linear ranges were evaluated and found to cover at least 3-4 orders of magnitude. In comparison with the existing U.S. EPA methods, this approach improves instrument sample throughput by at least 10-fold.

  6. Optimal operation of multivessel batch distillation columns

    SciTech Connect

    Furlonge, H.I.; Pantelides, C.C.; Soerensen, E.

    1999-04-01

    Increased interest in unconventional batch distillation column configurations offers new opportunities for increasing the flexibility and energy efficiency of batch distillation. One configuration of particular interest is the multivessel column, which can be viewed as a generalization of all previously studied batch column configurations. A detailed dynamic model was used for comparing various optimal operating policies for a batch distillation column with two intermediate vessels. A wide variety of degrees of freedom including reflux ratios, product withdrawal rates, heat input to the reboiler, and initial feed distribution were considered. A mixture consisting of methanol, ethanol, n-propanol and n-butanol was studied using an objective function relating to the economics of the column operation. Optimizing the initial distribution of the feed among the vessels improved column performance significantly. For some separations, withdrawing product from the vessels into accumulators was better than total reflux operation in terms of energy consumption. Open-loop optimal operation was also compared to a recently proposed feedback control strategy where the controller parameters are optimized. The energy consumption of a regular column was about twice that of a multivessel column having the same number of stages.

  7. Circulation in gas-slurry column reactors

    SciTech Connect

    Clark, N.; Kuhlman, J.; Celik, I.; Gross, R.; Nebiolo, E.; Wang, Yi-Zun.

    1990-08-15

    Circulation in bubble columns, such as those used in fischer-tropsch synthesis, detracts from their performance in that gas is carried on average more rapidly through the column, and the residence time distribution of the gas in the column is widened. Both of these factors influence mass-transfer operations in bubble columns. Circulation prediction and measurement has been undertaken using probes, one-dimensional models, laser Doppler velocimetry, and numerical modeling. Local void fraction was measured using resistance probes and a newly developed approach to determining air/water threshold voltage for the probe. A tall column of eight inch diameter was constructed of Plexiglas and the distributor plate was manufactured to distribute air evenly through the base of the column. Data were gathered throughout the volume at three different gas throughputs. Bubble velocities proved difficult to measure using twin probes with cross-correlation because of radial bubble movement. A series of three-dimensional mean and RMS bubble and liquid velocity measurements were also obtained for a turbulent flow in a laboratory model of a bubble column. These measurements have been made using a three-component laser Doppler velocimeter (LDV), to determine velocity distributions non-intrusively. Finally, the gas-liquid flow inside a vertically situated circular isothermal column reactor was simulated numerically. 74 refs., 170 figs., 5 tabs.

  8. A UPLC-MS/MS method for simultaneous determination of danshensu, protocatechuic aldehyde, rosmarinic acid, and ligustrazine in rat plasma, and its application to pharmacokinetic studies of Shenxiong glucose injection in rats.

    PubMed

    Zheng, Lin; Gong, Zipeng; Lu, Yuan; Xie, Yumin; Huang, Yong; Liu, Yue; Lan, Yanyu; Wang, Aimin; Wang, Yonglin

    2015-08-01

    A rapid and sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of the four major active ingredients, danshensu, protocatechuic aldehyde, rosmarinic acid, and ligustrazine, in the traditional Chinese medicine Shenxiong glucose injection in rat plasma. Acidified and alkalized plasma samples were extracted using ethyl acetate, and separated on a Waters C18 column (2.1mm×50mm, 1.7μm) by using a gradient mobile phase system of acetonitrile-water containing 0.1% formic acid and luteoloside as an internal standard. Electrospray ionization in the positive-ion mode and multiple reaction monitoring were used to identify and quantitate the active components. All calibration curves showed good linearity (r>0.994) over the concentration range, with a lower limit of quantification (LLOQ) between 0.02 and 0.21μg/mL. The precision of the in vivo study was evaluated by intra- and inter-day assays, and the percentage of relative standard deviation was within 15%. Moreover, satisfactory extraction efficiency was obtained (between 83.94 and 117.81%) by liquid-liquid extraction. The validated method was successfully applied in a pharmacokinetic study in rats after intravenous administration of Shenxiong glucose injection. The results showed that the four bioactive ingredients in Shenxiong glucose injection have linear pharmacokinetic properties in rats after intravenous injection within the administered dose range and partially different ones compared to single ingredient. PMID:26118621

  9. Simultaneous determination of parecoxib sodium and its active metabolite valdecoxib in rat plasma by UPLC-MS/MS and its application to a pharmacokinetic study after intravenous and intramuscular administration.

    PubMed

    Liu, Meina; Yu, Qiuyang; Li, Ping; Zhu, Meng; Fang, Mingming; Sun, Bingjun; Sun, Mengchi; Sun, Yinghua; Zhang, Peng; He, Zhonggui; Sun, Jin; Wang, Yongjun; Liu, Xiaohong

    2016-06-01

    In this study, we developed and validated a new, rapid, specific and sensitive ultra-performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method to simultaneously determine parecoxib sodium (PX) and its active metabolite, valdecoxib (VX), in rat plasma. Plasma samples were prepared by plasma protein precipitation combined with a liquid-liquid extraction method. The separation was carried out on a Kinetex C18 column (2.1mm×50mm, 2.6μm) with a gradient elution using methanol (A) and a 2mM ammonium acetate aqueous solution (B). The analysis was performed in less than 3min with a flow rate of 0.2mL/min. Ketoprofen was used as an internal standard (IS). Mass spectrometric detection was conducted with a triple quadrupole detector equipped with electrospray ionization in the negative ion mode (ESI(-)) using multiple reaction monitoring (MRM). The calibration curves were linear over the concentration ranges of 5-4000ng/mL for PX and 5-2000ng/mL for VX with all correlation coefficients greater than 0.998. The intra- and inter-day relative standard deviations (RSD) for both analytes were within 15% and the accuracy was within 85-115% at all quality control levels. The mean extraction recoveries for all analytes obtained from three concentrations of QC plasma samples were more than 89.0% efficient. Selectivity, matrix effect, dilution integrity and stability were also validated. The method was successfully used to investigate the pharmacokinetics of PX and VX in rat plasma after intravenous and intramuscular administration of PX. PMID:27107851

  10. Development and application of a UPLC-MS/MS method for simultaneous determination of fenofibric acid and berberine in rat plasma: application to the drug-drug pharmacokinetic interaction study of fenofibrate combined with berberine after oral administration in rats.

    PubMed

    Li, Guofei; Yang, Fan; Liu, Mei; Su, Xianying; Zhao, Mingming; Zhao, Limei

    2016-07-01

    With the purpose of carrying out pharmacokinetic interaction studies ofnberberine (BBR) and fenofibrate (FBT), an UPLC-MS/MS method has been developed and validated. The analytes, BBR and fenofibric acid (FBA, metabolite of FBT) and the internal standard, tetrahydropalmatine, were extracted with dichloromethane-diethyl ether (3:2, v/v) and separated on an Agilent Eclipse XDB C18 column using a mobile phase composed of acetonitrile and water. With positive ion electrospray ionization, the analytes were monitored on a triple quadrupole mass spectrometer in multiple reaction monitoring mode. Linear calibration curves were obtained over the concentration ranges of 0.1-100.0 ng/mL for BBR and 10.0-50,000.0 ng/mL for FBA. For BBR and FBA, the intra- and inter-day precisions were <11.5 and 11.9%, respectively. The accuracy was within 11.7% and 11.3%. The mean recoveries of BBR at three concentrations of 0.2, 20.0, 80.0 ng/mL were >85.6%, and those of FBA at three concentrations of 20.0, 2500.0, 40,000.0 ng/mL were >87.9%. Consequently, the proposed method was applied to the pharmacokinetic interaction study of FBT combined with BBR after oral administration in rats and was proved to be sensitive, specific and reliable to analyze BBR and FBA in biological samples simultaneously. Copyright © 2016 John Wiley & Sons, Ltd.

  11. Use of HPLC/UPLC-spectrophotometry for detection of formazan in in vitro Reconstructed human Tissue (RhT)-based test methods employing the MTT-reduction assay to expand their applicability to strongly coloured test chemicals.

    PubMed

    Alépée, N; Barroso, J; De Smedt, A; De Wever, B; Hibatallah, J; Klaric, M; Mewes, K R; Millet, M; Pfannenbecker, U; Tailhardat, M; Templier, M; McNamee, P

    2015-06-01

    A number of in vitro test methods using Reconstructed human Tissues (RhT) are regulatory accepted for evaluation of skin corrosion/irritation. In such methods, test chemical corrosion/irritation potential is determined by measuring tissue viability using the photometric MTT-reduction assay. A known limitation of this assay is possible interference of strongly coloured test chemicals with measurement of formazan by absorbance (OD). To address this, Cosmetics Europe evaluated use of HPLC/UPLC-spectrophotometry as an alternative formazan measurement system. Using the approach recommended by the FDA guidance for validation of bio-analytical methods, three independent laboratories established and qualified their HPLC/UPLC-spectrophotometry systems to reproducibly measure formazan from tissue extracts. Up to 26 chemicals were then tested in RhT test systems for eye/skin irritation and skin corrosion. Results support that: (1) HPLC/UPLC-spectrophotometry formazan measurement is highly reproducible; (2) formazan measurement by HPLC/UPLC-spectrophotometry and OD gave almost identical tissue viabilities for test chemicals not exhibiting colour interference nor direct MTT reduction; (3) independent of the test system used, HPLC/UPLC-spectrophotometry can measure formazan for strongly coloured test chemicals when this is not possible by absorbance only. It is therefore recommended that HPLC/UPLC-spectrophotometry to measure formazan be included in the procedures of in vitro RhT-based test methods, irrespective of the test system used and the toxicity endpoint evaluated to extend the applicability of these test methods to strongly coloured chemicals.

  12. Modeling of column apparatuses: A review

    SciTech Connect

    Doichinova, M. E-mail: petyabs@yahoo.com; Popova-Krumova, P. E-mail: petyabs@yahoo.com

    2013-12-18

    This paper presents a review of the modeling method on the base of the physical approximations of the mechanics of continua, which have been developed for processes in column apparatuses. This method includes diffusion type of model for modeling of mass transfer with chemical reaction in column apparatuses with and without circulation zones. The diffusion type of model is used for modeling of scale effect in column apparatuses too. The study concluded that the proposal method is possibility for investigation the influence of radial non uniformity of the velocity distribution on the process efficiency, influence of zones breadths on the mass transfer efficiency in the column. The method of the column apparatuses modeling can be used for modeling of physical and chemical absorption, chemical adsorption, homogeneous and heterogeneous (catalytic) chemical reactions, airlift reactors for chemical and photochemical reactions.

  13. Statistical search space reduction and two-dimensional data display approaches for UPLC-MS in biomarker discovery and pathway analysis.

    PubMed

    Crockford, Derek J; Lindon, John C; Cloarec, Olivier; Plumb, Robert S; Bruce, Stephen J; Zirah, Severine; Rainville, Paul; Stumpf, Chris L; Johnson, Kelly; Holmes, Elaine; Nicholson, Jeremy K

    2006-07-01

    A new analytical strategy for biomarker recovery from directly coupled ultra-performance liquid chromatography time-of-flight mass spectrometry (UPLC Tof MS) data on biofluids is presented and exemplified using a study on hydrazine-induced liver toxicity. A key step in the strategy involves a novel procedure for reducing the spectroscopic search space by differential analysis of cohorts of normal and pathological samples using an orthogonal projection to latent structures discriminant analysis (O-PLS-DA). This efficiently sorts principal discriminators of toxicity from the background of thousands of metabolic features commonly observed in data sets generated by UPLC-MS analysis of biological fluids and is thus a powerful tool for biomarker discovery. PMID:16808447

  14. UPLC/Q-TOF-MS analysis of iridoid glycosides and metabolites in rat plasma after oral administration of Paederia scandens extracts.

    PubMed

    Wang, Dong-Mei; Xu, Yi-Fei; Chen, Zhu; Huang, Lin-Fang; Chen, Shi-Lin

    2015-03-01

    A rapid and validated UPLC-MS method was developed for investigating the absorbed components of Paederia scandens (Lour.) Merrill (P. scandensy) in rat plasma. The bioactive constituents in plasma samples from rats administrated orally with P. scandens extract were analyzed by Ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS). Four prototype compounds were identified in rat serum as potential bioactive components of P. scandens by comparing their retention times and mass spectrometry data or by mass spectrometry analysis and retrieving the reference literatures. Glucuronidation after deglycosylation was the major metabolic pathway for the iridoid glycosides in P. scandens. These results showed that the methods had high sensitivity and resolution and were suitable for identifying the bioactive constituents in plasma after oral administration of P. scandens. providing helpful chemical information for further pharmacological and mechanistic researched on the P. scandens. PMID:25835366

  15. Determination of total folates in infant formula and adult nutritionals by trienzyme extraction and UPLC-MS/MS Quantitation: First Action 2011.06.

    PubMed

    Szpylka, John; DeVries, Jon; Cheney, Andrea; House, Steve

    2012-01-01

    The method for "Determination of Total Folates in Infant Formula and Adult Nutritionals by Trienzyme Extraction and UPLC-MS/MS Quantitation" was submitted to the Folate Working Group for consideration for adoption as Official First Action by AOAC INTERNATIONAL. This method uses ultra performance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS) to determine the total folates in infant formulas and adult nutritionals after trienzyme digestion. Deconjugation of the various folate polyglutamates to folate monoglutamates is achieved by using rat plasma conjugase after the sample digestion with protease and a-amylase during the trienzyme digestion process. This method shows linearity of folate concentrations in the range of 10-19 100 microg/100 g. Extension of the range to cover folate concentrations of 5-2 000 000 microg/100 g can be achieved with appropriate adjustment of the sample weight and SPE cleanup loading volume. The recoveries ranged from 94.10 to 101.34%.

  16. Development and Validation of an UPLC-MS/MS Method for Simultaneous Determination of Ibuprofen and Promethazine in Tablets Stored on Board the International Space Station

    NASA Technical Reports Server (NTRS)

    Wu, L.; Chow, D. S.-L.; Daniels, V. R.

    2016-01-01

    Therapeutic efficacy and safety of pharmaceuticals remain a critical issue for successful NASA medical operations of long-term space missions on International Space Station (ISS). Medications stored aboard the ISS are subjected to unique environmental factors for extended time periods that may cause physicochemical degradation or alterations in the integrity of formulations that include the active pharmaceutical ingredient (API) and the chemical matrix of the formulation. Degradation of API and adjuvants, in addition to alterations of the chemical matrix of the formulation, can decrease potency and bioavailability and increase the risk due to toxicity of degraded medications. UPLC-MS/MS analysis is efficient and highly sensitive to quantify API content and MS analysis enables the elucidation of the structures of degradation products for each formulation. Therefore the aim of this project was to develop and validate a rapid, specific, and sensitive UPLC-MS/MS assay for the simultaneous determination of ibuprofen and promethazine in tablets stored aboard the ISS.

  17. Comparison of sample preparation methods, validation of an UPLC-MS/MS procedure for the quantification of tetrodotoxin present in marine gastropods and analysis of pufferfish.

    PubMed

    Nzoughet, Judith Kouassi; Campbell, Katrina; Barnes, Paul; Cooper, Kevin M; Chevallier, Olivier P; Elliott, Christopher T

    2013-02-15

    Tetrodotoxin (TTX) is one of the most potent marine neurotoxins reported. The global distribution of this toxin is spreading with the European Atlantic coastline now being affected. Climate change and increasing pollution have been suggested as underlying causes for this. In the present study, two different sample preparation techniques were used to extract TTX from Trumpet shells and pufferfish samples. Both extraction procedures (accelerated solvent extraction (ASE) and a simple solvent extraction) were shown to provide good recoveries (80-92%). A UPLC-MS/MS method was developed for the analysis of TTX and validated following the guidelines contained in the Commission Decision 2002/657/EC for chemical contaminant analysis. The performance of this procedure was demonstrated to be fit for purpose. This study is the first report on the use of ASE as a mean for TTX extraction, the use of UPLC-MS/MS for TTX analysis, and the validation of this method for TTX in gastropods.

  18. Highly efficient capillary columns packed with superficially porous particles via sequential column packing.

    PubMed

    Treadway, James W; Wyndham, Kevin D; Jorgenson, James W

    2015-11-27

    Highly efficient capillary columns packed with superficially porous particles were created for use in ultrahigh pressure liquid chromatography. Superficially porous particles around 1.5μm in diameter were packed into fused silica capillary columns with 30, 50, and 75μm internal diameters. To create the columns, several capillary columns were serially packed from the same slurry, with packing progress plots being generated to follow the packing of each column. Characterization of these columns using hydroquinone yielded calculated minimum reduced plate heights as low as 1.24 for the most efficient 30μm internal diameter column, corresponding to over 500,000plates/m. At least one highly efficient column (minimum reduced plate height less than 2) was created for all three of the investigated column inner diameters, with the smallest diameter columns having the highest efficiency. This study proves that highly efficient capillary columns can be created using superficially porous particles and shows the efficiency potential of these particles.

  19. Microwaves Scattering by Underdense Inhomogeneous Plasma Column

    NASA Astrophysics Data System (ADS)

    Zhang, Lin; Ouyang, Jiting

    2016-03-01

    The scattering characteristics of microwaves (MWs) by an underdense inhomogeneous plasma column have been investigated. The plasma column is generated by hollow cathode discharge (HCD) in a glass tube filled with low pressure argon. The plasma density in the column can be varied by adjusting the discharge current. The scattering power of X-band MWs by the column is measured at different discharge currents and receiving angles. The results show that the column can affect the properties of scattering wave significantly regardless of its plasma frequency much lower than the incident wave frequency. The power peak of the scattering wave shifts away from 0° to about ±15° direction. The finite-different time-domain (FDTD) method is employed to analyze the wave scattering by plasma column with different electron density distributions. The reflected MW power from a metal plate located behind the column is also measured to investigate the scattering effect on reducing MW reflectivity of a metal target. This study is expected to deepen the understanding of plasma-electromagnetic wave interaction and expand the applications concerning plasma antenna and plasma stealth.

  20. Mechanical interactions of UIS support columns. [LMFBR

    SciTech Connect

    Kennedy, J.M.; Belytschko, T.B.

    1983-01-01

    Code development involving above-core structures (ACS) has recently focused on modeling the complexities of mechanical interactions in the ACS support columns which play a very important role in their behavior. These developments are directed toward two considerations: (1) the prediction of the forces exerted by the column in a hypothetical core-disruptive accident (HCDA) in order that the motion of the ACS can be predicted in a coupled fluid-structure analysis, (2) the calculation of the strains and deformations of the support columns so that situations which lead to complete failure can be identified. Finite element capabilities have been developed to handle various types of plant design for the analysis of coupled hydrodynamics and structural response. Beam elements, which previously represented the support columns were able to account for geometric nonlinearities and material nonlinearities, however, changes in the column cross section were not treated. Therefore, one of the aims of this study was to examine the effect of the change in cross section on the behavior of the support columns. A second effect which has been studied is the behavior of support columns consisting of two concentric cylinders.

  1. Computational analysis and ratiometric comparison approaches aimed to assist column selection in hydrophilic interaction liquid chromatography-tandem mass spectrometry targeted metabolomics.

    PubMed

    Sampsonidis, Ioannis; Witting, Michael; Koch, Wendelin; Virgiliou, Christina; Gika, Helen G; Schmitt-Kopplin, Philippe; Theodoridis, Georgios A

    2015-08-01

    In the present work two different approaches, a semi-quantitative and a Derringer function approach, were developed to assist column selection for method development in targeted metabolomics. These approaches were applied in the performance assessment of three HILIC columns with different chemistries (an amide, a diol and a zwitterionic phase). This was the first step for the development of a HILIC UPLC-MS/MS method that should be capable to analyze a large number of polar metabolites. Two gradient elution profiles and two mobile phase pH values were tested for the analysis of multi-analyte mixtures. Acquired chromatographic data were firstly treated by a ratiometric, "semi-quantitative" approach which quantifies various overall analysis parameters (e.g. the percent of detected compounds, retentivity and resolved critical pairs). These parameters were used to assess chromatographic performance in a rather conventional/traditional and cumbersome/labor-intensive way. Secondly, a comprehensive and automated comparison of the three columns was performed by monitoring several well-known chromatographic parameters (peak width, resolution, tailing factor, etc.) using a lab-built programming script which calculates overall desirability utilizing Derringer functions. Derringer functions exhibit the advantage that column performance is ultimately expressed in an objective single and quantitative value which can be easily interpreted. In summary, results show that each column exhibits unique strengths in metabolic profiling of polar compounds. The applied methodology proved useful for the selection of the most effective chromatographic system during method development for LC-MS/MS targeted metabolomics, while it could further assist in the selection of chromatographic conditions for the development of multi-analyte methods.

  2. UPLC-MSE profiling of Phytoplankton metabolites: application to the identification of pigments and structural analysis of metabolites in Porphyridium purpureum.

    PubMed

    Juin, Camille; Bonnet, Antoine; Nicolau, Elodie; Bérard, Jean-Baptiste; Devillers, Romain; Thiéry, Valérie; Cadoret, Jean-Paul; Picot, Laurent

    2015-04-01

    A fast and high-resolution UPLC-MSE analysis was used to identify phytoplankton pigments in an ethanol extract of Porphyridium purpureum (Pp) devoid of phycobiliproteins. In a first step, 22 standard pigments were analyzed by UPLC-MSE to build a database including retention time and accurate masses of parent and fragment ions. Using this database, seven pigments or derivatives previously reported in Pp were unequivocally identified: β,β-carotene, chlorophyll a, zeaxanthin, chlorophyllide a, pheophorbide a, pheophytin a, and cryptoxanthin. Minor amounts of Divinyl chlorophyll a, a chemotaxonomic pigment marker for prochlorophytes, were also unequivocally identified using the database. Additional analysis of ionization and fragmentation patterns indicated the presence of ions that could correspond to hydroxylated derivatives of chlorophyll a and pheophytin a, produced during the ethanolic extraction, as well as previously described galactosyldiacylglycerols, the thylakoid coenzyme plastoquinone, and gracilamide B, a molecule previously reported in the red seaweed Gracillaria asiatica. These data point to UPLC-MSE as an efficient technique to identify phytoplankton pigments for which standards are available, and demonstrate its major interest as a complementary method for the structural elucidation of ionizable marine molecules. PMID:25913708

  3. Qualitative and quantitative analysis data of the major constituents of Ilex paraguariensis leaves by UPLC-PDA and QTOF-MS.

    PubMed

    Blum-Silva, Carlos Henrique; Luz, Ana Beatriz Gobbo; Nascimento, Marcus Vinicius P S; de Campos Facchin, Bruno Matheus; Baratto, Bruna; Fröde, Tânia Silvia; Sandjo, Louis Pergaud; Dalmarco, Eduardo Monguilhott; Reginatto, Flávio Henrique

    2016-09-01

    Ilex paraguariensis A. St. Hil. is a native plant of South America widely consumed as beverages for its ethno pharmacological properties, such as antioxidant, anti-inflammatory, hypocholesterolemic as well as its benefits on the cardiovascular system. Since these properties are related to its chemical composition, the identification and quantification of the major compounds of I. paraguariensis extracts still remains relevant. The data described in this article supports previous results on the anti-inflammatory effect of I. paraguariensis A. St. Hil (Mate), "The anti-inflammatory effect of I. paraguariensis A. St. Hil (Mate) in a murine model of pleurisy" [1]. The present data article reports on nine major compounds identified in I. paraguariensis extracts and its related fractions by using UPLC-PDA and UPLC-QTOF. Identification of the constituents was based on their retention times, UV absorption spectra and mass spectra data, as well as by comparison with authentic samples. The validated parameters show that the quantification by UPLC-PDA methodology developed is sensitive, precise and accurate. PMID:27331104

  4. Analysis of E. rutaecarpa Alkaloids Constituents In Vitro and In Vivo by UPLC-Q-TOF-MS Combined with Diagnostic Fragment

    PubMed Central

    Yang, Shenshen; Tian, Meng; Yuan, Lei; Deng, Haoyue; Wang, Lei; Li, Aizhu; Hou, Zhiguo; Li, Yubo

    2016-01-01

    Evodia rutaecarpa (Juss.) Benth. (Rutaceae) dried ripe fruit is used for dispelling colds, soothing liver, and analgesia. Pharmacological research has proved that alkaloids are the main active ingredients of E. rutaecarpa. This study aimed to rapidly classify and identify the alkaloids constituents of E. rutaecarpa by using UPLC-Q-TOF-MS coupled with diagnostic fragments. Furthermore, the effects of the material base of E. rutaecarpa bioactive ingredients in vivo were examined such that the transitional components in the blood of rats intragastrically given E. rutaecarpa were analyzed and identified. In this study, the type of alcohol extraction of E. rutaecarpa and the corresponding blood sample were used for the analysis by UPLC-Q-TOF-MS in positive ion mode. After reviewing much of the literature and collected information on the fragments, we obtained some diagnostic fragments of the alkaloids. Combining the diagnostic fragments with the technology of UPLC-Q-TOF-MS, we identified the compounds of E. rutaecarpa and blood samples and compared the ion fragment information with that of the alkaloids in E. rutaecarpa. A total of 17 alkaloids components and 6 blood components were identified. The proposed method was rapid, accurate, and sensitive. Therefore, this technique can reliably and practically analyze the chemical constituents in traditional Chinese medicine (TCM). PMID:27446630

  5. UPLC-MSE Profiling of Phytoplankton Metabolites: Application to the Identification of Pigments and Structural Analysis of Metabolites in Porphyridium purpureum

    PubMed Central

    Juin, Camille; Bonnet, Antoine; Nicolau, Elodie; Bérard, Jean-Baptiste; Devillers, Romain; Thiéry, Valérie; Cadoret, Jean-Paul; Picot, Laurent

    2015-01-01

    A fast and high-resolution UPLC-MSE analysis was used to identify phytoplankton pigments in an ethanol extract of Porphyridium purpureum (Pp) devoid of phycobiliproteins. In a first step, 22 standard pigments were analyzed by UPLC-MSE to build a database including retention time and accurate masses of parent and fragment ions. Using this database, seven pigments or derivatives previously reported in Pp were unequivocally identified: β,β-carotene, chlorophyll a, zeaxanthin, chlorophyllide a, pheophorbide a, pheophytin a, and cryptoxanthin. Minor amounts of Divinyl chlorophyll a, a chemotaxonomic pigment marker for prochlorophytes, were also unequivocally identified using the database. Additional analysis of ionization and fragmentation patterns indicated the presence of ions that could correspond to hydroxylated derivatives of chlorophyll a and pheophytin a, produced during the ethanolic extraction, as well as previously described galactosyldiacylglycerols, the thylakoid coenzyme plastoquinone, and gracilamide B, a molecule previously reported in the red seaweed Gracillaria asiatica. These data point to UPLC-MSE as an efficient technique to identify phytoplankton pigments for which standards are available, and demonstrate its major interest as a complementary method for the structural elucidation of ionizable marine molecules. PMID:25913708

  6. UPLC-ESI-Q-TOF-MS(E) identification of urinary metabolites of the emerging sport nutrition supplement methoxyisoflavone in human subjects.

    PubMed

    Lecompte, Yannick; Rosset, Martine; Richeval, Camille; Humbert, Luc; Arpino, Patrick

    2014-08-01

    Methoxyisoflavone (5-methyl-7-methoxyisoflavone) is a synthetic isoflavone used by bodybuilders for its ergogenic properties. A recent study demonstrated that methoxyisoflavone metabolites can induce false-positive results in urinary immunoassay screening tests for cannabinoids, and only one metabolite has been identified. To improve the knowledge on the metabolic pathways of methoxyisoflavone, ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF) was applied. Urine samples were obtained from methoxyisoflavone regular users. After enzymatic hydrolysis and liquid-liquid extraction, the samples were analyzed by UPLC-Q-TOF fitted with an electrospray ionization source (ESI) operating under positive ion mode. Mass data were acquired with the MS(E) method. Five metabolites were identified. Those were divided into two metabolic pathways, depending on whether the B ring hydroxylation was preceded or not by the O-demethylation of the methoxy group. The MS(E) mass spectra of methoxyisoflavone and its metabolites are specific of isoflavones structures and revealed 1,3 retro Diels-Alder fragmentation and double CO loss. Losses of small neutral molecules CO and H2O, and radical CH3, typical of flavonoids, were also observed. This study illustrates the capacity of the sensitive UPLC-Q-TOF analytical system, combined with the MS(E) method of collection of fragmentation data, to rapidly elucidate the unknown xenobiotics metabolism. PMID:24742771

  7. UPLC-MSE profiling of Phytoplankton metabolites: application to the identification of pigments and structural analysis of metabolites in Porphyridium purpureum.

    PubMed

    Juin, Camille; Bonnet, Antoine; Nicolau, Elodie; Bérard, Jean-Baptiste; Devillers, Romain; Thiéry, Valérie; Cadoret, Jean-Paul; Picot, Laurent

    2015-04-22

    A fast and high-resolution UPLC-MSE analysis was used to identify phytoplankton pigments in an ethanol extract of Porphyridium purpureum (Pp) devoid of phycobiliproteins. In a first step, 22 standard pigments were analyzed by UPLC-MSE to build a database including retention time and accurate masses of parent and fragment ions. Using this database, seven pigments or derivatives previously reported in Pp were unequivocally identified: β,β-carotene, chlorophyll a, zeaxanthin, chlorophyllide a, pheophorbide a, pheophytin a, and cryptoxanthin. Minor amounts of Divinyl chlorophyll a, a chemotaxonomic pigment marker for prochlorophytes, were also unequivocally identified using the database. Additional analysis of ionization and fragmentation patterns indicated the presence of ions that could correspond to hydroxylated derivatives of chlorophyll a and pheophytin a, produced during the ethanolic extraction, as well as previously described galactosyldiacylglycerols, the thylakoid coenzyme plastoquinone, and gracilamide B, a molecule previously reported in the red seaweed Gracillaria asiatica. These data point to UPLC-MSE as an efficient technique to identify phytoplankton pigments for which standards are available, and demonstrate its major interest as a complementary method for the structural elucidation of ionizable marine molecules.

  8. Neural network modeling of distillation columns

    SciTech Connect

    Baratti, R.; Vacca, G.; Servida, A.

    1995-06-01

    Neural network modeling (NNM) was implemented for monitoring and control applications on two actual distillation columns: the butane splitter tower and the gasoline stabilizer. The two distillation columns are in operation at the SARAS refinery. Results show that with proper implementation techniques NNM can significantly improve column operation. The common belief that neural networks can be used as black-box process models is not completely true. Effective implementation always requires a minimum degree of process knowledge to identify the relevant inputs to the net. After background and generalities on neural network modeling, the paper describes efforts on the development of neural networks for the two distillation units.

  9. The accretion column of AE Aqr

    NASA Astrophysics Data System (ADS)

    Rodrigues, Claudia; Costa, D. Joaquim; Luna, Gerardo; Lima, Isabel J.; Silva, Karleyne M. G.; De Araujo, Jose Carlos N.; Coelho, Jaziel

    2016-07-01

    AE Aqr is a magnetic cataclysmic variable, whose white dwarf rotates at the very fast rate of 33 s modulating the flux from high-energies to optical wavelengths. There are many studies of the origin of its emission, which consider emission from a rotating magnetic field or from an accretion column. Recently, MAGIC observations have discarded AE Aqr emission in very high energy gamma-rays discarding non-thermal emission. Furthermore, soft and hard X-ray data from Swift and NuSTAR were fitted using thermal models. Here we present the modelling of AE Aqr X-ray spectra and light curve considering the emission of a magnetic accretion column using the Cyclops code. The model takes into consideration the 3D geometry of the system, allowing to properly represent the white-dwarf auto eclipse, the pre-shock column absorption, and the varying density and temperature of a tall accretion column.

  10. PRTR ion exchange vault column sampling

    SciTech Connect

    Cornwell, B.C.

    1995-03-14

    This report documents ion exchange column sampling and Non Destructive Assay (NDA) results from activities in 1994, for the Plutonium Recycle Test Reactor (PRTR) ion exchange vault. The objective was to obtain sufficient information to prepare disposal documentation for the ion exchange columns found in the PRTR Ion exchange vault. This activity also allowed for the monitoring of the liquid level in the lower vault. The sampling activity contained five separate activities: (1) Sampling an ion exchange column and analyzing the ion exchange media for purpose of waste disposal; (2) Gamma and neutron NDA testing on ion exchange columns located in the upper vault; (3) Lower vault liquid level measurement; (4) Radiological survey of the upper vault; and (5) Secure the vault pending waste disposal.

  11. A Versatile, Automatic Chromatographic Column Packing Device

    ERIC Educational Resources Information Center

    Barry, Eugene F.; And Others

    1977-01-01

    Describes an inexpensive apparatus for packing liquid and gas chromatographic columns of high efficiency. Consists of stainless steel support struts, an Automat Getriebmotor, and an associated three-pulley system capable of 10, 30, and 300 rpm. (MLH)

  12. Fabrication of Graphite/Epoxy Column Elements

    NASA Technical Reports Server (NTRS)

    Bluck, R. M.; Grotbeck, G. H.; Reighard, W. M.

    1983-01-01

    Dimensionally precise columns wound on vertical mandrels. Dry fiber wound on tapered aluminum mandrel and outer sleeve. Winding and injection done at elevated temperature to minimize thermal-expansion problems during curing of resin. Technique used in textile industry.

  13. Modeling Tropical Precipitation in a Single Column.

    NASA Astrophysics Data System (ADS)

    Sobel, Adam H.; Bretherton, Christopher S.

    2000-12-01

    A modified formulation of the traditional single column model for representing a limited area near the equator is proposed. This formulation can also be considered a two-column model in the limit as the area represented by one of the columns becomes very large compared to the other. Only a single column is explicitly modeled, but its free tropospheric temperature, rather than its mean vertical velocity, is prescribed. This allows the precipitation and vertical velocity to be true prognostic variables, as in prior analytical theories of tropical precipitation. Two models developed by other authors are modified according to the proposed formulation. The first is the intermediate atmospheric model of J. D. Neelin and N. Zeng, but with the horizontal connections between columns broken, rendering it a set of disconnected column models. The second is the column model of N. O. Rennó, K. A. Emanuel, and P. H. Stone. In the first model, the set of disconnected column models is run with a fixed temperature that is uniform in the Tropics, and insolation, SST, and surface wind speed taken from a control run of the original model. The column models produce a climatological precipitation field that is grossly similar to that of the control run, despite that the circulation implied by the column models is not required to conserve mass. The addition of horizontal moisture advection by the wind from the control run substantially improves the simulation in dry regions. In the second model the sensitivity of the modeled steady-state precipitation and relative humidity to varying SST and wind speed is examined. The transition from shallow to deep convection is simulated in a `Lagrangian' calculation in which the column model is subjected to an SST that increases in time. In this simulation, the onset of deep convection is delayed to a higher SST than in the steady-state case, due to the effect of horizontal moisture advection (viewed in a Lagrangian reference frame). In both of the

  14. Flow in a metal hydride chromatographic column

    SciTech Connect

    Nichols, G.S.

    1990-01-01

    The flow of hydrogen isotopes in a metal hydride chromatographic column is calculated by a one-dimensional finite difference method. The Ergun equation is used to define the gas flow; and equilibrium pressure isotherms are used to define the column holdup. Solid phase loadings are shown to move as a wave front on absorption, but remain more uniform on desorption. 3 refs., 4 figs.

  15. Commander prepares glass columns for electrophoresis experiment

    NASA Technical Reports Server (NTRS)

    1982-01-01

    Commander Jack Lousma prepares on of the glass columns for the electrophoresis test in the middeck area of the Columbia. The experiment, deployed in an L-shaped mode in upper right corner, consists of the processing unit with glass columns in which the separation takes place; a camera (partially obscurred by Lousma's face) to document the process; and a cryogenic freezer to freeze and store the samples after separation.

  16. Avoid problems during distillation column startups

    SciTech Connect

    Sloley, A.W.

    1996-07-01

    The startup of a distillation column is the end product of the design process. Indeed, startup is the culmination of the theory and practice of designing the column to meet the process objectives. The author will direct most of this discussion towards column revamps due to their inherent complexity; however, the points apply equally to new columns, as well. The most important question that must be answered prior to a startup is how will the distillation system changes affect initial startup, process control of the system, and normal day-to-day operations? How will the operators run the system? Steady-state distillation-column simulations alone cannot provide an authoritative answer and, indeed, engineers` over-reliance on software too often has led them to ignore many practical aspects. Computer modeling, while an important engineering tool, is not reality. Distillation columns are real functioning pieces of equipment that require practical skills to successfully modify. They are not steady-state solutions that result from converged computer simulations. Early planning, coupled with thorough inspections and comprehensive reviews of instrumentation and procedures, can play a key role in assuring smooth startups.

  17. Interpretation of the lime column penetration test

    NASA Astrophysics Data System (ADS)

    Liyanapathirana, D. S.; Kelly, R. B.

    2010-06-01

    Dry soil mix (DSM) columns are used to reduce the settlement and to improve the stability of embankments constructed on soft clays. During construction the shear strength of the columns needs to be confirmed for compliance with technical assumptions. A specialized blade shaped penetrometer known as the lime column probe, has been developed for testing DSM columns. This test can be carried out as a pull out resistance test (PORT) or a push in resistance test (PIRT). The test is considered to be more representative of average column shear strength than methods that test only a limited area of the column. Both PORT and PIRT tests require empirical correlations of measured resistance to an absolute measure of shear strength, in a similar manner to the cone penetration test. In this paper, finite element method is used to assess the probe factor, N, for the PORT test. Due to the large soil deformations around the probe, an Arbitrary Lagrangian Eulerian (ALE) based finite element formulation has been used. Variation of N with rigidity index and the friction at the probe-soil interface are investigated to establish a range for the probe factor.

  18. Gas Chromatograph Method Optimization Trade Study for RESOLVE: 20-meter Column v. 8-meter Column

    NASA Technical Reports Server (NTRS)

    Huz, Kateryna

    2014-01-01

    RESOLVE is the payload on a Class D mission, Resource Prospector, which will prospect for water and other volatile resources at a lunar pole. The RESOLVE payload's primary scientific purpose includes determining the presence of water on the moon in the lunar regolith. In order to detect the water, a gas chromatograph (GC) will be used in conjunction with a mass spectrometer (MS). The goal of the experiment was to compare two GC column lengths and recommend which would be best for RESOLVE's purposes. Throughout the experiment, an Inficon Fusion GC and an Inficon Micro GC 3000 were used. The Fusion had a 20m long column with 0.25mm internal diameter (Id). The Micro GC 3000 had an 8m long column with a 0.32mm Id. By varying the column temperature and column pressure while holding all other parameters constant, the ideal conditions for testing with each column length in their individual instrument configurations were determined. The criteria used for determining the optimal method parameters included (in no particular order) (1) quickest run time, (2) peak sharpness, and (3) peak separation. After testing numerous combinations of temperature and pressure, the parameters for each column length that resulted in the most optimal data given my three criteria were selected. The ideal temperature and pressure for the 20m column were 95 C and 50psig. At this temperature and pressure, the peaks were separated and the retention times were shorter compared to other combinations. The Inficon Micro GC 3000 operated better at lower temperature mainly due to the shorter 8m column. The optimal column temperature and pressure were 70 C and 30psig. The Inficon Micro GC 3000 8m column had worse separation than the Inficon Fusion 20m column, but was able to separate water within a shorter run time. Therefore, the most significant tradeoff between the two column lengths was peak separation of the sample versus run time. After performing several tests, it was concluded that better

  19. Mass transfer model liquid phase catalytic exchange column simulation applicable to any column composition profile

    SciTech Connect

    Busigin, A.

    2015-03-15

    Liquid Phase Catalytic Exchange (LPCE) is a key technology used in water detritiation systems. Rigorous simulation of LPCE is complicated when a column may have both hydrogen and deuterium present in significant concentrations in different sections of the column. This paper presents a general mass transfer model for a homogenous packed bed LPCE column as a set of differential equations describing composition change, and equilibrium equations to define the mass transfer driving force within the column. The model is used to show the effect of deuterium buildup in the bottom of an LPCE column from non-negligible D atom fraction in the bottom feed gas to the column. These types of calculations are important in the design of CECE (Combined Electrolysis and Catalytic Exchange) water detritiation systems.

  20. Identification and comparative oridonin metabolism in different species liver microsomes by using UPLC-Triple-TOF-MS/MS and PCA.

    PubMed

    Ma, Yinghua; Xie, Weiwei; Tian, Tingting; Jin, Yiran; Xu, Huijun; Zhang, Kerong; Du, Yingfeng

    2016-10-15

    Oridonin (ORI) is an active natural ent-kaurene diterpenoid ingredient with notable anti-cancer and anti-inflammation activities. Currently, a strategy was developed to identify metabolites and to assess the metabolic profiles of ORI in vitro using ultra-high-performance liquid chromatography-Triple/time-of-flight mass spectrometry (UPLC-Triple-TOF-MS/MS). Meanwhile, the metabolism differences of ORI in the liver microsomes of four different species were investigated using a principal component analysis (PCA) based on the metabolite absolute peak area values as the variables. Based on the proposed methods, 27 metabolites were structurally characterized. The results indicate that ORI is universally metabolized in vitro, and the metabolic pathway mainly includes dehydration, hydroxylation, di-hydroxylation, hydrogenation, decarboxylation, and ketone formation. Overall, there are obvious inter-species differences in types and amounts of ORI metabolites in the four species. These results will provide basic data for future pharmacological and toxicological studies of ORI and for other ent-kauranes diterpenoids. Meanwhile, studying the ORI metabolic differences helps to select the proper animal model for further pharmacology and toxicological assessment. PMID:27503750

  1. Simultaneous detection and comparative pharmacokinetics of amoxicillin, clavulanic acid and prednisolone in cows' milk by UPLC-MS/MS.

    PubMed

    Liu, Yuan; Zhu, Kui; Wang, Jianfen; Huang, Xiaoyong; Wang, Guanlin; Li, Congying; Cao, Jie; Ding, Shuangyang

    2016-01-01

    Amoxicillin (AMOX), clavulanic acid (CLAV) and prednisolone (PSL) are widely used in combination for the treatment of mastitis in lactating dairy cows. However, no method has been reported to detect these three chemicals in milk in a single assay. In the present work, a reliable and sensitive UPLC-MS/MS method was developed and validated for simultaneous determination of AMOX, CLAV and PSL in cow's milk. The analytes were determined by a positive and negative ionization electrospray mass spectrometer via multiple reaction monitoring. The linear ranges of AMOX, CLAV and PSL were from 2 to 1000ng/mL, 20-1000ng/mL and 1-1000ng/mL, respectively, with the correlation coefficients greater than 0.999. The limits of quantification (LOQs) were 2ng/mL (AMOX), 20ng/mL (CLAV) and 1ng/mL (PSL). Recoveries of the analytes of interest in milk samples were in the ranges of 84.2-101.4%. The intra-day and inter-day precisions ranged from 1.8% to 11.9%. This method was successfully applied to investigate the pharmacokinetics of AMOX, CLAV and PSL in milk from healthy and mastitic cows. The elimination times of AMOX and PSL in mastitic cows were longer than that in healthy cows, but the elimination times of CLAV did not show significant difference.

  2. Structure elucidation of degradation products of Z-ligustilide by UPLC-QTOF-MS and NMR spectroscopy.

    PubMed

    Zuo, Ai-Hua; Cheng, Meng-Chun; Zhuo, Rong-Jie; Wang, Li; Xiao, Hong-Bin

    2013-06-01

    Z-Ligustilide, a major phthalide isolated from a widely used traditional Chinese medicine Ligusticum chuanxiong, possesses various pharmacological activities including neuroprotective, anti-inflammatory, antiproliferative and vasorelaxing effects. However, it is unstable and inclined to degrade in natural conditions, which limits its study and application greatly. In this study, degradation behavior of Z-ligustilide and its degradation products stored at room temperature under direct sunlight were investigated and structure elucidated by HPLC-UV, UPLC-QTOF-MS and NMR. Z-ligustilide degradation and total five degradation products were generated and detected. Two degradation products were unequivocally identified as senkyunolide I and senkyunolide H by comparison with reference compounds. Another two degradation products were further isolated by semi-preparative HPLC and structure elucidated as (E)-6, 7-trans-dihydroxyligustilide and (Z)-6, 7-epoxyligustilide by 1H and 13C NMR, respectively. The degradation pathways of Z-ligustilide were finally proposed. Oxidation, hydrolysis and isomerization are the major degradation reactions. PMID:23984528

  3. Determination of vitamin A in infant formula and adult nutritionals by UPLC-UV: First Action 2011.07.

    PubMed

    Trisconi, Marie-José; Campos-Gimenez, Esther; Jaudzems, Greg; Dowell, Dawn

    2012-01-01

    Vitamin A, a fat-soluble vitamin, is essential for health and plays an important part in vision, bone growth, reproduction, regulating the immune system, cell function, and skin health. Due to the advances in technology and the expansion of its uses, LC technologies are being studied for effectiveness in detecting and quantifying vitamin A in an effort to help determine the amount of vitamin A in various types of samples. For this reason, an Expert Review Panel agreed on June 29, 2011, at the "Standards Development and International Harmonization: AOAC INTERNATIONAL Mid-Year Meeting," to approve "Determination of Vitamin A in Infant Formula and Adult Nutritionals by UPLC-UV" as AOAC Official Method 2011.07. To move from First to Final Action status, it was recommended that additional information be generated for all types of infant formulas and adult nutritional formula matrixes at varied concentration levels, as indicated in the standard method performance requirements. International units or retinol equivalents typically represent the concentration of vitamin A in food and supplements. However, for the purpose of this method, the concentration represented is presented in microg/100 g. PMID:22649910

  4. Monitoring sea lamprey pheromones and their degradation using rapid stream-side extraction coupled with UPLC-MS/MS

    USGS Publications Warehouse

    Wang, Huiyong; Johnson, Nicholas; Bernardy, Jeffrey; Hubert, Terry; Li, Weiming

    2013-01-01

    Pheromones guide adult sea lamprey (Petromyzon marinus) to suitable spawning streams and mates, and therefore, when quantified, can be used to assess population size and guide management. Here, we present an efficient sample preparation method where 100 mL of river water was spiked with deuterated pheromone as an internal standard and underwent rapid field-based SPE and elution in the field. The combination of field extraction with laboratory UPLC-MS/MS reduced the sample consumption from 1 to 0.1 L, decreased the sample process time from more than 1 h to 10 min, and increased the precision and accuracy. The sensitivity was improved more than one order of magnitude compared with the previous method. The influences of experimental conditions were assessed to optimize the separation and peak shapes. The analytical method has been validated by studies of stability, selectivity, precision, and linearity and by the determination of the limits of detection and quantification. The method was used to quantify pheromone concentration from five streams tributary to Lake Ontario and to estimate that the environmental half-life of 3kPZS is about 26 h.

  5. Immunoadjuvant activity, toxicity assays, and determination by UPLC/Q-TOF-MS of triterpenic saponins from Chenopodium quinoa seeds.

    PubMed

    Verza, Simone G; Silveira, Fernando; Cibulski, Samuel; Kaiser, Samuel; Ferreira, Fernando; Gosmann, Grace; Roehe, Paulo M; Ortega, George G

    2012-03-28

    The adjuvant activity of Chenopodium quinoa (quinoa) saponins on the humoral and cellular immune responses of mice subcutaneously immunized with ovalbumin (OVA) was evaluated. Two quinoa saponin fractions were obtained, FQ70 and FQ90, and 10 saponins were determined by UPLC/Q-TOF-MS. Mice were immunized subcutaneously with OVA alone or adjuvanted with Quil A (adjuvant control), FQ70, or FQ90. FQ70 and FQ90 significantly enhanced the amount of anti-OVA-specific antibodies in serum (IgG, IgG1, and IgG2b) in immunized mice. The adjuvant effect of FQ70 was significantly greater than that of FQ90. However, delayed type hypersensitivity responses were higher in mice immunized with OVA adjuvanted with FQ90 than mice treated with FQ70. Concanavalin A (Con A)-, lipopolysaccharide-, and OVA-stimulated splenocyte proliferation were measured, and FQ90 significantly enhanced the Con A-induced splenocyte proliferation. The results suggested that the two quinoa saponin fractions enhanced significantly the production of humoral and cellular immune responses to OVA in mice.

  6. Determination of vitamin A in infant formula and adult nutritionals by UPLC-UV: First Action 2011.07.

    PubMed

    Trisconi, Marie-José; Campos-Gimenez, Esther; Jaudzems, Greg; Dowell, Dawn

    2012-01-01

    Vitamin A, a fat-soluble vitamin, is essential for health and plays an important part in vision, bone growth, reproduction, regulating the immune system, cell function, and skin health. Due to the advances in technology and the expansion of its uses, LC technologies are being studied for effectiveness in detecting and quantifying vitamin A in an effort to help determine the amount of vitamin A in various types of samples. For this reason, an Expert Review Panel agreed on June 29, 2011, at the "Standards Development and International Harmonization: AOAC INTERNATIONAL Mid-Year Meeting," to approve "Determination of Vitamin A in Infant Formula and Adult Nutritionals by UPLC-UV" as AOAC Official Method 2011.07. To move from First to Final Action status, it was recommended that additional information be generated for all types of infant formulas and adult nutritional formula matrixes at varied concentration levels, as indicated in the standard method performance requirements. International units or retinol equivalents typically represent the concentration of vitamin A in food and supplements. However, for the purpose of this method, the concentration represented is presented in microg/100 g.

  7. Determination of microcystin-LR in drinking water using UPLC tandem mass spectrometry-matrix effects and measurement.

    PubMed

    Li, Wei; Duan, Jinming; Niu, Chaoying; Qiang, Naichen; Mulcahy, Dennis

    2011-10-01

    A simple detection method using ultra-performance liquid chromatography electrospray ionisation tandem mass spectrometry (UPLC-ESI-MS-MS) coupled with the sample dilution method for determining trace microcystin-LR (MC-LR) in drinking water is presented. The limit of detection (LOD) was 0.04 µg/L and the limit of quantitation (LOQ) was 0.1 µg/L. Water matrix effects of ionic strength, dissolved organic carbon (DOC) and pH were examined. The results indicate that signal detection intensity for MC-LR was significantly suppressed as the ionic strength increased from ultrapure water condition, whereas it increased slightly with solution pH and DOC at low concentrations. However, addition of methanol (MeOH) into the sample was able to counter the signal suppression effects. In this study, dilution of the tap water sample by adding 4% MeOH (v/v) was observed to be adequate to compensate for the signal suppression. The recoveries of the samples fortified with MC-LR (0.2, 1, and 10 µg/L) for three different tap water samples ranged from 84.4% to 112.9%.

  8. Development of an UPLC-MS/MS method for the determination of antibiotic ertapenem on dried blood spots.

    PubMed

    la Marca, Giancarlo; Giocaliere, Elisa; Villanelli, Fabio; Malvagia, Sabrina; Funghini, Silvia; Ombrone, Daniela; Filippi, Luca; De Gaudio, Marina; De Martino, Maurizio; Galli, Luisa

    2012-03-01

    Ertapenem (Invanz) is a newly developed carbapenem β-lactam antimicrobial agent. The drug usage in pediatric age needs an accurate drug monitoring for effective patient management. The aim of this study was to evaluate the use of dried blood spot (DBS) specimens to measure ertapenem concentration during treatment. The analysis was performed by UPLC-MS/MS operating in multiple reaction monitoring (MRM) mode. The calibration curve in matrix was linear in the concentration range of 0.5-100 mg/L with correlation coefficient value higher than 0.997. Performance parameters of this method like lower limit of detection (LLOD, 0.2 mg/L), lower limit of quantification (LLOQ, 0.5 mg/L), matrix effect (20%), intra- and inter-day imprecision (CV within than 15%) and accuracy (between 94 and 155%) of drug concentrations have been evaluated. The drug stability at different temperatures was tested for one month, to evaluate the risks of sample delivery at different climatic conditions. The reported method allows now ertapenem analysis and offers many advantages for patients including the possibility of collecting samples at home. This new assay is both precise and accurate and is especially suitable for therapeutic drug monitoring and pharmacokinetic studies in neonates in whom obtaining larger blood samples is not convenient or possible.

  9. Validation of JWH-018 and its metabolites in blood and urine by UPLC-MS/MS: Monitoring in forensic cases.

    PubMed

    Erol Öztürk, Yeter; Yeter, Oya; Alpertunga, Buket

    2015-03-01

    The herbal products referred to as 'Spice' have been used as 'legal alternatives' to cannabis worldwide since 2004. The first synthetic cannabinoid JWH-018 was detected in 'Spice' products in 2008, and has been banned by many legal authorities since the beginning of 2009. In order to prove use of JWH cannabinoids (JWHs), specific and robust methods were needed. We have developed a specific and reliable method for the detection and quantification of JWH-018, JWH-018 N-pentanoic acid, and JWH-018 N-(5-hydroxypentyl) in blood and urine using solid-phase extraction followed by UPLC-MS/MS analysis. The method has been validated in terms of linearity (0.1-50ng/mL), selectivity, intra-assay and inter-assay accuracy and precision (CV<15%), recovery (85-98%), limits of detection (LOD) (0.08-0.14ng/mL), and quantification (LOQ) (0.10-0.21ng/mL). Matrix effects, stability, and process efficiency were also assessed. The method has been applied to 868 authentic samples received by the Department of Chemistry (Istanbul) in the Council of Forensic Medicine of the Ministry of Justice.

  10. A sensitive analytical procedure for monitoring acrylamide in environmental water samples by offline SPE-UPLC/MS/MS.

    PubMed

    Togola, Anne; Coureau, Charlotte; Guezennec, Anne-Gwenaëlle; Touzé, Solène

    2015-05-01

    The presence of acrylamide in natural systems is of concern from both environmental and health points of view. We developed an accurate and robust analytical procedure (offline solid phase extraction combined with UPLC/MS/MS) with a limit of quantification (20 ng L(-1)) compatible with toxicity threshold values. The optimized (considering the nature of extraction phases, sampling volumes, and solvent of elution) solid phase extraction (SPE) was validated according to ISO Standard ISO/IEC 17025 on groundwater, surface water, and industrial process water samples. Acrylamide is highly polar, which induces a high variability during the SPE step, therefore requiring the use of C(13)-labeled acrylamide as an internal standard to guarantee the accuracy and robustness of the method (uncertainty about 25 % (k = 2) at limit of quantification level). The specificity of the method and the stability of acrylamide were studied for these environmental media, and it was shown that the method is suitable for measuring acrylamide in environmental studies.

  11. Analysis of Hydroxy Fatty Acids from the Pollen of Brassica campestris L. var. oleifera DC. by UPLC-MS/MS

    PubMed Central

    Yang, Nian-Yun; Yang, Yi-Fang; Li, Kun

    2013-01-01

    Ultraperformance liquid chromatography coupled with negative electrospray tandem mass spectrometry (UPLC-ESI-MS/MS) was used to determine 7 hydroxy fatty acids in the pollen of Brassica campestris L. var. oleifera DC. All the investigated hydroxy fatty acids showed strong deprotonated molecular ions [M–H]−, which underwent two major fragment pathways of the allyl scission and the β-fission of the alcoholic hydroxyl group. By comparison of their molecular ions and abundant fragment ions with those of reference compounds, they were tentatively assigned as 15,16-dihydroxy-9Z,12Z-octadecadienoic acid (1), 10,11,12-trihydroxy-(7Z,14Z)-heptadecadienoic acid (2), 7,15,16-trihydroxy-9Z,12Z-octadecadienoic acid (3), 15,16-dihydroxy-9Z,12Z-octadecadienoic acid (4), 15-hydroxy-6Z,9Z,12Z-octadecatrienoic acid (5), 15-hydroxy-9Z,12Z- octadecadienoic acid (6), and 15-hydroxy-12Z-octadecaenoic acid (7), respectively. Compounds 3, 5, and 7 are reported for the first time. PMID:26555998

  12. A sensitive analytical procedure for monitoring acrylamide in environmental water samples by offline SPE-UPLC/MS/MS.

    PubMed

    Togola, Anne; Coureau, Charlotte; Guezennec, Anne-Gwenaëlle; Touzé, Solène

    2015-05-01

    The presence of acrylamide in natural systems is of concern from both environmental and health points of view. We developed an accurate and robust analytical procedure (offline solid phase extraction combined with UPLC/MS/MS) with a limit of quantification (20 ng L(-1)) compatible with toxicity threshold values. The optimized (considering the nature of extraction phases, sampling volumes, and solvent of elution) solid phase extraction (SPE) was validated according to ISO Standard ISO/IEC 17025 on groundwater, surface water, and industrial process water samples. Acrylamide is highly polar, which induces a high variability during the SPE step, therefore requiring the use of C(13)-labeled acrylamide as an internal standard to guarantee the accuracy and robustness of the method (uncertainty about 25 % (k = 2) at limit of quantification level). The specificity of the method and the stability of acrylamide were studied for these environmental media, and it was shown that the method is suitable for measuring acrylamide in environmental studies. PMID:25471720

  13. Column Selection for Biomedical Analysis Supported by Column Classification Based on Four Test Parameters.

    PubMed

    Plenis, Alina; Rekowska, Natalia; Bączek, Tomasz

    2016-01-21

    This article focuses on correlating the column classification obtained from the method created at the Katholieke Universiteit Leuven (KUL), with the chromatographic resolution attained in biomedical separation. In the KUL system, each column is described with four parameters, which enables estimation of the FKUL value characterising similarity of those parameters to the selected reference stationary phase. Thus, a ranking list based on the FKUL value can be calculated for the chosen reference column, then correlated with the results of the column performance test. In this study, the column performance test was based on analysis of moclobemide and its two metabolites in human plasma by liquid chromatography (LC), using 18 columns. The comparative study was performed using traditional correlation of the FKUL values with the retention parameters of the analytes describing the column performance test. In order to deepen the comparative assessment of both data sets, factor analysis (FA) was also used. The obtained results indicated that the stationary phase classes, closely related according to the KUL method, yielded comparable separation for the target substances. Therefore, the column ranking system based on the FKUL-values could be considered supportive in the choice of the appropriate column for biomedical analysis.

  14. Column Selection for Biomedical Analysis Supported by Column Classification Based on Four Test Parameters

    PubMed Central

    Plenis, Alina; Rekowska, Natalia; Bączek, Tomasz

    2016-01-01

    This article focuses on correlating the column classification obtained from the method created at the Katholieke Universiteit Leuven (KUL), with the chromatographic resolution attained in biomedical separation. In the KUL system, each column is described with four parameters, which enables estimation of the FKUL value characterising similarity of those parameters to the selected reference stationary phase. Thus, a ranking list based on the FKUL value can be calculated for the chosen reference column, then correlated with the results of the column performance test. In this study, the column performance test was based on analysis of moclobemide and its two metabolites in human plasma by liquid chromatography (LC), using 18 columns. The comparative study was performed using traditional correlation of the FKUL values with the retention parameters of the analytes describing the column performance test. In order to deepen the comparative assessment of both data sets, factor analysis (FA) was also used. The obtained results indicated that the stationary phase classes, closely related according to the KUL method, yielded comparable separation for the target substances. Therefore, the column ranking system based on the FKUL-values could be considered supportive in the choice of the appropriate column for biomedical analysis. PMID:26805819

  15. Post Column Derivatization Using Reaction Flow High Performance Liquid Chromatography Columns.

    PubMed

    Jones, Andrew; Pravadali-Cekic, Sercan; Hua, Stanley; Kocic, Danijela; Camenzuli, Michelle; Dennis, Gary; Shalliker, Andrew

    2016-04-26

    A protocol for the use of reaction flow high performance liquid chromatography columns for methods employing post column derivatization (PCD) is presented. A major difficulty in adapting PCD to modern HPLC systems and columns is the need for large volume reaction coils that enable reagent mixing and then the derivatization reaction to take place. This large post column dead volume leads to band broadening, which results in a loss of observed separation efficiency and indeed detection in sensitivity. In reaction flow post column derivatization (RF-PCD) the derivatization reagent(s) are pumped against the flow of mobile phase into either one or two of the outer ports of the reaction flow column where it is mixed with column effluent inside a frit housed within the column end fitting. This technique allows for more efficient mixing of the column effluent and derivatization reagent(s) meaning that the volume of the reaction loops can be minimized or even eliminated altogether. It has been found that RF-PCD methods perform better than conventional PCD methods in terms of observed separation efficiency and signal to noise ratio. A further advantage of RF-PCD techniques is the ability to monitor effluent coming from the central port in its underivatized state. RF-PCD has currently been trialed on a relatively small range of post column reactions, however, there is currently no reason to suggest that RF-PCD could not be adapted to any existing one or two component (as long as both reagents are added at the same time) post column derivatization reaction.

  16. Analysis of stone-column reinforced foundations

    NASA Astrophysics Data System (ADS)

    Lee, J. S.; Pande, G. N.

    1998-12-01

    A numerical model is proposed to analyse elastic as well as elastoplastic behaviour of stone-column reinforced foundations. The stone-columns are assumed to be dispersed within the in situ soil and a homogenization technique is invoked to establish equivalent material properties for in situ soil and stone-column composite. The difficulties encountered in carrying out elastoplastic analyses of composite materials are overcome by adopting a separate yield function for each of the constituent materials and a sub-iteration procedure within an implicit backward Euler stress integration scheme. In the proposed procedure, equilibrium as well as kinematic conditions implied in the homogenization procedure are satisfied for both elastic as well as elastoplastic stress states.The proposed model is implemented in an axi-symmetric finite element code and numerical prediction is made for the behaviour of model circular footings resting on stone-column reinforced foundations. This prediction indicates good agreement with experimental observation. Finally, a new scheme in which the length of stone-column is variable is proposed and its behaviour is examined through a numerical example.

  17. Counterflow isotachophoresis in a monolithic column.

    PubMed

    Liu, Bingwen; Cong, Yongzheng; Ivory, Cornelius F

    2014-09-01

    This study describes stationary counterflow isotachophoresis (ITP) in a poly(acrylamide-co-N,N'-methylenebisacrylamide) monolithic column as a means for improving ITP processing capacity and reducing dispersion. The flow profile in the monolith was predicted using COMSOL's Brinkman Equation application mode, which revealed that the flow profile was mainly determined by monolith permeability. As monolith permeability decreases, the flow profile changes from a parabolic shape to a plug shape. An experimental monolithic column was prepared in a fused-silica capillary using an ultraviolet-initiated polymerization method. A monolithic column made from 8% (wt.) monomer was chosen for the stationary counterflow ITP experiments. Counterflow ITP in the monolithic column showed undistorted analyte zones with significantly reduced dispersion compared to the severe dispersion observed in an open capillary. Particularly, for r-phycoerythrin focused by counterflow ITP, its zone width in the monolithic column was only one-third that observed in an open capillary. These experiments demonstrate that stationary counterflow ITP in monoliths can be a robust and practical electrofocusing method.

  18. Non-planar microfabricated gas chromatography column

    DOEpatents

    Lewis, Patrick R.; Wheeler, David R.

    2007-09-25

    A non-planar microfabricated gas chromatography column comprises a planar substrate having a plurality of through holes, a top lid and a bottom lid bonded to opposite surfaces of the planar substrate, and inlet and outlet ports for injection of a sample gas and elution of separated analytes. A plurality of such planar substrates can be aligned and stacked to provide a longer column length having a small footprint. Furthermore, two or more separate channels can enable multi-channel or multi-dimensional gas chromatography. The through holes preferably have a circular cross section and can be coated with a stationary phase material or packed with a porous packing material. Importantly, uniform stationary phase coatings can be obtained and band broadening can be minimized with the circular channels. A heating or cooling element can be disposed on at least one of the lids to enable temperature programming of the column.

  19. Methylmercury production in the marine water column

    NASA Astrophysics Data System (ADS)

    Topping, G.; Davies, I. M.

    1981-03-01

    Although the biosynthesis of methylmercury in sediments is well established1, this is not necessarily the exclusive natural source of methylmercury entering the marine food chain, particularly commercial fish and shellfish species for human consumption. An examination of mercury levels in freshwater fish2, collected from a lake with a history of industrial mercury contamination, suggested that levels in fish are controlled in part by mercury in suspension and it followed that methylation should occur in the water column. Although methylmercury is present in seawater in coastal areas receiving discharges of waste containing either inorganic mercury3 or methylmercury4 there is no evidence that methylmercury is actually formed in the water column. We now present data which demonstrate that inorganic mercury can be methylated in the water column and we compare this production with that known to occur in marine sediments.

  20. Neutron camera employing row and column summations

    DOEpatents

    Clonts, Lloyd G.; Diawara, Yacouba; Donahue, Jr, Cornelius; Montcalm, Christopher A.; Riedel, Richard A.; Visscher, Theodore

    2016-06-14

    For each photomultiplier tube in an Anger camera, an R.times.S array of preamplifiers is provided to detect electrons generated within the photomultiplier tube. The outputs of the preamplifiers are digitized to measure the magnitude of the signals from each preamplifier. For each photomultiplier tube, a corresponding summation circuitry including R row summation circuits and S column summation circuits numerically add the magnitudes of the signals from preamplifiers for each row and for each column to generate histograms. For a P.times.Q array of photomultiplier tubes, P.times.Q summation circuitries generate P.times.Q row histograms including R entries and P.times.Q column histograms including S entries. The total set of histograms include P.times.Q.times.(R+S) entries, which can be analyzed by a position calculation circuit to determine the locations of events (detection of a neutron).

  1. Cadmium removal in a biosorption column

    SciTech Connect

    Volesky, B.; Prasetyo, I. . Dept. of Chemical Engineering)

    1994-05-01

    New biosorbent material derived from a ubiquitous brown marine alga Ascophyllum nodosum has been examined in packed-bed flow-through sorption columns. It effectively removed 10 mg/L of cadmium down to 1.5 ppb levels in the effluent, representing 99.985% removal. The experimental methodology used was based on the early Bohart and Adams sorption model, resulting in quantitative determination of the characteristic process parameters which can be used for performance comparison and process design. An average metal loading of the biosorbent (N[sub 0]) determined was 30 mg Cd/g, corresponding closely to that observed for the batch equilibrium metal concentration of 10 mg Cd/L. The critical bed depth (D[sub min]) for the potable water effluent quality standard varied with the column feed flow rate from 20 to 50 cm. The sorption column mass transfer and dispersion coefficients were determined, which are also required for solving the sorption model equations.

  2. Final Report, Distillation Column Flooding Predictor

    SciTech Connect

    George E. Dzyacky

    2003-05-31

    The Flooding Predictor is an advanced process control strategy comprising a patented pattern-recognition methodology that identifies pre-flood patterns discovered to precede flooding events in distillation columns. The grantee holds a U.S. patent on the modeling system. The technology was validated at the Separations Research Program, The University of Texas at Austin under a grant from the U. S. Department of Energy, Inventions & Innovation Program. Distillation tower flooding occurs at abnormally high vapor and/or liquid rates. The loss in tray efficiencies is attributed to unusual behavior of liquid inventories inside the column leading to conditions of flooding of the space in between trays with liquid. Depending on the severity of the flood condition, consequences range from off spec products to equipment damage and tower shutdown. This non-intrusive pattern recognition methodology, processes signal data obtained from existing column instrumentation. Once the pattern is identified empirically, it is modeled and coded into the plant's distributed control system. The control system is programmed to briefly "unload" the tower each time the pattern appears. The unloading takes the form of a momentary reduction in column severity, e.g., decrease bottom temperature, reflux or tower throughput. Unloading the tower briefly at the pre-flood state causes long-term column operation to become significantly more stable - allowing an increase in throughput and/or product purity. The technology provides a wide range of value between optimization and flooding. When a distillation column is not running at capacity, it should be run in such a way ("pushed") that optimal product purity is achieved. Additional benefits include low implementation and maintenance costs, and a high level of console operator acceptance. The previous commercial applications experienced 98% uptime over a four-year period. Further, the technology is unique in its ability to distinguish between different

  3. Determination of dexmedetomidine in children's plasma by ultra-performance liquid chromatography tandem mass spectrometry and application to pharmacokinetic study.

    PubMed

    Liu, Hua-Cheng; Sun, Wei; Wang, Cheng-Yu; Ying, Wei-Yang; Zheng, Li-Dan; Zeng, Rui-Feng; Wang, Zhe; Ge, Ren-Shan

    2016-06-15

    A rapid, sensitive, and selective ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed and validated for the determination and pharmacokinetic investigation of dexmedetomidine in children's plasma. Sample preparation was accomplished through a simple one-step deproteinization procedure with 0.2mL of acetonitrile to a 0.1mL plasma sample. Plasma samples were separated by UPLC on an Acquity UPLC BEH C18 column using a mobile phase consisting of acetonitrile-0.1% formic acid in water with gradient elution. The total run time was 3.1min and the elution of dexmedetomidine was at 1.24min. The detection was performed on a triple quadrupole tandem mass spectrometer in the multiple reaction-monitoring mode using the respective transitions m/z 201.3→95.1 for dexmedetomidine and m/z 204.2→98.0 for the internal standard, respectively. The calibration curve was linear over the range of 0.05-10ng/mL with a lower limit of quantitation of 0.05ng/mL. Mean recovery rate of dexmedetomidine in plasma was in the range of 86.7-89.1%. Intra-day and inter-day precision were both <11.6%. This method was successfully applied in pharmacokinetic study after commencement of 1.0μg/kg dexmedetomidine infusion in children. PMID:27179189

  4. [Determination of 12 sulfonamides in cosmetics by ultra performance liquid chromatography].

    PubMed

    Zheng, Hehui; Wang, Ping; Li, Jie

    2007-03-01

    A method for the determination of 12 sulfonamides (SAs) (sulfanilamide, sulfamonomethoxine, sulfacetamide, sulfamethoxazole, sulfadiazine, sulfisoxazole, sulfathiazole, sulfadi-methoxine, sulfamerazine, sulfaquinoxaline, sulfamethazine, sulfanitran) in cosmetics was developed by ultra performance liquid chromatography with photodiode array detector (UPLC-PDA). The chromatographic column used was Acquity UPLC BEHC C18 (50 mm x 2. 1 mm, 1. 7 microm) and the mobile phase was acetonitrile-0. 1% formic acid aqueous solution. A gradient elution program was utilized for the separation and determination. After liquid-liquid extraction, SAs were separated and detected by UPLC-PDA. The qualification analysis was done by using retention time and spectrum, and the quantification was based on the detection wavelength of 268 nm. The limits of qualification (S/N = 3) and quantification (S/N = 10) for 12 SAs were 1 microg/g and 2 -3 microg/g, respectively. The correlation coefficient of linear calibration curve was over 0. 999 7 within the SAs concentration range of 1 - 25 mg/L (except sulfanitran 0. 5 - 12. 5 mg/L). At the spiked levels of 40 and 8 microg (except sulfanitran 20 and 4 microg), the average recoveries for 12 SAs were 86. 8% - 98. 1% and 80. 1% - 96. 9%, respectively. Relative standard deviations were less than 10%. Routine tests show that the method is simple, fast, and has a good separation efficiency. It can be routinely used for the determination of these SAs in cosmetics. PMID:17580695

  5. Simultaneous determination of 21 preservatives in cosmetics by ultra performance liquid chromatography.

    PubMed

    Wu, T; Wang, C; Wang, X; Ma, Q

    2008-10-01

    An ultra performance liquid chromatography (UPLC) method has been developed for the simultaneous determination of 21 preservatives: 2-methyl-4-isothiazoline-3-ketone, bronopol, 5-chloro-2-methyl-4-isothiazoline-3-ketone, benzyl alcohol, 2-phenoxyethanol, methyl-p-hydroxy benzoate, ethyl-p-hydroxy benzoate, methyl benzoate, 4-hydroxybenzoic acid iso-propyl ester, propyl-p-hydroxy benzoate, 4-chloro-3-methylphenol, ethyl benzoate, 2-phenylphenol, 4-hydroxybenzoic acid iso-butyl ester, butyl-p-hydroxy benzoate, 4-chloro-3,5-dimethylphenol, phenyl benzoate, 2,4-dichloro-3,5-dimethylphenol, 2-benzyl-4-chlorophenol, triclocarban and triclosan in cosmetics. A Waters ACQUITY UPLC BEH C(18) column was used with 0.1% formic acid solution as the mobile phase under the condition of gradient elution. Preservatives were extracted with methanol by ultrasonicator, and then they were analysed by UPLC-PDA detector. All these preservatives were baseline separated in 8.5 min. The pre-treatment method of samples and the chromatographic condition of analysis were critically examined in this study. The recoveries ranged from 90.5 to 97.8%, with RSD values below 3.2%, and all correlation coefficients (r) were no less than 0.9997. Thus, this method could be used for analysing the preservatives in cosmetic products.

  6. Determination of nine sensitizing disperse dyes in activated sludge by ultrasound-assisted liquid-liquid extraction-ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry.

    PubMed

    Zhou, Linjun; Shi, Lili; Liu, Jining; Lv, Fenglan; Xu, Yanhua

    2016-01-01

    A method was developed on the basis of ultrasound-assisted liquid-liquid extraction ultra-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (ULLE-UPLC-ESI-MS/MS) to determine nine sensitizing disperse dyes in activated sludge. The samples were extracted using ULLE and separated through UPLC on an ACQUITY UPLCTM BEH C18 column with a gradient elution program of acetonitrile and acidified water (containing 2% acetonitrile, 0.2% formic acid, and 0.005 mol/L ammonium; pH 2.7) as the mobile phase. The samples were then identified and quantified through UPLC-ESI-MS/MS in a positive mode and multiple reaction monitoring. Results showed good linearity (10-1000 μg/L, 0.9934-0.9998), detection limit (0.08-2.17 μg/L), and quantification limit (0.27-7.38 μg/L) for the nine sensitizing disperse dyes, with recoveries ranging from 65.0 to 111.3%. The proposed method was applied to detect and determine the concentration of sensitizing disperse dyes in sludge samples obtained from various sewage treatment plants (six dyeing enterprises and one dye manufacturer). Three sensitizing disperse dyes were identified, and the lowest concentration detected was 10 μg/kg.

  7. 29 CFR 1926.756 - Beams and columns.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 29 Labor 8 2011-07-01 2011-07-01 false Beams and columns. 1926.756 Section 1926.756 Labor... (CONTINUED) SAFETY AND HEALTH REGULATIONS FOR CONSTRUCTION Steel Erection § 1926.756 Beams and columns. (a.... (c) (1) Double connections at columns and/or at beam webs over a column. When two structural...

  8. 29 CFR 1926.756 - Beams and columns.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 29 Labor 8 2013-07-01 2013-07-01 false Beams and columns. 1926.756 Section 1926.756 Labor... (CONTINUED) SAFETY AND HEALTH REGULATIONS FOR CONSTRUCTION Steel Erection § 1926.756 Beams and columns. (a.... (c) (1) Double connections at columns and/or at beam webs over a column. When two structural...

  9. 29 CFR 1926.756 - Beams and columns.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 29 Labor 8 2012-07-01 2012-07-01 false Beams and columns. 1926.756 Section 1926.756 Labor... (CONTINUED) SAFETY AND HEALTH REGULATIONS FOR CONSTRUCTION Steel Erection § 1926.756 Beams and columns. (a.... (c) (1) Double connections at columns and/or at beam webs over a column. When two structural...

  10. 29 CFR 1926.756 - Beams and columns.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 29 Labor 8 2010-07-01 2010-07-01 false Beams and columns. 1926.756 Section 1926.756 Labor... (CONTINUED) SAFETY AND HEALTH REGULATIONS FOR CONSTRUCTION Steel Erection § 1926.756 Beams and columns. (a.... (c) (1) Double connections at columns and/or at beam webs over a column. When two structural...

  11. Determination of ω-6 and ω-3 PUFA metabolites in human urine samples using UPLC/MS/MS.

    PubMed

    Sasaki, Ai; Fukuda, Hayato; Shiida, Narumi; Tanaka, Nobuaki; Furugen, Ayako; Ogura, Jiro; Shuto, Satoshi; Mano, Nariyasu; Yamaguchi, Hiroaki

    2015-02-01

    The ω-6 and ω-3 polyunsaturated fatty acids (PUFAs) such as arachidonic acid (AA), eicosapentaenoic acid (EPA), and docosahexaenoic acid (DHA) are the precursors of various bioactive lipid mediators including prostaglandins, thromboxanes, leukotrienes, hydroxyeicosatetraenoic acid, isoprostanes, lipoxins, and resolvins (Rvs). These lipid mediators play important roles in various physiological and pathological processes. The quantitative determination of PUFA metabolites seems necessary for disease research and for developing biomarkers. However, there is a paucity of analytical methods for the quantification of ω-6 and ω-3 PUFA metabolites—the specialized pro-resolving mediators (SPMs) present in the human urine. We developed a method for the quantification of ω-6 and ω-3 PUFA metabolites present in human urine using ultra-performance liquid chromatography/tandem mass spectrometry (UPLC/MS/MS). The developed method shows good linearity, with a correlation coefficient >0.99 for all of the analytes. The validation results indicate that our method is adequately reliable, accurate, and precise. The method was successfully used to examine urine samples obtained from 43 healthy volunteers. We could identify 20 PUFA metabolites, and this is the first report of the quantitative determination of RvD1, 17(R)-RvD1, 11-dehydro thromboxane B3, RvE2, and 5(S)-HETE in human urine. The urinary 8-iso PGF(2α) and PGE2 levels were significantly higher in the men smokers than in the men nonsmokers (p < 0.05). In this study, we developed an accurate, precise, and novel analytical method for estimating the ω-6 and ω-3 PUFA metabolites, and this is the first report that the SPMs derived from EPA and DHA are present in human urine.

  12. Development and validation of an UPLC-PDA method to quantify daptomycin in human plasma and in dried plasma spots.

    PubMed

    Baietto, Lorena; D'Avolio, Antonio; Pace, Simone; Simiele, Marco; Marra, Cristina; Ariaudo, Alessandra; Di Perri, Giovanni; De Rosa, Francesco Giuseppe

    2014-01-01

    Quantification of daptomycin in plasma samples may be useful in optimizing therapy especially in special patients' population. Nevertheless, therapeutic drug monitoring of daptomycin is still limited probably for the low number of laboratories which perform this analysis and for high shipment costs. We developed and validated a new UPLC-PDA method to quantify daptomycin in plasma and in dried plasma spots (DPS) collected on dried sample spots devices (DSSD). Daptomycin and quinoxaline, used as internal standard, were monitored at 262nm and 253nm, respectively. Daptomycin was extracted from plasma using acetonitrile and from DPS using an extraction solution (ethyl acetate-acetic acid-acetone-water; 50:20:20:10, v/v/v/v). Both assays were linear over the calibration range of 0.781 to 200μg/ml. Considering the method of extraction from plasma, mean intra and inter-day accuracy was -1.18% and -2.79%, respectively. Mean intra and inter-day precision was 7.91% and 9.22%, respectively. Regarding the extraction method from DPS, mean intra and inter-day accuracy was 2.21% and 2.41%, respectively. Mean intra and inter-day precision was 8.01% and 9.19%, respectively. Daptomycin in DPS was found to be stable for 7 days at room temperature (20-25°C) and for at least 30 days at 4°C. A statistically significant (p<0.001) linear correlation was found between daptomycin extracted from plasma and from DPS (r(2)=0.919). DPS represents a safe and cheap strategy to store and ship plasma samples. Thus, it is suited for pharmacokinetic studies and therapeutic drug monitoring of daptomycin in hospitals without a therapeutic drug monitoring laboratory.

  13. Development and validation of a new UPLC-PDA method to quantify linezolid in plasma and in dried plasma spots.

    PubMed

    Baietto, Lorena; D'Avolio, Antonio; Ariaudo, Alessandra; Corcione, Silvia; Simiele, Marco; Cusato, Jessica; Urbino, Rosario; Di Perri, Giovanni; Ranieri, V Marco; De Rosa, Francesco Giuseppe

    2013-10-01

    Linezolid is an oxazolidinone antibiotic used for the treatment of pneumonia and uncomplicated and complicated skin and soft tissues infections caused by Gram positive bacteria. It is also used as second line agent in multi-drug resistant tuberculosis. Therapeutic drug monitoring (TDM) of linezolid represents a valid tool in clinical practice to optimize therapy, especially in critically ill patients. Spreading of TDM is mainly limited by high costs shipment and lack of laboratories that offer a TDM service. To overcome these problems, the use of dried plasma spots or dried blood spots is increasing. The aim of this work was to develop and validate a new chromatographic method to analyze linezolid in plasma and in dried plasma spots and to evaluate the correlation between the two extraction methods. Linezolid extraction from plasma and from dried plasma spots was obtained using acetonitrile. Quinoxaline was used as internal standard. Analysis was performed by an ultra performance liquid chromatography (UPLC) system coupled with photo diode array (PDA) detector, at 254nm. Both analytical methods were linear (r(2)>0.999) over the calibration range of 30-0.117mg/L. Limit of quantification and limit of detection were 0.117mg/L and 0.058mg/L, respectively. Intra and inter-day precision (R.S.D.%) and accuracy (%) were <15%. Long term stability of linezolid in dried plasma spots showed absence of degradation at room temperature (20-25°C) and at 4°C, for at least one month. Linear regression analysis confirmed that the two methods of extraction have good correlation. Thus they are suited for TDM of linezolid and for pharmacokinetic studies.

  14. Seasonal and Species Variation of the Hepatotoxin Indospicine in Australian Indigofera Legumes As Measured by UPLC-MS/MS.

    PubMed

    Tan, Eddie T T; Materne, Christopher M; Silcock, Richard G; D'Arcy, Bruce R; Al Jassim, Rafat; Fletcher, Mary T

    2016-08-31

    Livestock industries have maintained a keen interest in pasture legumes because of the high protein content and nutritive value. Leguminous Indigofera plant species have been considered as having high feeding values to be utilized as pasture, but the occurrence of the toxic constituent indospicine in some species has restricted this utility. Indospicine has caused both primary and secondary hepatotoxicosis and also reproductive losses, but has only previously been determined in a small number of Indigofera species. This paper validates a high-throughput ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method to determine the indospicine content of various Indigofera species found in Australian pasture. Twelve species of Indigofera together with Indigastrum parviflorum plants were collected and analyzed. Of the 84 samples analyzed, *I. spicata (the asterisk indicates a naturalized species) contained the highest indospicine level (1003 ± 328 mg/kg DM, n = 4) followed by I. linnaei (755 ± 490 mg/kg DM, n = 51). Indospicine was not detected in 9 of the remaining 11 species and at only low levels (<10 mg/kg DM) in 2 of 8 I. colutea specimens and in 1 of 5 I. linifolia specimens. Indospicine concentrations were below quantitation levels for other Indigofera spp. (I. adesmiifolia, I. georgei, I. hirsuta, I. leucotricha, *I. oblongifolia, I. australis, and I. trita) and Indigastrum parviflorum. One of the more significant findings to emerge from this study is that the indospicine content of I. linnaei is highly variable (from 159 to 2128 mg/kg DM, n = 51) and differs across both regions and seasons. Its first regrowth after spring rain has a higher (p < 0.01) indospicine content than growth following more substantial summer rain. The species collected include the predominant Indigofera in Australia pasture, and of these, only *I. spicata and I. linnaei contain high enough levels of indospicine to pose a potential toxic threat to grazing

  15. Determination of benzoxazinoids in wheat and rye beers by HPLC-DAD and UPLC-QTOF MS.

    PubMed

    Pihlava, Juha-Matti; Kurtelius, Tuula

    2016-08-01

    Phenolic compounds in beer have received considerable interest. Besides the more typical phenolic acids and flavonoids, beer contains also lesser-known compounds, such as hordatines, their agmatine precursors and other phenolamines. Current work shows that beers brewed from wheat or rye malts, in addition to barley malts, contain benzoxazinoids, a group of nitrogen containing secondary metabolites typical to wheat and rye. In this work, HPLC-DAD was used for the quantification of major benzoxazinoids in 32 wheat and four rye beers. Of the wheat beers 22 samples and all of the rye beers contained benzoxazinoids, or their breakdown products. Concentrations of DIBOA (2,4-dihydroxy-1,4-benzoxazin-3-one) (as aglycon) varied from 1.7 to 21.9mg/l in wheat beers and from 5.6 to 31.6mg/l in rye beers. Breakdown products BOA (benzoxazolin-2-one), found in 15 beers, and MBOA (6-methoxy-benzoxazolin-2-one), found in two beers, were measured at concentrations ranging from 2.4 to 10.7mg/l and 8.4 to 10.5mg/l, respectively. Identification of benzoxazinoids by UPLC-QTOF MS was done on selected beers. Benzoxazinoid profiles varied greatly between different wheat beers, and compared to rye beers the chemical diversity of benzoxazinoids was higher. As far as the authors know, this is the first time that other benzoxazinoids, rather than just the decomposition products BOA or MBOA, have been reported in beer. The results also show that benzoxazinoids can be present in beer glycosylated with three or four hexose units.

  16. UPLC/Q-TOFMS-Based Metabolomics Studies on the Protective Effect of Panax notoginseng Saponins on Alcoholic Liver Injury.

    PubMed

    Liu, Fang; Bai, Xu; Ding, Ren-Bo; Hu, Yuan-Jia; Su, Huanxing; Wan, Jian-Bo

    2015-01-01

    Consistent, excessive alcohol consumption leads to liver injury. The aim of the present study is to evaluate the possible efficacy of Panax notoginseng saponins (PNS) against chronic alcohol-induced liver injury using LC-MS-based urinary metabolomics. Mice were fed a Lieber-DeCarli liquid diet containing alcohol or isocaloric maltose dextrin as a control diet with or without PNS (200 mg/kg/BW) for 4 weeks. Treatment with PNS significantly reduced the increases in plasma ALT and AST levels, hepatic levels of reactive oxygen species (ROS) and malondialdehyde (MDA), which induced by chronic alcohol exposure. Conversely, PNS was also found to restore the glutathione (GSH) depletion and increase the superoxide dismutase (SOD) activities. The end-point urine sample of each mouse was collected overnight (24 h) in metabolic cages and their metabolic profiling changes were analyzed using UPLC/Q-TOFMS followed by multivariate statistical analysis. After 4 week of Lieber-DeCarli alcohol diet feeding, the metabolic profile experienced great perturbation in PCA score plot, and the treatment of PNS could assist to regulate the disturbed metabolic profile induced by alcohol exposure. Additionally, sixteen potential biomarkers responsible for derivations of the metabolic profile induced by alcohol exposure were identified, and the alcohol-induced changes in these biomarkers, except hexanoylglycine, could be partially or nearly reversed by PNS treatment. Taken together, PNS protects against chronic alcohol-induced liver injury. Our findings demonstrated that the LC-MS-based metabolomics approach is a useful tool to investigate the efficacy of Chinese medicines. PMID:26133752

  17. UPLC/Q-TOF MS-Based Metabolomics and qRT-PCR in Enzyme Gene Screening with Key Role in Triterpenoid Saponin Biosynthesis of Polygala tenuifolia

    PubMed Central

    Li, Zhenyu; Xu, Xiaoshuang; Peng, Bing; Qin, Xuemei; Du, Guanhua

    2014-01-01

    Background The dried root of Polygala tenuifolia, named Radix Polygalae, is a well-known traditional Chinese medicine. Triterpenoid saponins are some of the most important components of Radix Polygalae extracts and are widely studied because of their valuable pharmacological properties. However, the relationship between gene expression and triterpenoid saponin biosynthesis in P. tenuifolia is unclear. Methodology/Findings In this study, ultra-performance liquid chromatography (UPLC) coupled with quadrupole time-of-flight mass spectrometry (Q-TOF MS)-based metabolomic analysis was performed to identify and quantify the different chemical constituents of the roots, stems, leaves, and seeds of P. tenuifolia. A total of 22 marker compounds (VIP>1) were explored, and significant differences in all 7 triterpenoid saponins among the different tissues were found. We also observed an efficient reference gene GAPDH for different tissues in this plant and determined the expression level of some genes in the triterpenoid saponin biosynthetic pathway. Results showed that MVA pathway has more important functions in the triterpenoid saponin biosynthesis of P. tenuifolia. The expression levels of squalene synthase (SQS), squalene monooxygenase (SQE), and beta-amyrin synthase (β-AS) were highly correlated with the peak area intensity of triterpenoid saponins compared with data from UPLC/Q-TOF MS-based metabolomic analysis. Conclusions/Significance This finding suggested that a combination of UPLC/Q-TOF MS-based metabolomics and gene expression analysis can effectively elucidate the mechanism of triterpenoid saponin biosynthesis and can provide useful information on gene discovery. These findings can serve as a reference for using the overexpression of genes encoding for SQS, SQE, and/or β-AS to increase the triterpenoid saponin production of P. tenuifolia. PMID:25148032

  18. Identification of a ligand for tumor necrosis factor receptor from Chinese herbs by combination of surface plasmon resonance biosensor and UPLC-MS.

    PubMed

    Cao, Yan; Li, Ying-Hua; Lv, Di-Ya; Chen, Xiao-Fei; Chen, Lang-Dong; Zhu, Zhen-Yu; Chai, Yi-Feng; Zhang, Jun-Ping

    2016-07-01

    Identification of bioactive compounds directly from complex herbal extracts is a key issue in the study of Chinese herbs. The present study describes the establishment and application of a sensitive, efficient, and convenient method based on surface plasmon resonance (SPR) biosensors for screening active ingredients targeting tumor necrosis factor receptor type 1 (TNF-R1) from Chinese herbs. Concentration-adjusted herbal extracts were subjected to SPR binding assay, and a remarkable response signal was observed in Rheum officinale extract. Then, the TNF-R1-bound ingredients were recovered, enriched, and analyzed by UPLC-QTOF/MS. As a result, physcion-8-O-β-D-monoglucoside (PMG) was identified as a bioactive compound, and the affinity constant of PMG to TNF-R1 was determined by SPR affinity analysis (K D  = 376 nM). Pharmacological assays revealed that PMG inhibited TNF-α-induced cytotoxicity and apoptosis in L929 cells via TNF-R1. Although PMG was a trace component in the chemical constituents of the R. officinale extract, it had considerable anti-inflammatory activities. It was found for the first time that PMG was a ligand for TNF receptor from herbal medicines. The proposed SPR-based screening method may prove to be an effective solution to analyzing bioactive components of Chinese herbs and other complex drug systems. Graphical abstract Scheme of the method based on SPR biosensor for screening and recovering active ingredients from complex herbal extracts and UPLC-MS for identifying them. Scheme of the method based on SPR biosensor for screening and recovering active ingredients from complex herbal extracts and UPLC-MS for identifying them.

  19. UFLC-MS/MS determination and pharmacokinetic studies of six Saikosaponins in rat plasma after oral administration of Bupleurum Dropping Pills.

    PubMed

    Guan, Xiufeng; Wang, Xiangyang; Yan, Kaijing; Chu, Yang; Li, Shuming; Li, Wei; Yan, Xueying; Ma, Xiaohui; Zhou, Shuiping; Sun, He; Liu, Changxiao

    2016-05-30

    A rapid and sensitive ultra fast liquid chromatography tandem mass spectrometry method (UFLC-MS/MS) was developed and validated for the simultaneous determination of six Saikosaponins (SSs) (SSa, SSb1, SSb2, SSd, SSc, SSf) of Bupleurum Dropping Pills (BDP) in rat plasma using chloramphenicol as the internal standard (IS). The SSs were separated using an ACQUITY UPLC(®) BEH C18 column (50 mm × 2.1mm, 1.7 μm) and detection of these compounds were done by using a Qtrap 5500 mass spectrometer coupled with negative electrospray ionization (ESI) source under the multiple reaction monitoring (MRM) mode. According to regulatory guidelines, the established method was fully validated and results were showed within acceptable limits. The lower limit of quantifications (LLOQs) of all analytes were 0.2 ng/mL. The validated method was successfully applied into a pharmacokinetic study of orally administered BDP in rats. PMID:26970984

  20. The use of ultra high-performance liquid chromatography for studying hydrolysis kinetics of CL-20 and related energetic compounds.

    PubMed

    Makarov, Alexey; Lobrutto, Rosario; Christodoulatos, Christos; Jerkovich, Anton

    2009-03-15

    Ultra high-performance liquid chromatography (UHPLC) utilizes columns packed with sub-2-mum stationary-phase particles and allows operation with pressures of up to 15,000 psi to yield increased resolution, speed, and sensitivity versus conventional HPLC. This promising new technology was used for the analysis of energetic compounds (RDX, HMX and CL-20) and a selective method was developed on an Acquity UPLC. A fast UHPLC method was applied to determine alkaline hydrolysis reaction kinetics of major energetic compounds. Activation energies of alkaline hydrolysis reaction for CL-20, RDX and HMX were comparable to those in literature, however they were determined in a shorter amount of time due to the speed of analysis of the chromatographic method. The use of liophilic salts (KPF(6)) as mobile-phase additives for the enhancement of separation selectivity of energetic compounds was demonstrated. PMID:18644671

  1. Use of HPLC/UPLC-spectrophotometry for detection of formazan in in vitro Reconstructed human Tissue (RhT)-based test methods employing the MTT-reduction assay to expand their applicability to strongly coloured test chemicals.

    PubMed

    Alépée, N; Barroso, J; De Smedt, A; De Wever, B; Hibatallah, J; Klaric, M; Mewes, K R; Millet, M; Pfannenbecker, U; Tailhardat, M; Templier, M; McNamee, P

    2015-06-01

    A number of in vitro test methods using Reconstructed human Tissues (RhT) are regulatory accepted for evaluation of skin corrosion/irritation. In such methods, test chemical corrosion/irritation potential is determined by measuring tissue viability using the photometric MTT-reduction assay. A known limitation of this assay is possible interference of strongly coloured test chemicals with measurement of formazan by absorbance (OD). To address this, Cosmetics Europe evaluated use of HPLC/UPLC-spectrophotometry as an alternative formazan measurement system. Using the approach recommended by the FDA guidance for validation of bio-analytical methods, three independent laboratories established and qualified their HPLC/UPLC-spectrophotometry systems to reproducibly measure formazan from tissue extracts. Up to 26 chemicals were then tested in RhT test systems for eye/skin irritation and skin corrosion. Results support that: (1) HPLC/UPLC-spectrophotometry formazan measurement is highly reproducible; (2) formazan measurement by HPLC/UPLC-spectrophotometry and OD gave almost identical tissue viabilities for test chemicals not exhibiting colour interference nor direct MTT reduction; (3) independent of the test system used, HPLC/UPLC-spectrophotometry can measure formazan for strongly coloured test chemicals when this is not possible by absorbance only. It is therefore recommended that HPLC/UPLC-spectrophotometry to measure formazan be included in the procedures of in vitro RhT-based test methods, irrespective of the test system used and the toxicity endpoint evaluated to extend the applicability of these test methods to strongly coloured chemicals. PMID:25701760

  2. Systems for column-based separations, methods of forming packed columns, and methods of purifying sample components

    DOEpatents

    Egorov, Oleg B.; O'Hara, Matthew J.; Grate, Jay W.; Chandler, Darrell P.; Brockman, Fred J.; Bruckner-Lea, Cynthia J.

    2000-01-01

    The invention encompasses systems for column-based separations, methods of packing and unpacking columns and methods of separating components of samples. In one aspect, the invention includes a method of packing and unpacking a column chamber, comprising: a) packing a matrix material within a column chamber to form a packed column; and b) after the packing, unpacking the matrix material from the column chamber without moving the column chamber. In another aspect, the invention includes a system for column-based separations, comprising: a) a fluid passageway, the fluid passageway comprising a column chamber and a flow path in fluid communication with the column chamber, the flow path being obstructed by a retaining material permeable to a carrier fluid and impermeable to a column matrix material suspended in the carrier fluid, the flow path extending through the column chamber and through the retaining material, the flow path being configured to form a packed column within the column chamber when a suspension of the fluid and the column matrix material is flowed along the flow path; and b) the fluid passageway extending through a valve intermediate the column chamber and the retaining material.

  3. Systems For Column-Based Separations, Methods Of Forming Packed Columns, And Methods Of Purifying Sample Components.

    DOEpatents

    Egorov, Oleg B.; O'Hara, Matthew J.; Grate, Jay W.; Chandler, Darrell P.; Brockman, Fred J.; Bruckner-Lea, Cynthia J.

    2004-08-24

    The invention encompasses systems for column-based separations, methods of packing and unpacking columns and methods of separating components of samples. In one aspect, the invention includes a method of packing and unpacking a column chamber, comprising: a) packing a matrix material within a column chamber to form a packed column; and b) after the packing, unpacking the matrix material from the column chamber without moving the column chamber. In another aspect, the invention includes a system for column-based separations, comprising: a) a fluid passageway, the fluid passageway comprising a column chamber and a flow path in fluid communication with the column chamber, the flow path being obstructed by a retaining material permeable to a carrier fluid and impermeable to a column matrix material suspended in the carrier fluid, the flow path extending through the column chamber and through the retaining material, the flow path being configured to form a packed column within the column chamber when a suspension of the fluid and the column matrix material is flowed along the flow path; and b) the fluid passageway extending through a valve intermediate the column chamber and the retaining material.

  4. Systems For Column-Based Separations, Methods Of Forming Packed Columns, And Methods Of Purifying Sample Components

    DOEpatents

    Egorov, Oleg B.; O'Hara, Matthew J.; Grate, Jay W.; Chandler, Darrell P.; Brockman, Fred J.; Bruckner-Lea, Cynthia J.

    2006-02-21

    The invention encompasses systems for column-based separations, methods of packing and unpacking columns and methods of separating components of samples. In one aspect, the invention includes a method of packing and unpacking a column chamber, comprising: a) packing a matrix material within a column chamber to form a packed column; and b) after the packing, unpacking the matrix material from the column chamber without moving the column chamber. In another aspect, the invention includes a system for column-based separations, comprising: a) a fluid passageway, the fluid passageway comprising a column chamber and a flow path in fluid communication with the column chamber, the flow path being obstructed by a retaining material permeable to a carrier fluid and impermeable to a column matrix material suspended in the carrier fluid, the flow path extending through the column chamber and through the retaining material, the flow path being configured to form a packed column within the column chamber when a suspension of the fluid and the column matrix material is flowed along the flow path; and b) the fluid passageway extending through a valve intermediate the column chamber and the retaining material.

  5. Density Gradient Columns for Chemical Displays.

    ERIC Educational Resources Information Center

    Guenther, William B.

    1986-01-01

    Procedures for preparing density gradient columns for chemical displays are presented. They include displays illustrating acid-base reactions, metal ion equilibria, and liquid density. The lifetime of these metastable displays is surprising, some lasting for months in display cabinets. (JN)

  6. Manual Microscale Column Chromatography Pressurization Apparatus

    NASA Astrophysics Data System (ADS)

    Baldwin, Bruce W.

    2003-10-01

    Pressurization of a Pasteur pipet for microscale chromatography is simplified by connecting a 20- or 30-mL syringe to the pipet using a length of Tygon tubing. This simple system allows the student to easily dry-pack a column using common chromatography packing materials. Results were uniformly good for introductory, organic, or upper-division research chemistry students.

  7. "Dry-column" chromatography of plant pigments

    NASA Technical Reports Server (NTRS)

    Woeller, F. H.; Lehwalt, M. F.; Oyama, V. I.

    1973-01-01

    Separation of plant pigments which can be accomplished on thin-layer silica plates with mixture of petroleum ether, halocarbon, acetone, and polar solvent can be readily translated into dry-column technique that yields reproducible chromatograms after elution in fashion of liquid chromatography with fluorimeter as detector. Best solvent system was found to be mixture of petroleum ether, dichloromethane, acetone, and ethyl acetate.

  8. On Row Rank Equal Column Rank

    ERIC Educational Resources Information Center

    Khalili, Parviz

    2009-01-01

    We will prove a well-known theorem in Linear Algebra, that is, for any "m x n" matrix the dimension of row space and column space are the same. The proof is based on the subject of "elementary matrices" and "reduced row-echelon" form of a matrix.

  9. Heat Integration in Batch Distillation Column

    NASA Astrophysics Data System (ADS)

    Maiti, Debadrita; Jana, Amiya K.; Samanta, Amar Nath

    2010-10-01

    A new heat integrated batch distillation column has been configured in this paper. Here the column and reboiler are connected in an annular arrangement and a compressor is positioned between them to maintain the pressure difference. The heat integration is between the rectifying batch column and one concentric reboiler. Ethanol-Water binary system is chosen as an example for the design and analysis of this heat integrated batch distillation column (HIBDiC). In this work, a sensitivity test for selecting the optimal value of the total number of trays and reboiler duty and a thermodynamic feasibility test for its design acceptability has been accomplished. The principal objective of this study is to investigate the influence of compression ratio (CR) on the energy consumption of distillation and to find out the optimal value of CR. Also a comparative analysis of HIBiDC on energy consumption in steady state as well as in dynamic state has been carried out on the basis of its conventional model. The proposed scheme is capable to save the energy up to 50.52% compared to its conventional one by selecting the CR of 1.4 as an optimal value.

  10. Improve distillation-column control design

    SciTech Connect

    Fruehauf, P.S.; Mahoney, D.P.

    1994-03-01

    Steady-state process models have long been used to assist the engineer in designing control strategies for distillation columns. Yet, a large number of industrial columns still operate in manual or with ineffectual controls. So, better control design techniques using steady-state models certainly are needed. In this article, the authors introduced an improved method that already has proven itself on 33 industrial columns. This article deals exclusively with the design of single-point composition controls. The vast majority of columns have one-sided composition specifications. With such specifications, a single-point composition control scheme can keep both top and bottom product compositions at or below limits for a wide range of disturbances. The predominance of one-sided specifications means that the main incentive for dual-point control schemes is achieving energy savings. In most cases, though, the energy savings are small and do not justify the added difficulty of implementing and maintaining dual-point control. Additionally, dual-point schemes often have significantly longer recoveries from upsets due to interactions between the control loops. The design procedure can be best thought of as a general approach rather than a single detailed procedure that covers all cases. The produce must be adapted to each problem because there are many different types of distillation and almost every industrial problem has some unique requirement.

  11. Contexts for Column Addition and Subtraction

    ERIC Educational Resources Information Center

    Lopez Fernandez, Jorge M.; Velazquez Estrella, Aileen

    2011-01-01

    In this article, the authors discuss their approach to column addition and subtraction algorithms. Adapting an original idea of Paul Cobb and Erna Yackel's from "A Contextual Investigation of Three-Digit Addition and Subtraction" related to packing and unpacking candy in a candy factory, the authors provided an analogous context by designing…

  12. Extendible column can be stowed on drum

    NASA Technical Reports Server (NTRS)

    Holtz, G. M.; Howard, E. A.

    1965-01-01

    Column formed from a series of segments held together by an internal spring or cable can be coiled on a drum or extended into a rigid structure. This storable coil is useful in boring for soil samples and supporting electrical and optical sensors.

  13. Inklings: Collected Columns on Leadership and Creativity.

    ERIC Educational Resources Information Center

    Campbell, David P.

    This book brings together 35 of David P. Campbell's essays originally published as a regular column in a quarterly publication called "Issues and Observations." The articles deal with topics ranging from leadership issues such as risk-taking, executive motivation, decision making, and corporate taboos, to more general concerns such as father-son…

  14. Synthesis and applications of monolithic HPLC columns

    NASA Astrophysics Data System (ADS)

    Liang, Chengdu

    Silica and carbon monolithic columns were synthesized and modified for liquid chromatography applications. Column configurations and cladding techniques were investigated in detail. Three novel approaches have been developed for the synthesis of bimodal porous rods. Out of these three methods, gel-casting was adopted for the synthesis of silica monoliths with ordered mesopores and uniform macropores; the use of colloidal templates and dual phase separation has been successfully implemented for the synthesis of carbon monoliths with well-controlled meso- and macro- porosities. The formation of mesopores in carbon materials has been further studied in the microphase separation of block copolymers. Electrochemical modification of carbon monoliths was discovered to be an efficient method for converting covalently bonded functionalities to carbon monoliths. N,N'-diethylaminobenzene has been attached to carbon surface for the separation of proteins and protein digests. The performances of carbon-based monolithic columns were studied intensely through frontal analysis and Van Deemter plot. Temperature and pressure effects were also investigated in carbon-based columns. The density of bonding on the modified carbon monoliths was characterized by thermogravimetric analysis.

  15. WATER COLUMN DATA AND SPECTRAL IRRADIANCE MODEL

    EPA Science Inventory

    Water samples collected monthly, for 18 months, from six sites in the Laguna Madre were analyzed to identify and quantify phytopigments using High Performance Liquid Chromatography (HPLC). In addition, water column pigment and nutrient data were acquired at 12 stations in Upper ...

  16. Column agglutination technology: the antiglobulin test.

    PubMed

    Reis, K J; Chachowski, R; Cupido, A; Davies, D; Jakway, J; Setcavage, T M

    1993-08-01

    A new system for typing and screening blood, based on the sieving effect of glass bead microparticles, has been developed. The test is performed in a microcolumn in which the red cell agglutinates are trapped in the glass bead matrix during centrifugation, and unagglutinated cells form a pellet at the bottom of the column. Anti-human globulin reagents were incorporated in the diluent and the new test system, column agglutination technology, was compared to conventional tube tests and low-ionic-strength method. Sera and plasmas (228 samples) were screened for red cell antibodies with two anti-human globulin reagents: one containing only anti-IgG and the other containing both anti-IgG and anti-C3b, -C3d. After initial testing, there was 94-percent agreement between column agglutination technology and tube tests, and after repeat testing, there was 97-percent agreement. The column agglutination technology anti-human globulin test eliminates the need to wash red cells, which decreases the overall test time. The test is easy to perform, and the results are more objective than those with tube and microplate methods.

  17. DNAPL transport through macroporous, clayey till columns

    SciTech Connect

    Joergensen, P.R. |; Broholm, K.; Sonnenborg, T.O.; Arvin, E.

    1998-07-01

    This paper provides the first experimental determination of the rates and distribution of transport of a dense, nonaqueous phase liquid (DNAPL) through a naturally bioporous and fractured clayey till deposit. Until now, assessment of DNAPL behavior in this type of deposit has relied on theoretical studies. Predictions of DNAPL transport have proven to be uncertain as a result of difficulties in measuring critical parameters such as DNAPL entry pressure and flow behavior in response to natural fracture/biopore apertures and the degree of interconnection of these structures. In the present investigation, the migration of free product trichloroethylene (TCE) was studied by means of two undisturbed clayey till columns under in situ effective soil stress conditions. The experiments revealed that transport of TCE was restricted to biopores in one column and fractures in another column, bypassing the low-permeability clayey matrix. Effective porosities of the columns, i.e., biopores and fractures, were two to three orders of magnitude lower than total porosities, i.e., macropores and matrix. Single phase water flow rates through the columns at water-saturated conditions followed a linear relationship with hydraulic gradient. TCE flow could not be predicted from the single-phase calculations because of nonlinearity observed between applied TCE injection heads and resulting TCE flow. TCE flow rates were 24 and 10.3 m/day at TCE gradients of 1.18 and 0.91, respectively. The observed flow rates indicate that in cases where vertical biopores or fractures fully penetrate clayey till aquitards, a low-viscosity DNAPL may quickly enter underlying aquifers. The experiments further indicate that 100 liters of a low-viscosity DNAPL are sufficient to contaminate approximately 25 to 100 m{sup 3} of till material because of the small effective porosity constituted by the biopores and fractures.

  18. UPLC-MS-ELSD-PDA as a powerful dereplication tool to facilitate compound identification from small molecule natural product libraries

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Generation of natural product libraries containing column fractions, each with only a few small molecules, by a high throughput, automated fractionation system has made it possible to implement an improved dereplication strategy for selection and prioritization of hits in a natural product discovery...

  19. ON THE ORIGIN OF THE HIGH COLUMN DENSITY TURNOVER IN THE H I COLUMN DENSITY DISTRIBUTION

    SciTech Connect

    Erkal, Denis; Gnedin, Nickolay Y.; Kravtsov, Andrey V.

    2012-12-10

    We study the high column density regime of the H I column density distribution function and argue that there are two distinct features: a turnover at N{sub H{sub I}} Almost-Equal-To 10{sup 21} cm{sup -2}, which is present at both z = 0 and z Almost-Equal-To 3, and a lack of systems above N{sub H{sub I}} Almost-Equal-To 10{sup 22} cm{sup -2} at z = 0. Using observations of the column density distribution, we argue that the H I-H{sub 2} transition does not cause the turnover at N{sub H{sub I}} Almost-Equal-To 10{sup 21} cm{sup -2} but can plausibly explain the turnover at N{sub H{sub I}} {approx}> 10{sup 22} cm{sup -2}. We compute the H I column density distribution of individual galaxies in the THINGS sample and show that the turnover column density depends only weakly on metallicity. Furthermore, we show that the column density distribution of galaxies, corrected for inclination, is insensitive to the resolution of the H I map or to averaging in radial shells. Our results indicate that the similarity of H I column density distributions at z = 3 and 0 is due to the similarity of the maximum H I surface densities of high-z and low-z disks, set presumably by universal processes that shape properties of the gaseous disks of galaxies. Using fully cosmological simulations, we explore other candidate physical mechanisms that could produce a turnover in the column density distribution. We show that while turbulence within giant molecular clouds cannot affect the damped Ly{alpha} column density distribution, stellar feedback can affect it significantly if the feedback is sufficiently effective in removing gas from the central 2-3 kpc of high-redshift galaxies. Finally, we argue that it is meaningful to compare column densities averaged over {approx} kpc scales with those estimated from quasar spectra that probe sub-pc scales due to the steep power spectrum of H I column density fluctuations observed in nearby galaxies.

  20. High-Throughput UPLC-MS Method for the Determination of N-Acetyl-l-Cysteine: Application in Tissue Distribution Study in Wistar Rats.

    PubMed

    Siddiqui, Masoom Raza; Wabaidur, Saikh Mohammad; Ola, Mohammad Shamsul; AlOthman, Zeid A; Rafiquee, Mohammad Zulfiqar Ali; Khan, Moonis Ali

    2016-08-01

    N-Acetylcysteine (NAC) is the N-acetyl derivative of the amino acid l-cysteine and is extensively used as a medicine to treat a variety of diseases. High-throughput ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS) method has been developed for the quantitative assessment of N-acetyl-l-cysteine. The method was further applied to study the distribution of the intraperitoneal injected drug into different tissues and plasma of Wistar rats, including liver, kidney, heart, lungs and spleen. The drug was having highest concentration in plasma and liver followed by kidney, lungs, heart and spleen. Method validation studies suggested being linear in the range of 1-15 µg mL(-1) for liver, kidney, heart, lungs and spleen and 1-120 µg mL(-1) for the plasma. The limit of detection and limit of quantitation were found to be 0.20 and 0.66 µg mL(-1), respectively. The recovery studies suggested that in all the cases, the obtained recovery was in the range of 98.51-101.88%. Our analyses provide a validated UPLC-MS method for the determination of NAC and its successful application for the analysis in plasma and tissues obtained from Wistar rats. PMID:27102930

  1. Screening of lignan patterns in Schisandra species using ultrasonic assisted temperature switch ionic liquid microextraction followed by UPLC-MS/MS analysis.

    PubMed

    Dong, Wei; Yu, Shuijing; Deng, Yangwu; Pan, Tao

    2016-01-01

    The ultrasonic assisted temperature-switch ionic liquid microextraction (UATS-ILME) has been successfully applied in extracting of seven lignans from Schisandra. 1-Butyl-3-methylimidazolium tetrafluoroborate ([C4MIM][BF4]) aqueous solution was selected for extracting the target analytes in raw material at 80°C. The lignans were deposited into a single drop by in situ forming 1-butyl-3-methylimidazolium hexafluorophosphate ([C4MIM][PF6]) by cooling down to 0°C and centrifuging for 10min. The extracts were analyzed by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) in a robust multiple-reaction monitoring (MRM) mode in five minutes. Meanwhile, the proposed method was validated and successfully applied to the determination of seven lignans in twelve Schisandra species. The results indicated that UATS-ILME combined with UPLC-MS/MS is a powerful and practical tool, which has great potential for comprehensive quality control of herbal medicines. PMID:26625336

  2. Metabolomic Approach for Discrimination of Four- and Six-Year-Old Red Ginseng (Panax ginseng) Using UPLC-QToF-MS.

    PubMed

    Shin, Jung-Sub; Park, Hee-Won; In, Gyo; Seo, Hyun Kyu; Won, Tae Hyung; Jang, Kyoung Hwa; Cho, Byung-Goo; Han, Chang Kyun; Shin, Jongheon

    2016-09-01

    Panax ginseng C.A. MEYER is one of the most popular medicinal herbs in Asia and the chemical constituents are changed by processing methods such as steaming or sun drying. Metabolomic analysis was performed to distinguish age discrimination of four- and six-year-old red ginseng using ultra-performance liquid chromatography quadruple time of flight mass spectrometry (UPLC-QToF-MS) with multivariate statistical analysis. Principal component analysis (PCA) showed clear discrimination between extracts of red ginseng of different ages and suggest totally six discrimination markers (two for four-year-old and four for six-year-old red ginseng). Among these, one marker was isolated and the structure determined by NMR spectroscopic analysis was 13-cis-docosenamide (marker 6-1) from six-year-old red ginseng. This is the first report of a metabolomic study regarding the age differentiation of red ginseng using UPLC-QToF-MS and determination of the structure of the marker. These results will contribute to the quality control and standardization as well as provide a scientific basis for pharmacological research on red ginseng.

  3. Analysis of 2-(2-Phenylethyl)chromones by UPLC-ESI-QTOF-MS and Multivariate Statistical Methods in Wild and Cultivated Agarwood.

    PubMed

    Li, Yuanbin; Sheng, Nan; Wang, Lingli; Li, Shijie; Chen, Jiannan; Lai, Xiaoping

    2016-01-01

    Agarwood is the fragrant resinous material mainly formed from species of Aquilaria. 2-(2-phenylethyl)chromones, especially the highly oxidized 5,6,7,8-tetrahydro-2-(2-phenylethyl)chromones, are the main representative compounds from agarwood. It is important to determine whether agarwood in trade is from cultivated trees or natural trees in the Convention on the International Trade in Endangered Species (CITES). We characterized the 2-(2-phenylethyl)chromones in agarwood by ultra-performance liquid chromatography coupled with electrospray ionization mass spectrometry (UPLC-ESI-QTOF-MS) and differentiated wild from cultivated agarwood by metabolomic analysis. A total of 141 chromones including 50 potentially new compounds were evaluated as belonging to four structural classes (unoxidized 2-(2-phenylethyl)chromones, 5,6,7,8-tetrahydro-2-(2-phenylethyl)-chromones, bi-2-(2-phenylethyl)chromones, and tri-2-(2-phenylethyl)chromones). The metabolic difference between wild and cultivated agarwood was analyzed by component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA). Fourteen markers of metabolisms in wild and cultivated agarwood were constructed (e.g., 6,7-dimethoxy-2-(2-phenylethyl)chromone, 6,8-dihydroxy-2-(2-phenylethyl)chromone, 6-methoxy-2-(2-phenylethyl)chromone, etc.). These results indicated that UPLC-ESI-QTOF-MS-based metabonomics analysis in agarwood may be useful for distinguishing wild agarwood from cultivated agarwood. PMID:27223280

  4. Chemical differentiation of Da-Cheng-Qi-Tang, a Chinese medicine formula, prepared by traditional and modern decoction methods using UPLC/Q-TOFMS-based metabolomics approach.

    PubMed

    Wan, Jian-Bo; Bai, Xu; Cai, Xiu-Jiang; Rao, Yi; Wang, Yue-Sheng; Wang, Yi-Tao

    2013-09-01

    In order to evaluate chemical consistency between traditional and modern decoctions of Da-Cheng-Qi-Tang (DCQT), a classical Chinese medicine formula commonly used in the treatment of digestive diseases, an ultra performance liquid chromatography-electrospray ionization-quadrupole time-of-flight mass spectrometry (UPLC-ESI-Q-TOFMS) combined with multivariate statistical analysis was established to globally characterize the chemical profile and discover differentiating chemical markers. Two kinds of decoctions, namely traditional decoction (multi-step decoction of constituent herbs), and modern decoction (one-step decoction of all herbs), were prepared and subjected to UPLC-MS analysis, the datasets of tR-m/z pairs, ion intensities and sample codes were processed with supervised orthogonal partial least squared discriminant analysis (OPLS-DA) to comprehensively compare the chemical difference between these two kinds of decoction samples. The global chemical difference was found between traditional and modern decoctions, and rhein, sennoside A/B, diosmetin, magnoloside B and naringin were the components contributing most to these differences. Based on the fact that traditional decoction of DCQT presents the higher concentration of rhein and sennoside A/B, mainly contributed to laxative activity of DCQT, the purgative effect of traditional decoction might be more potent, compared with modern decoction. However, the comparative study on purgative effect of traditional and modern DCQT remains to be further investigated using pharmacological approaches. Our findings also provide the early scientific evidence of traditional decoction method of DCQT.

  5. Association between Oxidative DNA Damage and Risk of Colorectal Cancer: Sensitive Determination of Urinary 8-Hydroxy-2′-deoxyguanosine by UPLC-MS/MS Analysis

    PubMed Central

    Guo, Cheng; Li, Xiaofen; Wang, Rong; Yu, Jiekai; Ye, Minfeng; Mao, Lingna; Zhang, Suzhan; Zheng, Shu

    2016-01-01

    Oxidative DNA damage plays crucial roles in the pathogenesis of numerous diseases including cancer. 8-hydroxy-2′-deoxyguanosine (8-OHdG) is the most representative product of oxidative modifications of DNA, and urinary 8-OHdG is potentially the best non-invasive biomarker of oxidative damage to DNA. Herein, we developed a sensitive, specific and accurate method for quantification of 8-OHdG in human urine. The urine samples were pretreated using off-line solid-phase extraction (SPE), followed by ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) analysis. By the use of acetic acid as an additive to the mobile phase, we improved the UPLC-MS/MS detection of 8-OHdG by 2.7−5.3 times. Using the developed strategy, we measured the contents of 8-OHdG in urine samples from 142 healthy volunteers and 84 patients with colorectal cancer (CRC). We observed increased levels of urinary 8-OHdG in patients with CRC and patients with tumor metastasis, compared to healthy controls and patients without tumor metastasis, respectively. Additionally, logistic regression analysis and receiver operator characteristic (ROC) curve analysis were performed. Our findings implicate that oxidative stress plays important roles in the development of CRC and the marked increase of urinary 8-OHdG may serve as a potential liquid biomarker for the risk estimation, early warning and detection of CRC. PMID:27585556

  6. Association between Oxidative DNA Damage and Risk of Colorectal Cancer: Sensitive Determination of Urinary 8-Hydroxy-2‧-deoxyguanosine by UPLC-MS/MS Analysis

    NASA Astrophysics Data System (ADS)

    Guo, Cheng; Li, Xiaofen; Wang, Rong; Yu, Jiekai; Ye, Minfeng; Mao, Lingna; Zhang, Suzhan; Zheng, Shu

    2016-09-01

    Oxidative DNA damage plays crucial roles in the pathogenesis of numerous diseases including cancer. 8-hydroxy-2‧-deoxyguanosine (8-OHdG) is the most representative product of oxidative modifications of DNA, and urinary 8-OHdG is potentially the best non-invasive biomarker of oxidative damage to DNA. Herein, we developed a sensitive, specific and accurate method for quantification of 8-OHdG in human urine. The urine samples were pretreated using off-line solid-phase extraction (SPE), followed by ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) analysis. By the use of acetic acid as an additive to the mobile phase, we improved the UPLC-MS/MS detection of 8-OHdG by 2.7‑5.3 times. Using the developed strategy, we measured the contents of 8-OHdG in urine samples from 142 healthy volunteers and 84 patients with colorectal cancer (CRC). We observed increased levels of urinary 8-OHdG in patients with CRC and patients with tumor metastasis, compared to healthy controls and patients without tumor metastasis, respectively. Additionally, logistic regression analysis and receiver operator characteristic (ROC) curve analysis were performed. Our findings implicate that oxidative stress plays important roles in the development of CRC and the marked increase of urinary 8-OHdG may serve as a potential liquid biomarker for the risk estimation, early warning and detection of CRC.

  7. UPLC-PDA-QTOFMS-guided isolation of prenylated xanthones and benzoylphloroglucinols from the leaves of Garcinia oblongifolia and their migration-inhibitory activity

    PubMed Central

    Zhang, Hong; Dan, Zheng; Ding, Zhi-Jie; Lao, Yuan-Zhi; Tan, Hong-Sheng; Xu, Hong-Xi

    2016-01-01

    A UPLC-PDA-QTOFMS-guided isolation strategy was employed to screen and track potentially new compounds from Garcinia oblongifolia. As a result, two new prenylated xanthones, oblongixanthones D and E (1–2), six new prenylated benzoylphloroglucinol derivatives, oblongifolins V–Z (3–7) and oblongifolin AA (8), as well as a known compound oblongifolin L (9), were isolated from the EtOAc-soluble fraction of an acetone extract of the leaves of Garcinia oblongifolia guided by UPLC-PDA-QTOFMS analysis. The structures of the new compounds were elucidated by 1D- and 2D-NMR spectroscopic analysis and mass spectrometry. Experimental and calculated ECD spectra were used to determine the absolute configurations. The results of wound healing and transwell migration assay showed that oblongixanthones D (1), E (2), and oblongifolin L (9) have the ability to inhibit cancer cell migration in lower cytotoxic concentrations. Western blotting results showed that these compounds exhibited an anti-metastasis effect mainly through downregulating RAF protein levels. In addition, 2 and 9 could inhibit phospho-MEK and phospho-ERK at downstream. Moreover, 1, 2, and 9 could inhibit snail protein level, suggesting that they could regulate the EMT pathway. PMID:27767059

  8. Chemical fingerprinting and quantitative constituent analysis of Siwu decoction categorized formulae by UPLC-QTOF/MS/MS and HPLC-DAD

    PubMed Central

    2013-01-01

    Background Siwu decoction categorized formulae (SWDCF) are widely used for treating gynecological diseases. This study aims to elucidate the differences of bioactive constituents in SWDCF by ultra-high performance liquid chromatography coupled with time-of-flight mass spectrometry (UPLC - QTOF - MS /MS) and HPLC-DAD. Methods An efficient method based on UPLC - QTOF - MS /MS was developed for identifying the chemical profiles of SWDCF. HPLC-DAD method was used for quantifying seven chemical markers in SWDCF. Results Eighty four components were identified or characterized, including ten organic acids, thirty glycosides (monoterpene or iridoid or phenylpropanoids glycosides), fourteen lactones, eighteen flavonoids, and eleven alkaloids in the complex system. The datasets of tR-m/z pairs, ion intensities and sample codes were processed with supervised orthogonal partial least squared discriminant analysis to compare these decoction samples. After a clear classification was established, OPLS-DA was performed and 16 common components with relative quantity in SWDCF samples were determined. Gallic acid, protocatechuic acid, vanillic acid, caffeic acid, paeoniflorin, ferulic acid, and senkyunolide I were selected as the chemical markers to identify SWDCF by HPLC-DAD. Conclusion The chemical profiles with 84 components in SWDCF, including monoterpene glycosides, acetophenones, galloyl glucoses, even some isomers in the complex system were characterized by UPLC–QTOF–MS/MS. PMID:23453004

  9. Association between Oxidative DNA Damage and Risk of Colorectal Cancer: Sensitive Determination of Urinary 8-Hydroxy-2'-deoxyguanosine by UPLC-MS/MS Analysis.

    PubMed

    Guo, Cheng; Li, Xiaofen; Wang, Rong; Yu, Jiekai; Ye, Minfeng; Mao, Lingna; Zhang, Suzhan; Zheng, Shu

    2016-01-01

    Oxidative DNA damage plays crucial roles in the pathogenesis of numerous diseases including cancer. 8-hydroxy-2'-deoxyguanosine (8-OHdG) is the most representative product of oxidative modifications of DNA, and urinary 8-OHdG is potentially the best non-invasive biomarker of oxidative damage to DNA. Herein, we developed a sensitive, specific and accurate method for quantification of 8-OHdG in human urine. The urine samples were pretreated using off-line solid-phase extraction (SPE), followed by ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) analysis. By the use of acetic acid as an additive to the mobile phase, we improved the UPLC-MS/MS detection of 8-OHdG by 2.7-5.3 times. Using the developed strategy, we measured the contents of 8-OHdG in urine samples from 142 healthy volunteers and 84 patients with colorectal cancer (CRC). We observed increased levels of urinary 8-OHdG in patients with CRC and patients with tumor metastasis, compared to healthy controls and patients without tumor metastasis, respectively. Additionally, logistic regression analysis and receiver operator characteristic (ROC) curve analysis were performed. Our findings implicate that oxidative stress plays important roles in the development of CRC and the marked increase of urinary 8-OHdG may serve as a potential liquid biomarker for the risk estimation, early warning and detection of CRC. PMID:27585556

  10. Qualitative and Quantitative Analysis of the Major Constituents in Chinese Medical Preparation Lianhua-Qingwen Capsule by UPLC-DAD-QTOF-MS

    PubMed Central

    Jia, Weina; Wang, Chunhua; Wang, Yuefei; Pan, Guixiang; Jiang, Miaomiao; Li, Zheng; Zhu, Yan

    2015-01-01

    Lianhua-Qingwen capsule (LQC) is a commonly used Chinese medical preparation to treat viral influenza and especially played a very important role in the fight against severe acute respiratory syndrome (SARS) in 2002-2003 in China. In this paper, a rapid ultraperformance liquid chromatography coupled with diode-array detector and quadrupole time-of-flight mass spectrometry (UPLC-DAD-QTOF-MS) method was established for qualitative and quantitative analysis of the major constituents of LQC. A total of 61 compounds including flavonoids, phenylpropanoids, anthraquinones, triterpenoids, iridoids, and other types of compounds were unambiguously or tentatively identified by comparing the retention times and accurate mass measurement with reference compounds or literature data. Among them, twelve representative compounds were further quantified as chemical markers in quantitative analysis, including salidroside, chlorogenic acid, forsythoside E, cryptochlorogenic acid, amygdalin, sweroside, hyperin, rutin, forsythoside A, phillyrin, rhein, and glycyrrhizic acid. The UPLC-DAD method was evaluated with linearity, limit of detection (LOD), limit of quantification (LOQ), precision, stability, repeatability, and recovery tests. The results showed that the developed quantitative method was linear, sensitive, and precise for the quality control of LQC. PMID:25654135

  11. Screening of lignan patterns in Schisandra species using ultrasonic assisted temperature switch ionic liquid microextraction followed by UPLC-MS/MS analysis.

    PubMed

    Dong, Wei; Yu, Shuijing; Deng, Yangwu; Pan, Tao

    2016-01-01

    The ultrasonic assisted temperature-switch ionic liquid microextraction (UATS-ILME) has been successfully applied in extracting of seven lignans from Schisandra. 1-Butyl-3-methylimidazolium tetrafluoroborate ([C4MIM][BF4]) aqueous solution was selected for extracting the target analytes in raw material at 80°C. The lignans were deposited into a single drop by in situ forming 1-butyl-3-methylimidazolium hexafluorophosphate ([C4MIM][PF6]) by cooling down to 0°C and centrifuging for 10min. The extracts were analyzed by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) in a robust multiple-reaction monitoring (MRM) mode in five minutes. Meanwhile, the proposed method was validated and successfully applied to the determination of seven lignans in twelve Schisandra species. The results indicated that UATS-ILME combined with UPLC-MS/MS is a powerful and practical tool, which has great potential for comprehensive quality control of herbal medicines.

  12. Do column frits contribute to the on-column, flow-induced degradation of macromolecules?

    PubMed

    Striegel, André M

    2014-09-12

    Flow-induced, on-column degradation is a major hindrance to the accurate characterization of ultra-high molar mass macromolecules and colloids. This degradation is a direct result of the large shear rates which are generated within the column, which cause chain scission to occur both in the interstitial medium and, it has been postulated, at the packing particle pore boundary. An additional putative source of degradation has been the column frits, though little experimental evidence exists to either support or refute this claim. To this effect, the present experiments examine the role of the frits in the degradation of high molar mass macromolecules. Two narrow dispersity polystyrene standards, the molar mass of which differs by a factor of two, were analyzed on three different size-exclusion chromatography (SEC) columns, each with frits of different pore size, at various flow rates. In the smallest pore size column, which also contained the smallest frits and which was packed with the smallest diameter particles, the larger standard was forced to degrade by increasing the flow rate of the mobile phase. During the course of the latter portion of the study, the inlet and the outlet frits were removed from the column, in stepwise fashion. It was concluded that neither frit played any appreciable role in the degradation. Results of our studies were applied to explain previously observed degradation in ultra-high pressure liquid chromatography of polymers. The general conclusion arrived at herein is that the column frits are likely to have a secondary role (as compared to interstitial and pore boundary stresses), or no role at all, in polymer degradation for cases where the frit radius is larger than or equal to the hydraulic radius rcof the column.

  13. How to select equivalent and complimentary reversed phase liquid chromatography columns from column characterization databases.

    PubMed

    Borges, Endler M

    2014-01-01

    Three RP-LC column characterization protocols [Tanaka et al. (1989), Snyder et al. (PQRI, 2002), and NIST SRM 870 (2000)] were evaluated using both Euclidian distance and Principal Components Analysis to evaluate effectiveness at identifying equivalent columns. These databases utilize specific chromatographic properties such as hydrophobicity, hydrogen bonding, shape/steric selectivity, and ion exchange capacity of stationary phases. The chromatographic parameters of each test were shown to be uncorrelated. Despite this, the three protocols were equally successful in identifying similar and/or dissimilar stationary phases. The veracity of the results has been supported by some real life pharmaceutical separations. The use of Principal Component Analysis to identify similar/dissimilar phases appears to have some limitations in terms of loss of information. In contrast, the use of Euclidian distances is a much more convenient and reliable approach. The use of auto scaled data is favoured over the use of weighted factors as the former data transformation is less affected by the addition or removal of columns from the database. The use of these free databases and their corresponding software tools shown to be valid for identifying similar columns with equivalent chromatographic selectivity and retention as a "backup column". In addition, dissimilar columns with complimentary chromatographic selectivity can be identified for method development screening strategies.

  14. Development and Validation of a UPLC-MS/MS Method to Monitor Cephapirin Excretion in Dairy Cows following Intramammary Infusion

    PubMed Central

    Ray, Partha; Knowlton, Katharine F.; Shang, Chao; Xia, Kang

    2014-01-01

    Cephapirin, a cephalosporin antibiotic, is used by the majority of dairy farms in the US. Fecal and urinary excretion of cephapirin could introduce this compound into the environment when manure is land applied as fertilizer, and may cause development of bacterial resistance to antibiotics critical for human health. The environmental loading of cephapirin by the livestock industry remains un-assessed, largely due to a lack of appropriate analytical methods. Therefore, this study aimed to develop and validate a cephapirin quantification method to capture the temporal pattern of cephapirin excretion in dairy cows following intramammary infusion. The method includes an extraction with phosphate buffer and methanol, solid-phase extraction (SPE) clean-up, and quantification using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The LOQ values of the developed method were 4.02 µg kg−1 and 0.96 µg L−1 for feces and urine, respectively. This robust method recovered >60% and >80% cephapirin from spiked blank fecal and urine samples, respectively, with acceptable intra- and inter-day variation (<10%). Using this method, we detected trace amounts (µg kg−1) of cephapirin in dairy cow feces, and cephapirin in urine was detected at very high concentrations (133 to 480 µg L−1). Cephapirin was primarily excreted via urine and its urinary excretion was influenced by day (P = 0.03). Peak excretion (2.69 mg) was on day 1 following intramammary infusion and decreased sharply thereafter (0.19, 0.19, 0.08, and 0.17 mg on day 2, 3, 4, and 5, respectively) reflecting a quadratic pattern of excretion (Quadratic: P = 0.03). The described method for quantification of cephapirin in bovine feces and urine is sensitive, accurate, and robust and allowed to monitor the pattern of cephapirin excretion in dairy cows. This data will help develop manure segregation and treatment methods to minimize the risk of antibiotic loading to the environment

  15. Modeling of Crystalline Silicotitanate Ion Exchange Columns

    SciTech Connect

    Walker, D.D.

    1999-03-09

    Non-elutable ion exchange is being considered as a potential replacement for the In-Tank Precipitation process for removing cesium from Savannah River Site (SRS) radioactive waste. Crystalline silicotitanate (CST) particles are the reference ion exchange medium for the process. A major factor in the construction cost of this process is the size of the ion exchange column required to meet product specifications for decontaminated waste. To validate SRS column sizing calculations, SRS subcontracted two reknowned experts in this field to perform similar calculations: Professor R. G. Anthony, Department of Chemical Engineering, Texas A&038;M University, and Professor S. W. Wang, Department of Chemical Engineering, Purdue University. The appendices of this document contain reports from the two subcontractors. Definition of the design problem came through several meetings and conference calls between the participants and SRS personnel over the past few months. This document summarizes the problem definition and results from the two reports.

  16. Employing anatomical knowledge in vertebral column labeling

    NASA Astrophysics Data System (ADS)

    Yao, Jianhua; Summers, Ronald M.

    2009-02-01

    The spinal column constitutes the central axis of human torso and is often used by radiologists to reference the location of organs in the chest and abdomen. However, visually identifying and labeling vertebrae is not trivial and can be timeconsuming. This paper presents an approach to automatically label vertebrae based on two pieces of anatomical knowledge: one vertebra has at most two attached ribs, and ribs are attached only to thoracic vertebrae. The spinal column is first extracted by a hybrid method using the watershed algorithm, directed acyclic graph search and a four-part vertebra model. Then curved reformations in sagittal and coronal directions are computed and aggregated intensity profiles along the spinal cord are analyzed to partition the spinal column into vertebrae. After that, candidates for rib bones are detected using features such as location, orientation, shape, size and density. Then a correspondence matrix is established to match ribs and vertebrae. The last vertebra (from thoracic to lumbar) with attached ribs is identified and labeled as T12. The rest of vertebrae are labeled accordingly. The method was tested on 50 CT scans and successfully labeled 48 of them. The two failed cases were mainly due to rudimentary ribs.

  17. Analysis of finishing reactive distillation columns

    SciTech Connect

    Espinosa, J.; Aguirre, P.; Frey, T.; Stichlmair, J.

    1999-01-01

    In this paper, a novel method to deal with the design and the synthesis of finishing reactive distillation columns with one reactive core, two rectifying sections, and one stripping section is presented. The attention of the work is concentrated on three subjects: (1) the feasibility of a given separation at both finite and total reflux operation; (2) the minimum energy demand operation; (3) the distribution of the reaction between the reactor and the finishing reactive column. The design problem presents the same grade of difficulty as that found in the design of conventional extractive columns. A geometric based method is used to explain key features of reactive distillation. Here, the relation between the reaction yield and the distillate flow rate plays a role similar to that of the entrainer flow in extractive distillation. Hence, special attention is given to the behavior of the profiles inside the rectifying section below the reactive core. The methodology is illustrated using the well-known MTBE case study.

  18. Whose Cortical Column Would that Be?

    PubMed Central

    da Costa, Nuno Maçarico; Martin, Kevan A. C.

    2010-01-01

    The cortical column has been an invaluable concept to explain the functional organization of the neocortex. While this idea was born out of experiments that cleverly combined electrophysiological recordings with anatomy, no one has ‘seen’ the anatomy of a column. All we know is that when we record through the cortex of primates, ungulates, and carnivores in a trajectory perpendicular to its surface there is a remarkable constancy in the receptive field properties of the neurons regarding one set of stimulus features. There is no obvious morphological analog for this functional architecture, in fact much of the anatomical data seems to challenge it. Here we describe historically the origins of the concept of the cortical column and the struggles of the pioneers to define the columnar architecture. We suggest that in the concept of a ‘canonical circuit’ we may find the means to reconcile the structure of neocortex with its functional architecture. The canonical microcircuit respects the known connectivity of the neocortex, and it is flexible enough to change transiently the architecture of its network in order to perform the required computations. PMID:20640245

  19. Dynamics of a Tapped Granular Column

    NASA Astrophysics Data System (ADS)

    Rosato, Anthony; Blackmore, Denis; Zuo, Luo; Hao, Wu; Horntrop, David

    2015-11-01

    We consider the behavior of a column of spheres subjected to a time-dependent vertical taps. Of interest are various dynamical properties, such as the motion of its mass center, its response to taps of different intensities and forms, and the effect of system size and material properties. The interplay between diverse time and length scales are the key contributors to the column's evolving dynamics. Soft sphere discrete element simulations were conducted over a very wide parameter space to obtain a portrait of column behavior as embodied by the collective dynamics of the mass center motion. Results compared favorably with a derived reduced-order paradigm of the mass center motion (surprisingly analogous to that for a single bouncing ball on an oscillating plate) with respect to dynamical regimes and their transitions. A continuum model obtained from a system of Newtonian equations, as a locally averaged limit in the transport mode along trajectories is described, and a numerical solution protocol for a one-dimensional system is outlined. Typical trajectories and density evolution profiles are shown. We conclude with a discussion of our investigations to relate predictions of the continuum and reduced dynamical systems models with discrete simulations.

  20. Ultra-performance liquid chromatography tandem mass-spectrometry (uplc-ms/ms) for the rapid, simultaneous analysis of thiamin, riboflavin, flavin adenine dinucleotide, nicotinamide and pyridoxal in human milk

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A novel, rapid and sensitive Ultra Performance Liquid-Chromatography tandem Mass-Spectrometry (UPLC-MS/MS) method for the simultaneous determination of several B-vitamins in human milk was developed. Resolution by retention time or multiple reaction monitoring (MRM) for thiamin, riboflavin, flavin a...

  1. Development and validation of stability-indicating assay method by UPLC for a fixed dose combination of atorvastatin and ezetimibe.

    PubMed

    Goel, Amit; Baboota, Sanjula; Sahni, Jasjeet K; Srinivas, Kona S; Gupta, Ravi S; Gupta, Abhishek; Semwal, Vinod P; Ali, Javed

    2013-03-01

    A stability-indicating ultra-performance liquid chromatography method was developed and validated for the simultaneous determination of a fixed dose combination of atorvastatin and ezetimibe in bulk drugs. The developed method was successfully applied to the simultaneous quantitative analysis of the combination drugs in tablet. The chromatographic separation was performed on a Kromasil Eternity C18 UHPLC column (2.5 µm, 2.1 × 50 mm) using a gradient elution of acetonitrile and ammonium acetate buffer (pH 6.70; 0.01M) as the mobile phase at a flow rate of 0.2 mL/min with column oven temperature of 40°C. Ultraviolet detection was performed at 245 nm. Total run time was 5 min, within which the primary compounds and their degradation products were separated. The method was validated for accuracy, repeatability, reproducibility and robustness. Linearity, limit of detection and limit of quantitation were established for atorvastatin and ezetimibe.

  2. [Scale-up of conical column with 10 degree opening angle as preparative liquid chromatographic column].

    PubMed

    Lu, Liejuan; Chen, Jie; Guan, Yafeng

    2009-05-01

    A preparative scale liquid chromatographic column with the conical shape of 10 degrees opening angle was constructed and evaluated. The column was designed with the inlet/outlet diameters of 54/27 mm, the column length of 150 mm and the column volume of 200 mL, and packed with the spherical C18 bonded silica with the particle size of 40-75 microm and the aperture of 11 nm. The mobile phase in the conical column showed a plug like flow profile and plug like chromatographic band shape. For naphthalene, the reduced plate height was about 2.11; the maximum sample load was 2.1 mg or 1.7 mL (10% reduction of plate number), which is 20%, 16% and 19% higher than that of cylindrical one of the same length and volume. As the injection mass increased from 2. 4 mg up to 12 mg, the resolution of ethyl paraben/butyl (R, ) reduced from 2. 14 down to 1.71, and the butyl paraben/naphthalene (Rs3) from 2.91 down to 2.52; the injection volume increased from 3 mL up to 19 mL, Rs2, reduced from 2.23 down to 1.28, and Rs3 from 2.95 down to 2.30, while the peaks were still in symmetric shape without tailing. This characteristic of the column shall benefit for the separation of trace components from matrix. This demonstrated the conical shaped preparative columns would have a broad practical applicability for obtaining pure compounds. PMID:19803133

  3. 18. VIEW SOUTH OF TIMBER COLUMNS ON FIRST FLOOR OF ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    18. VIEW SOUTH OF TIMBER COLUMNS ON FIRST FLOOR OF BUILDING 21 SHOWING TYPICAL MILL CONSTRUCTION; COLUMNS REST ON CAST IRON BASE PLATES - Scovill Brass Works, 59 Mill Street, Waterbury, New Haven County, CT

  4. 6. HISTORIC AMERICAN BUILDINGS SURVEY, INTERIOR SHOWING ORIGINAL GRANITE COLUMNS ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    6. HISTORIC AMERICAN BUILDINGS SURVEY, INTERIOR SHOWING ORIGINAL GRANITE COLUMNS AND COLUMN BRICKFACED AFTER THE GREAT FIRE 1904 - Old U.S. Appraisers Stores, Gay & Lombard Streets, Baltimore, Independent City, MD

  5. Detail of roof trusses showing phoenix columns. Note structural phoenix ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    Detail of roof trusses showing phoenix columns. Note structural phoenix column in foreground. - Phoenix Iron Company, Rolling Mill, North of French Creek, west of Fairview Avenue, Phoenixville, Chester County, PA

  6. CAR MACHINE SHOP, FIRST FLOOR, DETAIL OF WOOD COLUMN AND ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    CAR MACHINE SHOP, FIRST FLOOR, DETAIL OF WOOD COLUMN AND INVERTED KING-POST TRUSS TO PROVIDE INCREASED SPAN BETWEEN COLUMNS, LOOKING SOUTH. - Southern Pacific, Sacramento Shops, Car Machine Shop, 111 I Street, Sacramento, Sacramento County, CA

  7. A Convenient Method for Comparison of Efficiency of Fractionating Columns.

    ERIC Educational Resources Information Center

    Higgins, Robert H.

    1990-01-01

    Presented is a method for demonstrating the use of various fractionating columns to resolve mixtures into individual components and to correlate the resolving powers of column packings to their "hold-up" volumes. Fractions were analyzed using refractive indices. (KR)

  8. Method to fabricate silicon chromatographic column comprising fluid ports

    DOEpatents

    Manginell, Ronald P.; Frye-Mason, Gregory C.; Heller, Edwin J.; Adkins, Douglas R.

    2004-03-02

    A new method for fabricating a silicon chromatographic column comprising through-substrate fluid ports has been developed. This new method enables the fabrication of multi-layer interconnected stacks of silicon chromatographic columns.

  9. 3. Detail of beam splice and column capital on the ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    3. Detail of beam splice and column capital on the second floor of the Cloth Room Building/Old Bleach House, Monadnock Mills. Beam and column edges are chamfered. - Monadnock Mills, 15 Water Street, Claremont, Sullivan County, NH

  10. 14. Detail view of columns, capitals and beams at south ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    14. Detail view of columns, capitals and beams at south end of north section of mill. Note the transition from deep pocket to shallow pocket column capitals. - Lowe Mill, Eighth Avenue, Southwest, Huntsville, Madison County, AL

  11. 20. Detail of 8" square solid wood column at fruit ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    20. Detail of 8" square solid wood column at fruit and vegetable storage room; note ledger plates bolted to top of column - Fort Hood, World War II Temporary Buildings, Cold Storage Building, Seventeenth Street, Killeen, Bell County, TX

  12. 19. Detail of builtup 5" x 13" column at fruit ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    19. Detail of built-up 5" x 13" column at fruit and vegetable storage room; note ledger plates bolted to top of column - Fort Hood, World War II Temporary Buildings, Cold Storage Building, Seventeenth Street, Killeen, Bell County, TX

  13. Cross flow cyclonic flotation column for coal and minerals beneficiation

    DOEpatents

    Lai, Ralph W.; Patton, Robert A.

    2000-01-01

    An apparatus and process for the separation of coal from pyritic impurities using a modified froth flotation system. The froth flotation column incorporates a helical track about the inner wall of the column in a region intermediate between the top and base of the column. A standard impeller located about the central axis of the column is used to generate a centrifugal force thereby increasing the separation efficiency of coal from the pyritic particles and hydrophillic tailings.

  14. 46 CFR 174.085 - Flooding on column stabilized units.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... 46 Shipping 7 2012-10-01 2012-10-01 false Flooding on column stabilized units. 174.085 Section 174... Units § 174.085 Flooding on column stabilized units. (a) Watertight compartments that are outboard of... of the unit, must be assumed to be subject to flooding as follows: (1) When a column is...

  15. 46 CFR 174.085 - Flooding on column stabilized units.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... 46 Shipping 7 2014-10-01 2014-10-01 false Flooding on column stabilized units. 174.085 Section 174... Units § 174.085 Flooding on column stabilized units. (a) Watertight compartments that are outboard of... of the unit, must be assumed to be subject to flooding as follows: (1) When a column is...

  16. 46 CFR 174.085 - Flooding on column stabilized units.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... 46 Shipping 7 2011-10-01 2011-10-01 false Flooding on column stabilized units. 174.085 Section 174... Units § 174.085 Flooding on column stabilized units. (a) Watertight compartments that are outboard of... of the unit, must be assumed to be subject to flooding as follows: (1) When a column is...

  17. Three-way analysis of the UPLC-PDA dataset for the multicomponent quantitation of hydrochlorothiazide and olmesartan medoxomil in tablets by parallel factor analysis and three-way partial least squares.

    PubMed

    Dinç, Erdal; Ertekin, Zehra Ceren

    2016-01-01

    An application of parallel factor analysis (PARAFAC) and three-way partial least squares (3W-PLS1) regression models to ultra-performance liquid chromatography-photodiode array detection (UPLC-PDA) data with co-eluted peaks in the same wavelength and time regions was described for the multicomponent quantitation of hydrochlorothiazide (HCT) and olmesartan medoxomil (OLM) in tablets. Three-way dataset of HCT and OLM in their binary mixtures containing telmisartan (IS) as an internal standard was recorded with a UPLC-PDA instrument. Firstly, the PARAFAC algorithm was applied for the decomposition of three-way UPLC-PDA data into the chromatographic, spectral and concentration profiles to quantify the concerned compounds. Secondly, 3W-PLS1 approach was subjected to the decomposition of a tensor consisting of three-way UPLC-PDA data into a set of triads to build 3W-PLS1 regression for the analysis of the same compounds in samples. For the proposed three-way analysis methods in the regression and prediction steps, the applicability and validity of PARAFAC and 3W-PLS1 models were checked by analyzing the synthetic mixture samples, inter-day and intra-day samples, and standard addition samples containing HCT and OLM. Two different three-way analysis methods, PARAFAC and 3W-PLS1, were successfully applied to the quantitative estimation of the solid dosage form containing HCT and OLM. Regression and prediction results provided from three-way analysis were compared with those obtained by traditional UPLC method.

  18. [Simultaneous determination of 24 industrial dyes in grain and meat products by ultra performance liquid chromatography-tandem mass spectrometry].

    PubMed

    Feng, Yuechao; Jia, Li; He, Yahui; Wang, Jianfeng; Liu, Yan; Fan, Xiaojing

    2013-10-01

    An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/ MS) analytical method was established for the simultaneous determination of 24 forbidden industrial dyes in grain and meat products. The sample was extracted with methanol and acetonitrile, and cleaned-up by a WAX solid phase extraction column. The solution was separated on an ACQUITY UPLC BEH C18 column eluted with a mixture of 10 mmol/L ammonium acetate-0.2% formic acid aqueous solution and methanol-acetonitrile (7:3, v/v) as the mobile phases, and then analyzed in multiple reaction monitoring (MRM) mode. The correlation coefficients were above 0.99, the average recoveries were 61%-116%, and the relative standard deviations (RSD, n = 6) were lower than 13%. The quantification limits were 0.1-4.0 microg/kg. This method is simple, effective, sensitive, and suitable for the determination and confirmation of the 24 forbidden industrial dyes in grain and meat products.

  19. Targeted toxicological screening for acidic, neutral and basic substances in postmortem and antemortem whole blood using simple protein precipitation and UPLC-HR-TOF-MS.

    PubMed

    Telving, Rasmus; Hasselstrøm, Jørgen Bo; Andreasen, Mette Findal

    2016-09-01

    A broad targeted screening method based on broadband collision-induced dissociation (bbCID) ultra-performance liquid chromatography high-resolution time-of-flight mass spectrometry (UPLC-HR-TOF-MS) was developed and evaluated for toxicological screening of whole blood samples. The acidic, neutral and basic substances covered by the method were identified in postmortem and antemortem whole blood samples from forensic autopsy cases, clinical forensic cases and driving under the influence of drugs (DUID) cases by a reverse target database search. The screening method covered 467 substances. Validation was performed on spiked whole blood samples and authentic postmortem and antemortem whole blood samples. For most of the basic drugs, the established cut-off limits were very low, ranging from 0.25ng/g to 50ng/g. The established cut-off limits for most neutral and acidic drugs, were in the range from 50ng/g to 500ng/g. Sample preparation was performed using simple protein precipitation of 300μL of whole blood with acetonitrile and methanol. Ten microliters of the reconstituted extract were injected and separated within a 13.5min UPLC gradient reverse-phase run. Positive electrospray ionization (ESI) was used to generate the ions in the m/z range of 50-1000. Fragment ions were generated by bbCID. Identification was based on retention time, accurate mass, fragment ion(s) and isotopic pattern. A very sensitive broad toxicological screening method using positive electrospray ionization UPLC-HR-TOF-MS was achieved in one injection. This method covered basic substances, substances traditionally analyzed in negative ESI (e.g., salicylic acid), small highly polar substances such as beta- and gamma-hydroxybutyric acid (BHB and GHB, respectively) and highly non-polar substances such as amiodarone. The new method was shown to combine high sensitivity with a very broad scope that has not previously been reported in toxicological whole blood screening when using only one injection

  20. Development and validation of an UPLC-MS/MS method for the quantification of tamoxifen and its main metabolites in human scalp hair.

    PubMed

    Drooger, Jan C; Jager, Agnes; Lam, Mei-Ho; den Boer, Mathilda D; Sleijfer, Stefan; Mathijssen, Ron H J; de Bruijn, Peter

    2015-10-10

    The aim of this study was to validate an earlier developed high-performance highly sensitive ultra performance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS) method for quantification of tamoxifen and its three main metabolites (N-desmethyl-tamoxifen, 4-hydroxy-tamoxifen and 4-hydroxy-N-desmethyl-tamoxifen) in scalp hair. This non-invasive method might, by segmental analysis of hair, be useful in the determination of the concentration of drugs and its metabolites over time, which can be used to study a wide variety of clinical relevant questions. Hair samples (150-300 hair strands, cut as close to the scalp as possible from the posterior vertex region of the head) were collected from female patients taking tamoxifen 20mg daily (n=19). The analytes were extracted using a liquid-liquid extraction procedure with carbonate buffer at pH 8.8 and a mixture of n-hexane/isopropranol method, followed by UPLC-MS/MS chromatography, based on an earlier validated method. The calibration curves were linear in the range of 1.00-200 pmol for tamoxifen and N-desmethyl-tamoxifen, with lower limit of quantitation of 1.00 pmol and 0.100-20.0 pmol with lower limit of quantitation of 0.100 pmol for endoxifen and 4-hydroxy-tamoxifen. Assay performance was fair with a within-run and between-run variability less than 9.24 at the three quality control samples and less than 15.7 for the lower limit of quantitation. Importantly, a steep linear decline was observed from distal to proximal hair segments. Probably, this is due to UV exposure as we showed degradation of tamoxifen and its metabolites after exposure to UV-light. Furthermore, higher concentrations of tamoxifen were found in black hair samples compared to blond and brown hair samples. We conclude that measurement of the concentration of tamoxifen and its main metabolites in hair is possible, with the selective, sensitive, accurate and precise UPLC-MS/MS method. However, for tamoxifen, it seems not possible to determine

  1. Column density profiles of multiphase gaseous haloes

    NASA Astrophysics Data System (ADS)

    Liang, Cameron J.; Kravtsov, Andrey V.; Agertz, Oscar

    2016-05-01

    We analyse circumgalactic medium (CGM) in a suite of high-resolution cosmological re-simulations of a Milky Way size galaxy and show that CGM properties are quite sensitive to details of star formation-feedback loop modelling. The simulation that produces a realistic late-type galaxy, fails to reproduce existing observations of the CGM. In contrast, simulation that does not produce a realistic galaxy has the predicted CGM in better agreement with observations. This illustrates that properties of galaxies and properties of their CGM provide strong complementary constraints on the processes governing galaxy formation. Our simulations predict that column density profiles of ions are well described by an exponential function of projected distance d: N ∝ e^{-d/h_s}. Simulations thus indicate that the sharp drop in absorber detections at larger distances in observations does not correspond to a `boundary' of an ion, but reflects the underlying steep exponential column density profile. Furthermore, we find that ionization energy of ions is tightly correlated with the scaleheight hs: h_s ∝ E_ion^{0.74}. At z ≈ 0, warm gas traced by low-ionization species (e.g. Mg II and C IV) has hs ≈ 0.03 - 0.07Rvir, while higher ionization species (O VI and Ne VIII) have hs ≈ 0.32 - 0.45Rvir. Finally, the scaleheights of ions in our simulations evolve slower than the virial radius for z ≤ 2, but similarly to the halo scale radius, rs. Thus, we suggest that the column density profiles of galaxies at different redshifts should be scaled by rs rather than the halo virial radius.

  2. OH vertical column abundance - Tropical measurements

    NASA Astrophysics Data System (ADS)

    Burnett, Clyde R.; Minschwaner, Kenneth R.; Burnett, Elizabeth B.

    1990-09-01

    Measurements of the vertical column abundance of atmospheric hydroxyl (OH) have been made during the period 1987-1989 at the National Weather Service (NWS) station at Moen, Truk, Federated States of Micronesia (7 deg N, 152 deg E). A total of 384 independent data sets was obtained. Tropical OH abundance levels average about 22 percent above corresponding mid-latitude values, with OH levels during late winter and early spring up to 50 percent above those observed at 40 deg N. Stratospheric wind and temperature data obtained from the daily NWS radiosonde data are examined for correlations with the OH results.

  3. OH vertical column abundance - Tropical measurements

    NASA Technical Reports Server (NTRS)

    Burnett, Clyde R.; Minschwaner, Kenneth R.; Burnett, Elizabeth B.

    1990-01-01

    Measurements of the vertical column abundance of atmospheric hydroxyl (OH) have been made during the period 1987-1989 at the National Weather Service (NWS) station at Moen, Truk, Federated States of Micronesia (7 deg N, 152 deg E). A total of 384 independent data sets was obtained. Tropical OH abundance levels average about 22 percent above corresponding mid-latitude values, with OH levels during late winter and early spring up to 50 percent above those observed at 40 deg N. Stratospheric wind and temperature data obtained from the daily NWS radiosonde data are examined for correlations with the OH results.

  4. Wiring dendrites in layers and columns.

    PubMed

    Luo, Jiangnan; McQueen, Philip G; Shi, Bo; Lee, Chi-Hon; Ting, Chun-Yuan

    2016-06-01

    The most striking structure in the nervous system is the complex yet stereotyped morphology of the neuronal dendritic tree. Dendritic morphologies and the connections they make govern information flow and integration in the brain. The fundamental mechanisms that regulate dendritic outgrowth and branching are subjects of extensive study. In this review, we summarize recent advances in the molecular and cellular mechanisms for routing dendrites in layers and columns, prevalent organizational structures in the brain. We highlight how dendritic patterning influences the formation of synaptic circuits. PMID:27315108

  5. Growing Cobalt Silicide Columns In Silicon

    NASA Technical Reports Server (NTRS)

    Fathauer, Obert W.

    1991-01-01

    Codeposition by molecular-beam epitaxy yields variety of structures. Proposed fabrication process produces three-dimensional nanometer-sized structures on silicon wafers. Enables control of dimensions of metal and semiconductor epitaxial layers in three dimensions instead of usual single dimension (perpendicular to the plane of the substrate). Process used to make arrays of highly efficient infrared sensors, high-speed transistors, and quantum wires. For fabrication of electronic devices, both shapes and locations of columns controlled. One possible technique for doing this electron-beam lithography, see "Making Submicron CoSi2 Structures on Silicon Substrates" (NPO-17736).

  6. Research on Configurations of Thermally Integrated Distillation Column(TIDC)

    NASA Astrophysics Data System (ADS)

    Sun, Lanyi; Li, Jun; Liu, Xuenuan; Li, Qingsong

    Taking a C3 distillation column as the base case, possible configurations for Thermally Integrated Distillation Columns (TIDC) are proposed and compared to a conventional column and a column with a vapor recompression system (VRC). Thermal efficiency of the TIDC appears to be strongly sensitive to column configuration and a highly efficient asymmetrical configuration with stripping section stages thermally interconnected with the same number of stages in the upper part of the rectifying section emerges as the most promising option. The relationships among pressure ratio of rectifying section to stripping section and energy consumption were also discussed.

  7. 9. Detail view of columns on first floor. This row ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    9. Detail view of columns on first floor. This row of columns indicates the former location of the exterior mill wall before World War II era expansion. The unusual column and beam connection was a key part of the mill structural system patented by Providence, Rhode Island engineers Charles Praray and Charles Makepeace in 1894. Each column was originally located in the apex of triangular window bay, but not connected to the exterior wall. Modifications on the right side of each column support the beams of the addition. - Dixie Cotton Mill, 710 Greenville Street, La Grange, Troup County, GA

  8. Performance of single particle fritted capillary columns in electrochromatography.

    PubMed

    Zhang, Bo; Liu, Qing; Yang, Lijun; Wang, Qiuquan

    2013-01-11

    Development of capillary electrochromatography (CEC) largely depends on column technology. The past ten years or so have seen a great number of CEC works performed on monolithic columns, due to simplicity and robustness in column fabrication. Monolithic columns eliminate the issue of column fritting, which conventionally made particle-packed capillary columns fragile and introduced nonuniformity to the chromatographic bed. The particulate packing material, however, is still a popular type of stationary phase widely used in CEC, as the rich library of HPLC packing material provides a wide range of choices for chromatographic separations performed in electrodriven mode. In this study, we investigated a purely physical fritting method, single particle fritting technology, to immobilize particulate chromatographic material inside capillary tube in a sinter-free manner to produce robust capillary columns. Single particle fritted columns present significantly improved column-to-column reproducibility (n=10) in peak efficiency, retention factor, peak area and asymmetry (%RSD=5.4, 7.7, 6.2 and 6.1, respectively, at 26 kV), enabling their practical application in high throughput parallel analysis using multiple columns.

  9. Lindane biodegradation in groundwater using semi-continuous soil columns

    SciTech Connect

    LaPat-Polasko, L.T.; Lazarr, N.C.; Reker, M.A.

    1995-12-31

    To evaluate the potential for bioremediation of various isomers of benzene hexachloride (BHC) including lindane (gamma BHC)-contaminated groundwater, a bench-scale study was conducted using site groundwater and soil collected from a chemical manufacturing facility located in southwest Missouri. Three soil columns were prepared to evaluate various conditions under which contaminant biodegredation is known to occur: Column 1 (the hydrogen peroxide and nutrient column) received site groundwater, hydrogen peroxide (an oxygen source to promote aerobic conditions) and ammonium polyphosphate (nutrients); Column 2 received site groundwater, nutrients and sodium sulfite (a reductant to promote anaerobic conditions); and Column 3 received the same amendments as Column 1 but under sterile conditions. Column 3 was used to evaluate abiotic losses of contaminants. The indigenous soil and/or groundwater microbial population removed more than 99 percent of the BHC isomers present in the hydrogen peroxide and nutrient column influent in 24 hours. Abiotic losses of contaminants were less than 20 percent after initial column exchanges based on the results of sterile column data. Anaerobic conditions were not as conducive to contaminant degradation. During the 24-hour exchange periods, less than 80 percent BHC removal was observed in the groundwater effluents from the anaerobic column.

  10. Tentative identification, quantitation, and principal component analysis of green pu-erh, green, and white teas using UPLC/DAD/MS

    PubMed Central

    Zhao, Yang; Chen, Pei; Lin, Longze; Harnly, J.M.; Yu, Liangli (Lucy); Li, Zhangwan

    2013-01-01

    Tea (Camellia sinensis L.), an important drink and a natural medicine for thousands of years, contains many health beneficial compounds. Growing season, geographical region, and fermentation methods create many variations in tea compositions, which contribute to each tea's uniqueness. In this study, a simple, rapid, and efficient ultra-performance liquid chromatography (UPLC) method combined with diode array detector (DAD) and mass spectroscopic (MS) detection and chemometrics analysis was used to analyse three different types of teas (green pu-erh, green tea, white tea). Using the developed method, 68 compounds were identified and 54 were quantified based on retention times, UV spectra, and MS spectra by referencing to available standards and data in the literatures. The results showed the chemical differences between the tested teas. Principal component analysis (PCA) was applied to classify and distinguish between tea samples. PMID:25544798

  11. Identification and quantitation of cocaine, benzoylecgonine, and cocaethylene in blood, serum, and plasma using ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS).

    PubMed

    Kriger, Scott; Gunn, Josh; Terrell, Andrea R

    2010-01-01

    Cocaine is a widely abused stimulant. Numerous methods exist for the identification of the drug, or more commonly, one of its metabolites in urine. Urine testing is useful for most cases, but it is necessary to use other matrices in forensic situations and when subjects are anuric. We describe a novel method for the analysis of cocaine, benzoylecgonine, and cocaethylene in blood, serum, and plasma utilizing ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). Sample preparation has been minimized to a simple deproteinization step in which each specimen is mixed with an acetonitrile-internal standard mixture. The method has excellent precision across the linear range of 25-2,000 ng/mL for each analyte. With a run-time of 4 min, this method provides a significant improvement over traditional GC/MS methods. PMID:20077068

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

    PubMed

    Górnaś, Paweł; Mišina, Inga; Grāvīte, Ilze; Soliven, Arianne; Kaufmane, Edīte; Segliņa, Dalija

    2015-01-01

    Composition of tocochromanols in kernels recovered from 16 different apricot varieties (Prunus armeniaca L.) was studied. Three tocopherol (T) homologues, namely α, γ and δ, were quantified in all tested samples by an RP-HPLC/FLD method. The γ-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 α and γ 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 (α-T), 42.48-73.27 (γ-T) and 0.77-2.09 (δ-T). Moreover, the ratio between individual tocopherol homologues α:γ:δ was nearly constant in all varieties and amounted to approximately 2:39:1.

  13. A Platelet/CMC coupled with offline UPLC-QTOF-MS/MS for screening antiplatelet activity components from aqueous extract of Danshen.

    PubMed

    Chen, Ying; Zhang, Na; Ma, Jian; Zhu, Yan; Wang, Meng; Wang, Xiaoming; Zhang, Peng

    2016-01-01

    Platelets play crucial roles in thromboembolic and cardiovascular disease. The main platelets membrane receptors include adenosine diphosphate receptors, thrombin receptors, thromboxane prostanoid receptors and collagen receptors. In this study, a Platelet/CMC coupled with offline UPLC-QTOF-MS/MS system was built to screen antiplatelet activity components from aqueous extract of Danshen, which serve as an agent of antiplatelet aggregation in Traditional Chinese Medicine. Rosmarinic acid, lithospermic acid, salvianolic acid B, two isomers of salvianolic acid B, salvianolic acid C, salvianolic acid D and salvianolic acid H/I were identified as the potential antiplatelet activity components. Moreover, rosmarinic acid, lithospermic acid, salvianolic acid B, salvianolic acid C and danshensu were tested in platelet aggregation in vitro assay. The results suggested their retention time was closely related to the antiplatelet aggregation activities. This study provides a rapid, effective and novel method for screening the potential antiplatelet activity components from Chinese herb medicines.

  14. Rapid profiling of phenolic compounds of green and fermented Bergenia crassifolia L. leaves by UPLC-DAD-QqQ-MS and HPLC-DAD-ESI-QTOF-MS.

    PubMed

    Salminen, Juha-Pekka; Shikov, Alexander N; Karonen, Maarit; Pozharitskaya, Olga N; Kim, Jorma; Makarov, Valery G; Hiltunen, Raimo; Galambosi, Bertalan

    2014-01-01

    Bergenia crassifolia L., Saxifragaceae, is an evergreen perennial plant known in traditional medicine of Russia, Mongolia and China. Polyphenols are responsible for the number of pharmacological effects of Bergenia. UPLC-DAD-QqQ-MS and LC-DAD-ESI-QTOF-MS were used for the rapid profiling of phenolic compounds, mainly hydrolysable tannins. Green leaves consisted of 55% ellagitannins, 29% gallic acid derivatives and 11% flavonoids, with the remaining gallic acid, arbutin, bergenin and caffeoyl quinic acid. In fermented leaves, 31% of gallic acid was found, followed with 28% ellagitannins, 18% gallic acid derivatives and 18% flavonoids, with the remaining caffeoyl quinic acid, bergenin and arbutin. Tellimagrandin I, pedunculagin, caffeoyl quinic acid, monogalloyl quinic acid, 1-O-galloylglucose and 1,2,6-tri-O-galloylglucose were identified for the very first time.

  15. Synthesis of Isotopically Labeled (13)C3-Simazine and Development of a Simultaneous UPLC-MS/MS Method for the Analysis of Simazine in Soil.

    PubMed

    Song, Yan; Guo, Yangzhen; Zhang, Xia; Yang, Yue; Chen, Shuo; She, Gaimei; She, Dongmei

    2016-01-14

    The isotope dilution mass spectrometry (IDMS) is a highly efficient method for tackling the ion suppression in complex matrix by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), but a lack of commercial internal standards is a limiting factor for these analyses. Herein, an economical and efficient strategy for the synthesis of (13)C3-simazine via a three-step procedure was developed. The isotope-labeled internal standard was used for determination of simazine residue in soil samples. The quantitation method has a limit of detection of 0.015 μg/kg and quantitation of 0.08 μg/kg. The inter-day and intra-day precision of the method were below 4.6%. Recovery values were ranged between 92.9% and 99.2%. All the samples obtained from six provinces in China contained from 1 to 62 μg/kg of simazine.

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

    PubMed

    Górnaś, Paweł; Mišina, Inga; Grāvīte, Ilze; Soliven, Arianne; Kaufmane, Edīte; Segliņa, Dalija

    2015-01-01

    Composition of tocochromanols in kernels recovered from 16 different apricot varieties (Prunus armeniaca L.) was studied. Three tocopherol (T) homologues, namely α, γ and δ, were quantified in all tested samples by an RP-HPLC/FLD method. The γ-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 α and γ 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 (α-T), 42.48-73.27 (γ-T) and 0.77-2.09 (δ-T). Moreover, the ratio between individual tocopherol homologues α:γ:δ was nearly constant in all varieties and amounted to approximately 2:39:1. PMID:25567675

  17. Quantitative analysis of unconjugated and total bisphenol A in human urine using solid-phase extraction and UPLC-MS/MS: method implementation, method qualification and troubleshooting.

    PubMed

    Buscher, Brigitte; van de Lagemaat, Dick; Gries, Wolfgang; Beyer, Dieter; Markham, Dan A; Budinsky, Robert A; Dimond, Stephen S; Nath, Rajesh V; Snyder, Stephanie A; Hentges, Steven G

    2015-11-15

    The aim of the presented investigation was to document challenges encountered during implementation and qualification of a method for bisphenol A (BPA) analysis and to develop and discuss precautions taken to avoid and to monitor contamination with BPA during sample handling and analysis. Previously developed and published HPLC-MS/MS methods for the determination of unconjugated BPA (Markham et al. Journal of Analytical Toxicology, 34 (2010) 293-303) [17] and total BPA (Markham et al. Journal of Analytical Toxicology, 38 (2014) 194-203) [20] in human urine were combined and transferred into another laboratory. The initial method for unconjugated BPA was developed and evaluated in two independent laboratories simultaneously. The second method for total BPA was developed and evaluated in one of these laboratories to conserve resources. Accurate analysis of BPA at sub-ppb levels is a challenging task as BPA is a widely used material and is ubiquitous in the environment at trace concentrations. Propensity for contamination of biological samples with BPA is reported in the literature during sample collection, storage, and/or analysis. Contamination by trace levels of BPA is so pervasive that even with extraordinary care, it is difficult to completely exclude the introduction of BPA into biological samples and, consequently, contamination might have an impact on BPA biomonitoring data. The applied UPLC-MS/MS method was calibrated from 0.05 to 25ng/ml. The limit of quantification was 0.1ng/ml for unconjugated BPA and 0.2ng/ml for total BPA, respectively, in human urine. Finally, the method was applied to urine samples derived from 20 volunteers. Overall, BPA can be analyzed in human urine with acceptable recovery and repeatability if sufficient measures are taken to avoid contamination throughout the procedure from sample collection until UPLC-MS/MS analysis. PMID:26465088

  18. Evidence of non-extractable florfenicol residues: development and validation of a confirmatory method for total florfenicol content in kidney by UPLC-MS/MS.

    PubMed

    Faulkner, Dermot; Cantley, Margaret; Walker, Matthew; Crooks, Steven; Kennedy, David; Elliott, Christopher

    2016-06-01

    The parent compound florfenicol (FF) is a broad-spectrum antibacterial compound licensed in the UK for use in cattle, pigs and the aquaculture industry. The analysis of porcine tissues in this study demonstrates that significant amounts of solvent non-extractable FF-related residues are present in incurred tissues (kidney and muscle) from treated animals. The results indicate that methods based on solvent extraction alone may carry a significant risk of reporting false-negative results. The use of a strong acid hydrolysis step prior to solvent extraction of tissue samples is necessary for an accurate estimate of the total tissue FF content. A robust and sensitive method for the determination of total FF residue content in kidney samples by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed and validated. This method covers the synthetic amphenicol drug FF and its metabolites, measured as the marker residue florfenicol amine (FFA) as per Commission Regulation (EU) No. 37/2010. Non-extractable and intermediate metabolites are converted to the hydrolysis product FFA, and then partitioned into ethyl acetate. Extracts are solvent exchanged prior to a dispersive solid-phase extraction step, then analysed using an alkaline reverse-phase gradient separation by UPLC-MS/MS. The method was validated around the maximum residue levels (MRLs) set out in Regulation (EU) No. 37/2010 for bovine kidney in accordance with Commission Decision No. 2002/657/EC. The following method performance characteristics were assessed during a single laboratory validation study: selectivity, specificity, sensitivity, linearity, matrix effects, accuracy and precision (decision limit (CCα) and detection capability (CCβ) were determined). PMID:27053017

  19. Anti-acetylcholinesterase potential and metabolome classification of 4 Ocimum species as determined via UPLC/qTOF/MS and chemometric tools.

    PubMed

    Farag, M A; Ezzat, S M; Salama, M M; Tadros, M G

    2016-06-01

    Ocimum (sweet basil) is a plant of considerable commercial importance in traditional medicine worldwide as well as for the flavor and food industry. The goal of this study was to examine Ocimum extracts anti-acetylcholinesterase activity and to correlate the activity with their secondary metabolites profiles via a metabolome based ultraperformance liquid chromatography-mass spectrometry (UPLC-MS) approach coupled to chemometrics. The metabolomic differences in phenolics from leaves derived from 4 Ocimum species: Ocimum basilicum, Ocimum africanum, Ocimum americanum and Ocimum minimum were assessed. Under optimized conditions, 81 metabolites were identified including 21 hydroxy cinnamic acids, 4 benzoic acid conjugates, 14C/O flavonoid conjugates, 2 alcohols, 5 acyl sugars, 4 triterpenes and 12 fatty acids. Several salviolanic acid derivatives including salviolanic acid A, B, C & I found in Salvia, were found in Ocimum herein for the first time. Unsupervised principal component analysis (PCA) and supervised orthogonal projection to latent structures-discriminant analysis (OPLS-DA) were further used for comparing and classification of samples. A clear separation among the four investigated Ocimum species was revealed, with O. africanum samples found most enriched in hydroxy cinnamates conjugates (HC) and flavonoids. To the best of our knowledge, this is the first report for compositional differences among Ocimum leaves via a metabolomic approach revealing that among examined species O. africanum leaves present a better source of Ocimum bioactive metabolites. The anticholinesrase activity of examined species was further assessed with a potent IC50 values for O. americanum, O. africanum, O. basilicum ranging from 2.5 to 6.6mg/ml, whereas O. minimum was least active with IC50 of 31.4mg/ml. Furthermore, major HC i.e., caftaric, chlorogenic and rosmarinic acids identified in extracts via UPLC-MS analysis exhibited IC50 values of 24, 0.5 and 7.9mg/ml respectively

  20. High-throughput and rapid quantification of lipids by nanoflow UPLC-ESI-MS/MS: application to the hepatic lipids of rabbits with nonalcoholic fatty liver disease.

    PubMed

    Byeon, Seul Kee; Lee, Jong Cheol; Chung, Bong Chul; Seo, Hong Seog; Moon, Myeong Hee

    2016-07-01

    A rapid and high-throughput quantification method (approximately 300 lipids within 20 min) was established using nanoflow ultrahigh-pressure liquid chromatography-tandem mass spectrometry (nUPLC-ESI-MS/MS) with selective reaction monitoring (SRM) and applied to the quantitative profiling of the hepatic lipids of rabbits with different metabolic conditions that stimulate the development of nonalcoholic fatty liver disease (NAFLD). Among the metabolic conditions of rabbits in this study [inflammation (I), high-cholesterol diet (HC), and high-cholesterol diet combined with inflammation (HCI)], significant perturbation in hepatic lipidome (>3-fold and p < 0.01) was observed in the HC and HCI groups, while no single lipid showed a significant change in group I. In addition, this study revealed a dramatic increase (>2-fold) in relatively high-abundant monohexosylceramides (MHCs), sphingomyelins (SMs), and triacylglycerols (TGs) in both the HC and HCI groups, especially in MHCs as all 11 MHCs increased by larger than 3- to 12-fold. As the levels of the relatively high-abundant lipids in the above classes increased, the total lipidome level of each class increased significantly by approximately 2-fold to 5-fold. Other classes of lipids also generally increased, which was likely induced by the increase in mitogenic and nonapoptotic MHCs and SMs, as they promote cell proliferation. On the other hand, a slight decrease in the level of apoptotic ceramides (Cers) was observed, which agreed with the general increase in total lipid level. As distinct changes in hepatic lipidome were observed from HC groups, this suggests that HC or HCI is highly associated with NAFLD but not inflammation alone itself. Graphical Abstract Schematic of lipidomic analysis from hepatic tissue using nanoflow LC-ESI-MS/MS and nUPLC-ESI-MS/MS.

  1. First Detection of Tetrodotoxin in Greek Shellfish by UPLC-MS/MS Potentially Linked to the Presence of the Dinoflagellate Prorocentrum minimum

    PubMed Central

    Vlamis, Aristidis; Katikou, Panagiota; Rodriguez, Ines; Rey, Verónica; Alfonso, Amparo; Papazachariou, Angelos; Zacharaki, Thetis; Botana, Ana M.; Botana, Luis M.

    2015-01-01

    During official shellfish control for the presence of marine biotoxins in Greece in year 2012, a series of unexplained positive mouse bioassays (MBA) for lipophilic toxins with nervous symptomatology prior to mice death was observed in mussels from Vistonikos Bay–Lagos, Rodopi. This atypical toxicity coincided with (a) absence or low levels of regulated and some non-regulated toxins in mussels and (b) the simultaneous presence of the potentially toxic microalgal species Prorocentrum minimum at levels up to 1.89 × 103 cells/L in the area’s seawater. Further analyses by different MBA protocols indicated that the unknown toxin was hydrophilic, whereas UPLC-MS/MS analyses revealed the presence of tetrodotoxins (TTXs) at levels up to 222.9 μg/kg. Reviewing of official control data from previous years (2006–2012) identified a number of sample cases with atypical positive to asymptomatic negative MBAs for lipophilic toxins in different Greek production areas, coinciding with periods of P. minimum blooms. UPLC-MS/MS analysis of retained sub-samples from these cases revealed that TTXs were already present in Greek shellfish since 2006, in concentrations ranging between 61.0 and 194.7 μg/kg. To our knowledge, this is the earliest reported detection of TTXs in European bivalve shellfish, while it is also the first work to indicate a possible link between presence of the toxic dinoflagellate P. minimum in seawater and that of TTXs in bivalves. Confirmed presence of TTX, a very heat-stable toxin, in filter-feeding mollusks of the Mediterranean Sea, even at lower levels to those inducing symptomatology to humans, indicates that this emerging risk should be seriously taken into account by the EU to protect the health of shellfish consumers. PMID:26008234

  2. Using UPLC-QTOF-MS to analyze the chemical changes between traditional and dispensing granule decoctions of San-Ao-Tang.

    PubMed

    Ma, Chunhua; Qian, Yefei; Fan, Xinsheng; Shang, ErXin; Yao, Xin; Ma, Shiping

    2014-04-01

    In the present study, a chemical profiling approach based on ultra-performance liquid chromatography coupled with photodiode array detection and time-of-flight mass spectrometry (UPLC-PDA-TOF-MS) was proposed to rapidly evaluate the chemical consistency between traditional and dispensing granule decoctions of traditional medicine combinatorial formulae and validated using San-Ao-Tang (SAT) as a model combinatorial formula. SAT is an effective traditional Chinese medicine, which is usually used in treating asthma and other diseases of the respiratory system. Two decoctions were prepared: traditional decoction, which is a water extract of three mixed constituent herbs of SAT; and dispensing granule decoction, which is a mixed water extract of each individual herb of SAT. Batches of these two decoction samples were subjected to UPLC-PDA-TOF-MS analysis and the data sets of t(R)-m/z pairs, ion intensities and sample codes were processed with supervised orthogonal partial least squared discriminant analysis to holistically compare their differences. Once a clear classification trend was found in the score plot, further statistics were performed to generate points at the two ends of S, and the components that correlated to these ions were regarded as the most changed components during decoction of the combinatorial formula. The changed components were identified by comparing the mass/ultraviolet spectra and retention times with those of reference compounds and/or tentatively assigned by matching empirical molecular formulae with those of the known compounds published in the literature. Using the proposed approach, global chemical differences were found between traditional and dispensing granule decoctions, like ephedrine, pseudoephedrine, norpseudoephedrine, licorice saponine H2, licorice saponine G2 and amygdalin. PMID:23572319

  3. Chemical quantification and antioxidant assay of four active components in Ficus hirta root using UPLC-PAD-MS fingerprinting combined with cluster analysis

    PubMed Central

    2013-01-01

    Background Root of Ficus hirta (RFH) is widely consumed in China as a plant-derived popular food. However, contents of the active constituents of RFH are unknown, and the chemical as well as bioactive properties of RFH may be affected by growing area. In order to ensure the standard efficacy of health products made with RFH, its active constituents should firstly be determined and, secondly, a means of assessing samples for their contents of these constituents is needed. Results Four active components, including two coumarins, namely psoralen and bergapten, and two flavonoids, namely luteolin and apigenin, in twenty RFH samples were quantified using a new ultra performance liquid chromatography coupled with photodiode array detector and mass spectrometry (UPLC-PAD-MS) method, and the content level in descending order was psoralen > bergapten > luteolin > apigenin. Chromatographic fingerprint similarity evaluation and cluster analysis were used to assess geographical origin of RFH, and the results revealed a high level of similarity for the tested RFH samples obtained from Hainan, Guangdong, Guangxi provinces and Hong Kong. 2, 2-Diphenyl-1-picrylhydrazyl (DPPH) radical scavenging assay was conducted to evaluate the antioxidant potencies of the four components, and the results clearly demonstrated that luteolin was most effective; apigenin exhibited a moderate potency, whereas psoralen and bergapten possessed little effect against free radical reactions. Structure-activity relationship of the components was elucidated, and the 3′-hydroxyl group of luteolin was found to be directly responsible for its antioxidant activity. Conclusion The present UPLC-PAD-MS method and DPPH radical scavenging assay performed well for the purpose of constituent quantification and antioxidant assay. Global profiles were highly similar for RFH samples from different origins. Both the coumarins and flavonoids were involved in the health benefit of RFH. PMID:23835498

  4. Column flooding and entrainment. [Estimation of maximum allowable vapor velocity and entrainment in a distillation column

    SciTech Connect

    Lygeros, A.I.; Magoulas, K.G.

    1986-12-01

    Here is a way to estimate maximum allowable vapor velocity and entrainment in a distillation column. The method can easily be computerized. It is based on equations derived from the widely accepted correlations. The equation for flooding velocity is applicable to bubble-cup, sieve and valve trays, while the entrainment equation applies only to sieve trays.

  5. Comparison between a spray column and a sieve tray column operating as liquid-liquid heat exchangers

    SciTech Connect

    Keller, A.; Jacobs, H.R.; Boehm, R.F.

    1980-12-01

    The performance of a spray column and a sieve tray column was compared as a liquid-liquid heat exchanger. In carrying out these studies a 15.2 cm (6.0 in.) diameter column, 183 cm (6.0 ft) tall was utilized. The performance of the spray column as a heat exchanger was shown to correlate with the model of Letan-Kehat which has as a basis that the heat transfer is dominated by the wakeshedding characteristics of the drops over much of the column length. This model defines several hydrodynamic zones along the column of which the wake formation zone at the bottom appears to have the most efficient heat transfer. The column was also operated with four perforated plates spaced two column diameters apart in order to take advantage of the wake formation zone heat transfer. The plates induce coalescence of the dispersed phase and reformation of the drops, and thus cause a repetition of the wake formation zone. It is shown that the overall volumetric heat transfer coefficient in a perforated plate column is increased by a minimum of eleven percent over that in a spray column. A hydrodynamic model that predicts the performance of a perforated plate column is suggested.

  6. [A novel solid phase extraction column combined with ultra performance liquid chromatography/tandem mass spectrometry for selective enrichment and determination of clenbuterol in pork].

    PubMed

    Meng, Wenying; Guo, Zhimou; Shen, Weijian; Shen, Chongyu; Wu, Bin; Liu, Yanming; Zhang, Feifang; Liang, Xinmiao

    2012-02-01

    A simple and efficient method based on a novel solid phase extraction (SPE) cartridge and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/ MS) was developed for the determination of clenbuterol residue in pork. The minced pork sample was ultrasonically extracted by 5% (v/v) perchloric acid and centrifuged at 10 000 r/min for 15 min, then the supernatant was purified by an SMCX cartridge, which is a novel SPE column based on homemade silica matrix with two mixed modes of reversed-phase and strong cation exchange, for the selective enrichment and purification of the analyte. The linear range of the method was 0.25 - 50 microg/kg with a correlation coefficient of 0.998 2. The average recoveries ranged from 62.2% to 72.0% at the three spiked levels of 1.25, 12.5 and 50 microg/kg with the relative standard deviations (RSDs) between 4.2% and 6.1%. The limit of detection (S/N = 3) was 0.05 microg/kg. The method is simple, fast and can be extended to enrich and determine beta-agonist drugs.

  7. Column properties and flow profiles of a flat, wide column for high-pressure liquid chromatography

    SciTech Connect

    Mriziq, Khaled S; Guiochon, Georges A

    2008-01-01

    The design and the construction of a pressurized, flat, wide column for high-performance liquid chromatography (HPLC) are described. This apparatus, which is derived from instruments that implement over-pressured thin layer chromatography, can carry out only uni-dimensional chromatographic separations. However, it is intended to be the first step in the development of more powerful instruments that will be able to carry out two-dimensional chromatographic separations, in which case, the first separation would be a space-based separation, LC{sup x}, taking place along one side of the bed and the second separation would be a time-based separation, LC{sup t}, as in classical HPLC but proceeding along the flat column, not along a tube. The apparatus described consists of a pressurization chamber made of a Plexiglas block and a column chamber made of stainless steel. These two chambers are separated by a thin Mylar membrane. The column chamber is a cavity which is filled with a thick layer (ca. 1 mm) of the stationary phase. Suitable solvent inlet and outlet ports are located on two opposite sides of the sorbent layer. The design allows the preparation of a homogenous sorbent layer suitable to be used as a chromatographic column, the achievement of effective seals of the stationary phase layer against the chamber edges, and the homogenous flow of the mobile phase along the chamber. The entire width of the sorbent layer area can be used to develop separations or elute samples. The reproducible performance of the apparatus is demonstrated by the chromatographic separations of different dyes. This instrument is essentially designed for testing detector arrays to be used in a two-dimensional LC{sup x} x LC{sup t} instrument. The further development of two-dimension separation chromatographs based on the apparatus described is sketched.

  8. Heat Transfer Analysis for a Fixed CST Column

    SciTech Connect

    Lee, S.Y.

    2004-02-19

    In support of a small column ion exchange (SCIX) process for the Savannah River Site waste processing program, a transient two-dimensional heat transfer model that includes the conduction process neglecting the convection cooling mechanism inside the crystalline silicotitanate (CST) column has been constructed and heat transfer calculations made for the present design configurations. For this situation, a no process flow condition through the column was assumed as one of the reference conditions for the simulation of a loss-of-flow accident. A series of the modeling calculations has been performed using a computational heat transfer approach. Results for the baseline model indicate that transit times to reach 130 degrees Celsius maximum temperature of the CST-salt solution column are about 96 hours when the 20-in CST column with 300 Ci/liter heat generation source and 25 degrees Celsius initial column temperature is cooled by natural convection of external air as a primary heat transfer mechanism. The modeling results for the 28-in column equipped with water jacket systems on the external wall surface of the column and water coolant pipe at the center of the CST column demonstrate that the column loaded with 300 Ci/liter heat source can be maintained non-boiling indefinitely. Sensitivity calculations for several alternate column sizes, heat loads of the packed column, engineered cooling systems, and various ambient conditions at the exterior wall of the column have been performed under the reference conditions of the CST-salt solution to assess the impact of those parameters on the peak temperatures of the packed column for a given transient time. The results indicate that a water-coolant pipe at the center of the CST column filled with salt solution is the most effective one among the potential design parameters related to the thermal energy dissipation of decay heat load. It is noted that the cooling mechanism at the wall boundary of the column has significant

  9. Comparison of two column characterisation systems based on pharmaceutical applications.

    PubMed

    Haghedooren, Erik; Németh, Tamás; Dragovic, Sanja; Noszál, Béla; Hoogmartens, Jos; Adams, Erwin

    2008-05-01

    A useful column characterisation system should help chromatographers to select the most appropriate column to use, e.g. when a particular chromatographic column is not available or when facing the dilemma of selecting a suitable column for analysis according to an official monograph. Official monographs of the European Pharmacopoeia and the United States Pharmacopeia are not allowed to mention the brand name of the stationary phase used for the method development. Also given the overwhelming offer of several hundreds of commercially available reversed-phase liquid chromatographic columns, the choice of a suitable column could be difficult sometimes. To support rational column selection, a column characterisation study was started in our laboratory in 2000. In the same period, Euerby et al. also developed a column characterisation system, which is now released as Column Selector by ACD/Labs. The aim of this project was to compare the two existing column characterisation systems, i.e. the KUL system and the Euerby system. Other research groups active in this field will not be discussed here. Euerby et al. developed a column characterisation system based on 6 test parameters, while the KUL system is based on 4 chromatographic parameters. Comparison was done using a set of 63 columns. For 7 different pharmaceutical separations (fluoxetine, gemcitabine, erythromycin, tetracycline, tetracaine, amlodipine and bisacodyl), a ranking was built based on an F-value (KUL method) or Column Difference Factor value (Euerby method) versus a (virtual) reference column. Both methods showed a similar ranking. The KUL and Euerby methods do not perfectly match, but they yield very similar results, allowing with a relatively high certainty, the selection of similar or dissimilar columns as compared to a reference column. An analyst that uses either of the two methods, will end up with a similar ranking. From a practical point of view, it must be noted that the KUL method only includes 4

  10. Enhanced reductive dechlorination in columns treated with edible oil emulsion

    NASA Astrophysics Data System (ADS)

    Long, Cameron M.; Borden, Robert C.

    2006-09-01

    The effect of edible oil emulsion treatment on enhanced reductive dechlorination was evaluated in a 14 month laboratory column study. Experimental treatments included: (1) emulsified soybean oil and dilute HCl to inhibit biological activity; (2) emulsified oil only; (3) emulsified oil and anaerobic digester sludge; and (4) continuously feeding soluble substrate. A single application of emulsified oil was effective in generating strongly reducing, anaerobic conditions for over 14 months. PCE was rapidly reduced to cis-DCE in all three live columns. Bioaugmentation with a halorespiring enrichment culture resulted in complete dechlorination of PCE to ethene in the soluble substrate column (yeast extract and lactate). However, an additional treatment with a pulse of yeast extract and bioaugmentation culture was required to stimulate complete dechlorination in the emulsion treated columns. Once the dechlorinating population was established, the emulsion only column degraded PCE from 90-120 μM to below detection with concurrent ethene production in a 33 day contact time. The lower biodegradation rates in the emulsion treated columns compared to the soluble substrate column suggest that emulsified oil barriers may require a somewhat longer contact time for effective treatment. In the HCl inhibited column, partitioning of PCE to the retained oil substantially delayed PCE breakthrough. However, reduction of PCE to more soluble degradation products ( cis-DCE, VC and ethene) greatly reduced the impact of oil-water partitioning in live columns. There was only a small decline in the hydraulic conductivity ( K) of column #1 (low pH + emulsion, Kfinal/ Kinitial = 0.57) and column #2 (live + emulsion, Kfinal/ Kinitial = 0.73) indicating emulsion injection did not result in appreciable clogging of the clayey sand. However, K loss was greater in column #3 (sludge +emulsion, Kfinal/ Kinitial = 0.12) and column #4 (soluble substrate, Kfinal/ Kinitial = 0.03) indicating clogging due

  11. The vertebral column of Australopithecus sediba.

    PubMed

    Williams, Scott A; Ostrofsky, Kelly R; Frater, Nakita; Churchill, Steven E; Schmid, Peter; Berger, Lee R

    2013-04-12

    Two partial vertebral columns of Australopithecus sediba grant insight into aspects of early hominin spinal mobility, lumbar curvature, vertebral formula, and transitional vertebra position. Au. sediba likely possessed five non-rib-bearing lumbar vertebrae and five sacral elements, the same configuration that occurs modally in modern humans. This finding contrasts with other interpretations of early hominin regional vertebral numbers. Importantly, the transitional vertebra is distinct from and above the last rib-bearing vertebra in Au. sediba, resulting in a functionally longer lower back. This configuration, along with a strongly wedged last lumbar vertebra and other indicators of lordotic posture, would have contributed to a highly flexible spine that is derived compared with earlier members of the genus Australopithecus and similar to that of the Nariokotome Homo erectus skeleton.

  12. Dynamic CT scanning of spinal column trauma

    SciTech Connect

    Brown, B.M.; Brant-Zawadzki, M.; Cann, C.E.

    1982-12-01

    Dynamic sequential computed tomographic scanning with automatic table incrementation uses low milliampere-second technique to eliminate tube cooling delays between scanning slices and, thus, markedly shortens examination times. A total of 25 patients with spinal column trauma involving 28 levels were studied with dynamic scans and retrospectively reviewed. Dynamic studies were considerably faster than conventional spine examinations and yielded reliable diagnosis. Bone disruption and subluxation was accurately evaluated, and the use of intrathecal metrizamide in low doses allowed direct visualization of spinal cord or radicular compromise. Multiplanar image reformation was aided by the dynamic incrementation technique, since motion between slices (and the resulting misregistration artifact on image reformation) was minimized. A phantom was devised to test spatial resolution of computed tomography for objects 1-3 mm in size and disclosed minimal differences for dynamic and conventional computed tomographic techniques in resolving medium-to-high-contrast objects.

  13. Ewing's sarcoma of the vertebral column

    SciTech Connect

    Pilepich, M.V.; Vietti, T.J.; Nesbit, M.E.; Tefft, M.; Kissane, J.; Burgert, O.; Pritchard, D.; Gehan, E.A.

    1981-01-01

    Twenty-two patients with vertebral primaries were registered in the Intergroup Ewing's Sarcoma Study between 1973 and 1977. The radiation doses to the primary tumors ranged between 3800 and 6200 rad. All patients received intensive combination chemotherapy. After a followup ranging between 14 and 62 months, 14 patients remained disease-free. All patients with primary tumor of the cervical and dorsal spine remained disease-free. Of eight patients with lesions in the distal spine, (sacrococcygeal region) six developed recurrence, in three a local recurrence was observed despite doses of 6000 rad or higher. Doses of 5000 rad or less (in addition to combination chemotherapy as used in the Intergroup Ewing's Study) appear adequate in controlling the primary tumors of the proximal segments of the spinal column.

  14. The vertebral column of Australopithecus sediba.

    PubMed

    Williams, Scott A; Ostrofsky, Kelly R; Frater, Nakita; Churchill, Steven E; Schmid, Peter; Berger, Lee R

    2013-04-12

    Two partial vertebral columns of Australopithecus sediba grant insight into aspects of early hominin spinal mobility, lumbar curvature, vertebral formula, and transitional vertebra position. Au. sediba likely possessed five non-rib-bearing lumbar vertebrae and five sacral elements, the same configuration that occurs modally in modern humans. This finding contrasts with other interpretations of early hominin regional vertebral numbers. Importantly, the transitional vertebra is distinct from and above the last rib-bearing vertebra in Au. sediba, resulting in a functionally longer lower back. This configuration, along with a strongly wedged last lumbar vertebra and other indicators of lordotic posture, would have contributed to a highly flexible spine that is derived compared with earlier members of the genus Australopithecus and similar to that of the Nariokotome Homo erectus skeleton. PMID:23580532

  15. Micro-column plasma emission liquid chromatograph

    DOEpatents

    Gay, Don D.

    1984-01-01

    In a direct current plasma emission spectrometer for use in combination with a micro-column liquid chromatograph, an improved plasma source unit. The plasma source unit includes a quartz capillary tube having an inlet means, outlet off gas means and a pair of spaced electrodes defining a plasma region in the tube. The inlet means is connected to and adapted to receive eluant of the liquid chromatograph along with a stream of plasma-forming gas. There is an opening through the wall of the capillary tube penetrating into the plasma region. A soft glass capillary light pipe is disposed at the opening, is connected to the spectrometer, and is adapted to transmit light passing from the plasma region to the spectrometer. There is also a source of electromotive force connected to the electrodes sufficient to initiate and sustain a plasma in the plasma region of the tube.

  16. Rapid Column Extraction Methods for Urine

    SciTech Connect

    Maxwell, S.L. III

    2000-06-09

    A new fecal analysis method that dissolves plutonium oxide was developed at the Westinghouse Savannah River Site. Diphonix Resin (Eichrom Industries), is used to pre-concentrate the actinides from digested fecal samples. A rapid microwave digestion technique is used to remove the actinides from the Diphonix Resin, which effectively extracts plutonium and americium from acidic solutions containing hydrofluoric acid. After resin digestion, the plutonium and americium are recovered in a small volume of nitric acid that is loaded onto small extraction chromatography columns, TEVA Resin and TRU Resin (Eichrom Industries). The method enables complete dissolution of plutonium oxide and provides high recovery of plutonium and americium with good removal of thorium isotopes such as thorium-228.

  17. The flotation column as a froth separator

    SciTech Connect

    Schultz, C.W.; Mehta, R.K.; Bates, J.B. )

    1991-12-01

    The Mineral Resources Institute, The University of Alabama, has for the past three years been engaged in a program to develop a beneficiation system for eastern (Devonian) oil shales. One objective of that program was to evaluate advanced technologies for effecting a kerogen-mineral matter separation. Column flotation was among the advanced technologies selected for evaluation. One observation made in the course of optimization testing was that introducing the feed into the froth (above the pulp- froth interface) resulted in an improved combination of concentrate grade and kerogen recovery. This observation was reported in a previous paper. Because the practice of maintaining the pulp froth interface below the feed point is contrary to conventional practice, it was decided to subject the observation to a systematic series of tests. This paper describes a recent series of tests and the results that were obtained.

  18. Novel electrostatic column for ion projection lithography

    SciTech Connect

    Chalupka, A.; Stengl, G.; Buschbeck, H.; Lammer, G.; Vonach, H.; Fischer, R.; Hammel, E.; Loeschner, H.; Nowak, R.; Wolf, P. ); Finkelstein, W.; Hill, R.W. ); Berry, I.L. ); Harriott, L.R. ); Melngailis, J. ); Randall, J.N. ); Wolfe, J.C. ); Stroh, H.; Wollnik, H. ); Mondelli, A.A.; Petillo, J.J. ); Leung, K. (Lawrence Berkeley Laboratory, University of Californi

    1994-11-01

    Ion projection lithography (IPL) is being considered for high volume sub-0.25-[mu]m lithography. A novel ion-optical column has been designed for exposing 20[times]20 mm[sup 2] fields at 3[times] reduction from stencil mask to wafer substrates. A diverging lens is realized by using the stencil mask as the first electrode of the ion-optical column. The second and third electrode form an accelerating field lens. The aberrations of the first two lenses (diverging lens and field lens) are compensated by an asymmetric Einzel lens projecting an ion image of the stencil mask openings onto the wafer substrate with better than 2 mrad telecentricity. Less than 30 nm intrafield distortion was calculated within 20[times]20 mm[sup 2] exposure fields. The calculation uncertainty is estimated to be about 10 nm. The calculation holds for helium ions with [approx]10 keV ion energy at the stencil mask and 150 keV ion energy at the wafer plane. A virtual ion source size of 10 [mu]m has been assumed. The calculated chromatic aberrations are less than 60 nm, assuming 6 eV energy spread of the ions extracted from a duoplasmatron source. Recently a multicusp ion source has been developed for which preliminary results indicate an energy spread of less than 2 eV. Thus, with a multicusp source chromatic aberrations of less than 20 nm are to be expected. The ion energy at the crossover between the field lens and the asymmetric Einzel lens is 200 keV. Therefore, stochastic space charge induced degradations in resolution can be kept sufficiently low. The divergence of the ion image projected to the wafer plane is less than 2 mrad. Thus, the usable'' depth of focus for the novel ion optics is in the order of 10 [mu]m.

  19. Multiple column high-throughput e-beam inspection (EBI)

    NASA Astrophysics Data System (ADS)

    Lam, David K.; Monahan, Kevin M.; Liu, Enden D.; Tran, Cong; Prescop, Ted

    2012-03-01

    Single-column e-beam systems are used in production for the detection of electrical defects, but are too slow to be used for the detection of small physical defects, and can't meet future inspection requirements. This paper presents a multiplecolumn e-beam technology for high throughput wafer inspection. Multibeam has developed all-electrostatic columns for high-resolution imaging. The elimination of magnetic coils enables the columns to be small; e-beam deflection is faster in the absence of magnetic hysteresis. Multiple miniaturecolumns are assembled in an array. An array of 100 columns covers the entire surface of a 300mm wafer, affording simultaneous cross-wafer sampling. Column performance simulations and system architecture are presented. Also provided are examples of high throughput, more efficient, multiple-column wafer inspection.

  20. Parallel array of independent thermostats for column separations

    DOEpatents

    Foret, Frantisek; Karger, Barry L.

    2005-08-16

    A thermostat array including an array of two or more capillary columns (10) or two or more channels in a microfabricated device is disclosed. A heat conductive material (12) surrounded each individual column or channel in array, each individual column or channel being thermally insulated from every other individual column or channel. One or more independently controlled heating or cooling elements (14) is positioned adjacent to individual columns or channels within the heat conductive material, each heating or cooling element being connected to a source of heating or cooling, and one or more independently controlled temperature sensing elements (16) is positioned adjacent to the individual columns or channels within the heat conductive material. Each temperature sensing element is connected to a temperature controller.

  1. Temperature-compensated 8-bit column driver for AMLCD

    NASA Astrophysics Data System (ADS)

    Dingwall, Andrew G. F.; Lin, Mark L.

    1995-06-01

    An all-digital, 5 V input, 50 Mhz bandwidth, 10-bit resolution, 128- column, AMLCD column driver IC has been designed and tested. The 10-bit design can enhance display definition over 6-bit nd 8-bit column drivers. Precision is realized with on-chip, switched-capacitor DACs plus transparently auto-offset-calibrated, opamp outputs. Increased resolution permits multiple 10-bit digital gamma remappings in EPROMs over temperature. Driver IC features include externally programmable number of output column, bi-directional digital data shifting, user- defined row/column/pixel/frame inversion, power management, timing control for daisy-chained column drivers, and digital bit inversion. The architecture uses fewer reference power supplies.

  2. Applicability of hydroxylamine nitrate reductant in pulse-column contactors

    SciTech Connect

    Reif, D.J.

    1983-05-01

    Uranium and plutonium separations were made from simulated breeder reactor spent fuel dissolver solution with laboratory-sized pulse column contactors. Hydroxylamine nitrate (HAN) was used for reduction of plutonium (1V). An integrated extraction-partition system, simulating a breeder fuel reprocessing flowsheet, carried out a partial partition of uranium and plutonium in the second contactor. Tests have shown that acceptable coprocessing can be ontained using HAN as a plutonium reductant. Pulse column performance was stable even though gaseous HAN oxidation products were present in the column. Gas evolution rates up to 0.27 cfm/ft/sup 2/ of column cross section were tested and found acceptable.

  3. Monolithic capillary columns based on pentaerythritol tetraacrylate for peptide analysis

    NASA Astrophysics Data System (ADS)

    Kucherenko, E. V.; Melnik, D. M.; Korolev, A. A.; Kanateva, A. Yu.; Pirogov, A. V.; Kurganov, A. A.

    2015-09-01

    Monolythic medium-polar capillary columns based on pentaerythritol tetraacrylate were optimized for separation of peptides. The synthesis temperature and time, the fraction of monomer in the initial polymerization mixture, and the nature of alcohol contained in the complex porogen were chosen as optimization parameters. The highest efficiency was attained for columns obtained with 33 and 34% monomer at a polymerization time of 75 min and a temperature of 75°C. The columns with the optimum structure were effective in separation of a model mixture of five peptides. The sensitivity of the method was 200 ng of peptide per column.

  4. Optimal packing characteristics of rolled, continuous stationary-phase columns.

    PubMed

    Li, Chenghong; Ladisch, Christine M; Yang, Yiqi; Hendrickson, Richard; Keim, Craig; Mosier, Nathan; Ladisch, Michael R

    2002-01-01

    Rolled, continuous stationary phases were constructed by tightly rolling and inserting a whole textile fabric into a chromatography column. This work reports the column performance, in terms of plate height, void fraction, and resolution, of 10 cellulose-based fabrics. The relation between fabric structural properties of yarn diameter, fabric count, fabric compressibility, and column performance are quantitated. General requirements, including reproducibility of packing, for choosing fabrics to make a good SEC column are identified. This research showed that the packed columns have an optimal mass of fabric that minimizes plate height and maximizes resolution, in a manner that is consistent with chromatography theory. Mass of material packed is then an important column parameter to consider when optimizing columns for the rapid desalting of proteins. Proteins were completely separated from salt and glucose in less than 8 min at a pressure drop less than 500 psi on the rolled, continuous stationary-phase columns. These results, together with stability and reproducibility, suggest potential industrial applications for cellulose-based rolled, continuous stationary-phase columns where speed is a key parameter in the production process. PMID:11934301

  5. Mini-columns for Conducting Breakthrough Experiments. Design and Construction

    SciTech Connect

    Dittrich, Timothy M.; Reimus, Paul William; Ware, Stuart Douglas

    2015-06-11

    Experiments with moderately and strongly sorbing radionuclides (i.e., U, Cs, Am) have shown that sorption between experimental solutions and traditional column materials must be accounted for to accurately determine stationary phase or porous media sorption properties (i.e., sorption site density, sorption site reaction rate coefficients, and partition coefficients or Kd values). This report details the materials and construction of mini-columns for use in breakthrough columns to allow for accurate measurement and modeling of sorption parameters. Material selection, construction techniques, wet packing of columns, tubing connections, and lessons learned are addressed.

  6. 15. FIRST FLOOR WAREHOUSE SPACE, SHOWING COLUMN / BEAM CONNECTION. ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    15. FIRST FLOOR WAREHOUSE SPACE, SHOWING COLUMN / BEAM CONNECTION. VIEW TO SOUTHWEST. - Commercial & Industrial Buildings, Dubuque Seed Company Warehouse, 169-171 Iowa Street, Dubuque, Dubuque County, IA

  7. Stability of leaning column at Devils Tower National Monument, Wyoming

    USGS Publications Warehouse

    Harp, Edwin L.; Lindsay, Charles R.

    2006-01-01

    In response to reports from climbers that an 8-meter section (referred to as the leaning column) of the most popular climbing route on Devils Tower in northeastern Wyoming is now moving when being climbed, scientists from the U.S. Geological Survey inspected the site to determine the stability of the column and the underlying column that serves as a support pedestal. Evidence of a recent tensile spalling failure was observed on the pedestal surface immediately beneath the contact with the overlying leaning column. The spalling of a flake-shaped piece of the pedestal, probably due to the high stress concentration exerted by the weight of the leaning column along a linear contact with the pedestal, is likely causing the present movement of the leaning column. Although it is unlikely that climbers will dislodge the leaning column by their weight alone, the possibility exists that additional spalling failures may occur from the pedestal surface and further reduce the stability of the leaning column and result in its toppling. To facilitate detection of further spalling failures from the pedestal, its surface has been coated with a layer of paint. Any new failures from the pedestal could result in the leaning column toppling onto the climbing route or onto the section of the Tower trail below.

  8. Fracture Behaviour of Glass Columns Experimental Study of Axial Loaded Glass Columns

    NASA Astrophysics Data System (ADS)

    Jakab, A.; Nehme, K.; Nehme, S. G.

    2016-04-01

    Nowadays supporting structures can be transparent due to the development of glass strengthening procedures. The building glass as a versatile building material enables the efforts of the architects due to its transparency. This paper focuses on glass columns in the topic of load-bearing glasses and also on the design and load bearing capacity of fins and stability issues. Laboratory experiments were carried out at the BME, Department of Building Materials and Engineering Geology on the fracture behaviour of centrally compressed glass columns. More than 120 specimens where loaded until fracture. The load and deformations were measured. Based on the experimental results the critical force was determined and with force-deflection diagrams were illustrated the fracture and stability processes. Authors are going to compare the results of the laboratory experiments and theoretical calculations.

  9. Evolution of mantle column beneath Bartoy volcanoes.

    NASA Astrophysics Data System (ADS)

    Ashchepkov, Igor; Karmanov, Nikolai; Kanakin, Sergei; Ntaflos, Theodoros

    2013-04-01

    Pleistocene Bartoy volcanoes 1.5-0.8 Ma (Ashchepkov et al., 2003) represent variable set of hydrous cumulates and megacrysts and peridotite mantle xenoliths from spinel facies (Ashchepkov, 1991; Ionov, Kramm, 1992). Hydrous peridotites give series of the temperature groups: 1) deformed Fe - lherzolites (1200-1100o) , 2) Phl porhyroclastiμ (1100-1020o), 3) Amph -Phl (1020-940o), 4) Dry protogranular (1020-940o), 5)Amph equigranular (940-880o) and 6) dry and fine grained (880-820o). and Fe-rich poikilitic (700-600o) (Ashchepkov, 1991). T according (Nimis, Taylor, 2000) The sequence of the megacrysts crystallized on the wall of basaltic feeder in pre - eruption stage is starting from HT dark green websterites (1300-1200o), black Cpx- Gar varieties (1250-1200o) evolved to Phl -CPx (1200-1130o) and Cpx - Kaers (1130-1020o) - Cpx low in TiO2., Ilm and San (<1000o) like in Vitim (Ashchepkov et la., 2011). The differentiation trends looks branched but the question if they. Differentiation ain relatively large magma bodies p produced Ga- Cpx (+Amph-Phl- Ilm +-San) and then Cpx-Gar -Pl cumulates in( ~8-12 kbar) interval. In the ToC-Fe# diagram the Intermediate trend between lherzolites and megacrysts sub parallel to lherzolitic is correspondent to the fractionation of the hydrous alkali basalt melts in vein network created from the highly H2O bearing basaltic derivates formed in intermediate magma chambers. The interaction of the peridotites with the pulsing rising and evolving basaltic system produced the wall rock metasomatism and separate groups of peridotites in different levels of mantle column. PT calculations show two PT path and probably melt intrusion events. Trace elements in glass from crystalline basalts show Zr, Pb dips and Ta, Nb, Sr enrichment for the black megacrystalline Cpx , Gar series. They show link with evolved basalts by HFSE, Ba enrichment but Cpx from kaersutite and further Gar - Cpx cumulates show depressions in Ta, Nb, Zr, and Pb moderate

  10. Quantitative Assessment of the Influence of Rhizoma Zingiberis on the Level of Aconitine in Rat Gut Sacs and Qualitative Analysis of the Major Influencing Components of Rhizoma Zingiberis on Aconitine Using UPLC/MS

    PubMed Central

    Xin, Yang; Liu, Shuying

    2015-01-01

    This study attempted to clarify the material basis for the detoxification of Rhizoma Zingiberis (RZ) on aconitine, an analgesic drug, by quantitatively assessing the influence of RZ on the in vitro intestinal concentration of aconitine using an everted gut sac model and by qualitatively identifying the components in the RZ extract. To quantify aconitine in rat everted gut sacs, both an accurate processing method and a sensitive detection method were required. We developed a three-step sample processing method to protect the components from decomposition and applied ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC/TQMS) to quantify aconitine, glucose and digoxin. In addition, ultra-performance liquid chromatography coupled with linear ion trap mass spectrometry (UPLC/ITMS) was applied to detect the potential antidotal components in the RZ extract. Finally, the RZ extract reduced the level of aconitine in everted gut sacs, and eleven gingerols were successfully identified, which could be considered potential antidotal components for aconitine. This study demonstrated the application of two UPLC/MS methods for analyzing the material basis for the reciprocity between Chinese medicine components in everted gut sacs. PMID:25978042

  11. Differentiating organically and conventionally grown oregano using ultraperformance liquid chromatography mass spectrometry (UPLC-MS), headspace gas chromatography with flame ionization detection (headspace-GC-FID), and flow injection mass spectrum (FIMS) fingerprints combined with multivariate data analysis.

    PubMed

    Gao, Boyan; Qin, Fang; Ding, Tingting; Chen, Yineng; Lu, Weiying; Yu, Liangli Lucy

    2014-08-13

    Ultraperformance liquid chromatography mass spectrometry (UPLC-MS), flow injection mass spectrometry (FIMS), and headspace gas chromatography (headspace-GC) combined with multivariate data analysis techniques were examined and compared in differentiating organically grown oregano from that grown conventionally. It is the first time that headspace-GC fingerprinting technology is reported in differentiating organically and conventionally grown spice samples. The results also indicated that UPLC-MS, FIMS, and headspace-GC-FID fingerprints with OPLS-DA were able to effectively distinguish oreganos under different growing conditions, whereas with PCA, only FIMS fingerprint could differentiate the organically and conventionally grown oregano samples. UPLC fingerprinting provided detailed information about the chemical composition of oregano with a longer analysis time, whereas FIMS finished a sample analysis within 1 min. On the other hand, headspace GC-FID fingerprinting required no sample pretreatment, suggesting its potential as a high-throughput method in distinguishing organically and conventionally grown oregano samples. In addition, chemical components in oregano were identified by their molecular weight using QTOF-MS and headspace-GC-MS.

  12. Quantitative Assessment of the Influence of Rhizoma Zingiberis on the Level of Aconitine in Rat Gut Sacs and Qualitative Analysis of the Major Influencing Components of Rhizoma Zingiberis on Aconitine Using UPLC/MS.

    PubMed

    Xin, Yang; Liu, Shuying

    2015-01-01

    This study attempted to clarify the material basis for the detoxification of Rhizoma Zingiberis (RZ) on aconitine, an analgesic drug, by quantitatively assessing the influence of RZ on the in vitro intestinal concentration of aconitine using an everted gut sac model and by qualitatively identifying the components in the RZ extract. To quantify aconitine in rat everted gut sacs, both an accurate processing method and a sensitive detection method were required. We developed a three-step sample processing method to protect the components from decomposition and applied ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC/TQMS) to quantify aconitine, glucose and digoxin. In addition, ultra-performance liquid chromatography coupled with linear ion trap mass spectrometry (UPLC/ITMS) was applied to detect the potential antidotal components in the RZ extract. Finally, the RZ extract reduced the level of aconitine in everted gut sacs, and eleven gingerols were successfully identified, which could be considered potential antidotal components for aconitine. This study demonstrated the application of two UPLC/MS methods for analyzing the material basis for the reciprocity between Chinese medicine components in everted gut sacs.

  13. [Determination of 9 cephalosporin drug residues in beef by ultra performance liquid chromatography-tandem mass spectrometry].

    PubMed

    Bai, Guotao; Chu, Xiaogang; Pan, Guoqing; Li, Xiuqin; Yong, Wei

    2009-07-01

    A confirmative method to determine 9 cephalosporin residues in beef by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. The sample was homogenized and extracted with acetonitrile and water for 1 min at 14,000 r/min, centrifuged at 10,000 r/min and 4 degrees C for 10 min. A total of 2 mL saturated sodium chloride solution was added to avoid foaming during the acetonitrile evaporation, the acetonitrile was evaporated below 37 degrees C using a rotary evaporator, and then cleaned up on an Oasis HLB (500 mg, 6 mL) SPE column by washing with 5 mL water and eluting with acetonitrile-water (7:3, v/v). The eluate was blown to dryness under a stream of nitrogen and adjusted to 3.0 mL with water. The separation was carried out on an ACQUITY UPLC BEH C18 column within 5 min, analyzed by UPLC-MS/MS system with external standard method. The limits of quantification (LOQs) of cefuroxime, ceftiofur and cefalonium were 10, 0.5 and 0.5 microg/kg, respectively; the LOQs of other cephalosporins were 1.0 microg/kg. The recoveries of cephalosporins ranged from 74.2% to 119% and the relative standard deviations (RSDs) ranged from 2.9% to 15% for the spiked beef sample. The method is quick, easy, very sensitive and suitable for the determination of cephalosporin residues in beef.

  14. SPR Hydrostatic Column Model Verification and Validation.

    SciTech Connect

    Bettin, Giorgia; Lord, David; Rudeen, David Keith

    2015-10-01

    A Hydrostatic Column Model (HCM) was developed to help differentiate between normal "tight" well behavior and small-leak behavior under nitrogen for testing the pressure integrity of crude oil storage wells at the U.S. Strategic Petroleum Reserve. This effort was motivated by steady, yet distinct, pressure behavior of a series of Big Hill caverns that have been placed under nitrogen for extended period of time. This report describes the HCM model, its functional requirements, the model structure and the verification and validation process. Different modes of operation are also described, which illustrate how the software can be used to model extended nitrogen monitoring and Mechanical Integrity Tests by predicting wellhead pressures along with nitrogen interface movements. Model verification has shown that the program runs correctly and it is implemented as intended. The cavern BH101 long term nitrogen test was used to validate the model which showed very good agreement with measured data. This supports the claim that the model is, in fact, capturing the relevant physical phenomena and can be used to make accurate predictions of both wellhead pressure and interface movements.

  15. Kelvin waves in total column ozone

    NASA Technical Reports Server (NTRS)

    Ziemke, J. R.; Stanford, J. L.

    1994-01-01

    Tropical Kelvin waves have been observed previously in ozone mixing ratio data from the SBUV (Solar Backscatter Ultraviolet) and LIMS (Limb Infrared Monitor of the Stratosphere) instruments on board the Nimbus-7 satellite. The present study investigates Kelvin wave features in total column ozone, using version 6 data from the Total Ozone Mapping Spectrometer (TOMS) instrument (also on Nimbus-7). Results show eastward-propagating zonal waves 1-2 with periods approx. 5-15 days, amplitudes approx. 3-5 Dobson Units (1-2% of the time mean), and latitudinal symmetry typical of Kelvin waves. The analyses and a linear model in this study suggest that the primary source of the perturbations is slow Kelvin waves in the lower-to-middle stratosphere. Maximum Kelvin wave signatures occur in conjunction with westward lower-to-middle stratospheric equatorial zonal winds (a quasi-biennial oscillation (QBO) wind modulation effect). The significance of these results is that the TOMS data are shown to be useful for investigations with global coverage of a major component of tropical stratospheric dynamics, Kelvin waves. The TOMS data set with its excellent coverage and high quality should be useful in validating model studies in the relatively data sparse and dynamically difficult tropical region.

  16. Development and validation of an UPLC method for determination of content uniformity in low-dose solid drugs products using the design space approach.

    PubMed

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

    2013-10-15

    A simple and reproducible UPLC method was developed and validated for the quantitative analysis of finasteride in low-dose drug products. Method validation demonstrated the reliability and consistency of analytical results. Due to the regulatory requirements of pharmaceutical analysis in particular, evaluation of robustness is vital to predict how small variations in operating conditions affect the responses. Response surface methodology as an optimization technique was used to evaluate the robustness. For this, a central composite design was implemented around the nominal conditions. Statistical treatment of the responses (retention factor and drug concentrations expressed as percentage of label claim) showed that methanol content in mobile-phase and flow rate were the most influential factors. In the optimization process, the compromise decision support problem (cDSP) strategy was used. Construction of the robust domain from response-surfaces provided tolerance windows for the factors affecting the effectiveness of the method. The specified limits for the USP uniformity of dosage units assay (98.5-101.5%) and the purely experimental variations based on the repeatability test for center points (nominal conditions repetitions) were used as criteria to establish the tolerance windows, which allowed definition design space (DS) of analytical method. Thus, the acceptance criteria values (AV) proposed by the USP-uniformity of assay only depend on the sampling error. If the variation in the responses corresponded to approximately twice the repeatability standard deviation, individual values for percentage label claim (%LC) response may lie outside the specified limits; this implies the data are not centered between the specified limits, and that this term plus the sampling error affects the AV value. To avoid this fact, the limits specified by the Uniformity of Dosage Form assay (i.e., 98.5-101.5%) must be taken into consideration to fix the tolerance windows for each

  17. Validation of a fast liquid chromatography-UV method for the analysis of drugs used in combined cardiovascular therapy in human plasma.

    PubMed

    Iriarte, Gorka; Gonzalez, Oskar; Ferreirós, Nerea; Maguregui, Miren Itxaso; Alonso, Rosa Maria; Jiménez, Rosa Maria

    2009-10-01

    Ultra-performance liquid chromatography (UPLC) was investigated as a faster alternative to high-performance liquid chromatography (HPLC) for the simultaneous analysis of drugs usually prescribed in cardiovascular therapy. Upon a previously developed and validated solid phase extraction (SPE)-HPLC-photodiode array (PDA)-fluorescence (FLR) method, separation of chlorthalidone (CLTD; diuretic), valsartan and its metabolite (VAL and VAL-M1 respectively; angiotensin II receptor antagonist drugs) and fluvastatin (FLUV; statin) was performed in human plasma using an RP C18 column (50mmx2.1mm, 1.7microm, Waters Acquity UPLC (BEH)) and a tunable UV-vis (TUV) detector. After method transfer, different system variables were modulated to study the evolution of responses of the analytes and the endogenous interferences. The improved method was fully validated and the results were compared with its precursor HPLC method relating to analysis time, efficiency and sensitivity. The studied compounds were separated in less than 8min and the method showed good linearity (20-3000microg/L for chlorthalidone, 110-1100microg/L for valsartan-M1, 67-1900microg/L for valsartan and 48-1100microg/L for fluvastatin), precision and accuracy. The proposed method was found to be reproducible (RSD<10%), accurate (RE<15%), robust and suitable for quantitative analysis of the studied drugs in plasma obtained from patients under combined cardiovascular treatment. PMID:19660995

  18. An ultra-pressure liquid chromatography-tandem mass spectrometry method for the simultaneous determination of three physalins in rat plasma and its application to pharmacokinetic study of Physalis alkekengi var. franchetii (Chinese lantern) in rats.

    PubMed

    Zheng, Yunliang; Chen, Yong; Ren, Yiping; Luan, Lianjun; Wu, Yongjiang

    2012-01-25

    An ultra-high pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the quantification of three major ingredients in Chinese lantern preparations (CLP) in rat plasma. Following extraction by ethyl acetate, the analytes were separated on an Acquity UPLC BEH Shield RP C(18) column using a gradient mobile phase system of acetonitrile-water. Electrospray ionization (ESI) tandem interface was employed prior to mass spectrometric detection. The calibration curves were linear over the range of 5.0-500.0 ng/ml for physalin D, 2.3-230.0 ng/ml for physalin G and 0.71-71.0 ng/ml for 4,7-didehydroneophysalin B. The average extraction recoveries, examined at four concentration levels, carried from 57.1% to 76.9%, and the accuracies ranged from 94.0% to 113.3% with precision (RSD) <15%. The validated method was successfully applied to the determination of the three physalins in rat plasma after intragastric administration of CLP suspension.

  19. [Screening and confirmation of 24 hormones in cosmetics by ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry].

    PubMed

    Li, Zhaoyong; Wang, Fengmei; Niu, Zengyuan; Luo, Xin; Zhang, Gang; Chen, Junhui

    2014-05-01

    A method of ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry (UPLC-LTQ/Orbitrap MS) was established to screen and confirm 24 hormones in cosmetics. Various cosmetic samples were extracted with methanol. The extract was loaded onto a Waters ACQUITY UPLC BEH C18 column (50 mm x 2.1 mm, 1.7 microm) using a gradient elution of acetonitrile/water containing 0.1% (v/v) formic acid for the separation. The accurate mass of quasi-molecular ion was acquired by full scanning of electrostatic field orbitrap. The rapid screening was carried out by the accurate mass of quasi-molecular ion. The confirmation analysis for targeted compounds was performed with the retention time and qualitative fragments obtained by data dependent scan mode. Under the optimal conditions, the 24 hormones were routinely detected with mass accuracy error below 3 x 10(-6) (3 ppm), and good linearities were obtained in their respective linear ranges with correlation coefficients higher than 0.99. The LODs (S/N = 3) of the 24 compounds were < or = 10 microg/kg, which can meet the requirements for the actual screening of cosmetic samples. The developed method was applied to screen the hormones in 50 cosmetic samples. The results demonstrate that the method is a useful tool for the rapid screening and identification of the hormones in cosmetics.

  20. Simultaneous determination of shanzhiside methyl ester, 8-O-acetylshan- zhiside methyl ester and luteolin-7-O-β-D-glucopyranoside in rat plasma by ultra performance liquid chromatography-tandem mass spectrometry and its application to a pharmacokinetic study after oral administration of Lamiophlomis rotata Pill.

    PubMed

    Chen, Jing; Wang, Yang; Liang, Xinlei; Sun, Tingting; Luo, Jinghan; Guo, Xingjie; Zhao, Longshan

    2016-05-01

    A rapid, sensitive and specific ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the quantification of shanzhiside methyl ester, 8-O-acetylshanzhiside methyl ester and luteolin-7-O-β-D-glucopyranoside of Lamiophlomis rotata Pill in rat plasma was developed and validated. After liquid-liquid extraction with n-butyl alcohol/ethyl acetate (70:30, v/v), analytes and paeoniflorin (internal standard, IS) were separated on an Acquity BEH UPLC C18 column (100 × 2.1 mm, 1.7 μm) with gradient elution at a flow rate of 0.2 mL/min. All calibration curves had good linearity (r>0.9929) over the concentration ranges of 1-1000 ng/mL for shanzhiside methyl ester and 8-O-acetylshanzhiside methyl ester, 0.3-150 ng/mL for luteolin-7-O-β-D-glucopyranoside. The intra- and inter-day precisions were all within 11.1% and the accuracy (relative error, RE%) all ranged from -13.6% to 5.3%. The method also guaranteed an acceptable selectivity, recovery and stability, which was successfully applied to a pharmacokinetic study of the three analytes in rats after oral administration of Lamiophlomis rotata Pill. PMID:27023158

  1. Determination of rutin in rat plasma by ultra performance liquid chromatography tandem mass spectrometry and application to pharmacokinetic study.

    PubMed

    Chen, Mengchun; Zhang, Xiaoqian; Wang, Hao; Lin, Baoli; Wang, Shuanghu; Hu, Guoxin

    2015-04-01

    A sensitive and rapid ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS-MS) method for the determination of rutin in rat plasma was developed and validated. After addition of tolbutamide as internal standard (IS), protein precipitation by acetonitrile was used as sample preparation. The chromatographic separation was performed on an Acquity UPLC BEH C18 column (2.1 × 50 mm, 1.7 μm particle size), using acetonitrile-0.1% formic acid as the mobile phase with gradient elution, delivered at a flow-rate of 0.4 mL/min. Mass spectrometric analysis was performed using a XEVO TQD mass spectrometer coupled with an electro-spray ionization (ESI) source in the positive ion mode. The MRM transitions of m/z 610.91→302.98 and m/z 271.2→155.1 were used to quantify for rutin and tolbutamide, respectively. This assay method has been fully validated in terms of specificity, linearity, recovery and matrix effect, accuracy, precision and stability. Calibration curves were linear in the concentration ranges of 25-2000 ng/mL for rutin. Only 3 min was needed for an analytical run. This developed method was successfully used for determination of rutin in rat plasma for pharmacokinetic study.

  2. Exploring the Sulfur Nutrient Cycle Using the Winogradsky Column

    ERIC Educational Resources Information Center

    Rogan, Brian; Lemke, Michael; Levandowsky, Michael; Gorrell, Thomas

    2005-01-01

    The Winogradsky column demonstrates how the metabolic diversity of prokaryotes transforms sulfur to different forms with varying redox states and hence, supplies nutrients and/or energy to the organism. The Winogardsky column is an excellent way to show that not all bacteria are pathogens and they have an important role in the geochemical cycling…

  3. An Automated Distillation Column for the Unit Operations Laboratory

    ERIC Educational Resources Information Center

    Perkins, Douglas M.; Bruce, David A.; Gooding, Charles H.; Butler, Justin T.

    2005-01-01

    A batch distillation apparatus has been designed and built for use in the undergraduate unit operations laboratory course. The column is fully automated and is accompanied by data acquisition and control software. A mixture of 1­-propanol and 2-­propanol is separated in the column, using either a constant distillate rate or constant composition…

  4. Stabilization of the Circulation Flow of the Cryogenic Distillation Column

    NASA Astrophysics Data System (ADS)

    Juromskiy, V. M.

    Two-circuit system of automatic stabilization of the hydrodynamics of the cryogenic distillation column is considered. Control system eliminates flooding/depletion of column in long-term mode of operation when the accuracy of stabilization of the circulation flow is better than 1%.

  5. Ultrasonic testing device having an adjustable water column

    SciTech Connect

    Roach, Dennis P.; Neidigk, Stephen O.; Rackow, Kirk A.; Duvall, Randy L.

    2015-09-01

    An ultrasonic testing device having a variable fluid column height is disclosed. An operator is able to adjust the fluid column height in real time during an inspection to to produce optimum ultrasonic focus and separate extraneous, unwanted UT signals from those stemming from the area of interest.

  6. SURFACTANT ENHANCED REMEDIATION OF SOIL COLUMNS CONTAMINATED BY RESIDUAL TETRACHLOROETHYLENE

    EPA Science Inventory

    The ability of aqueous surfactant solutions to recover tetrachloroethylene (PCE) entrapped in Ottawa sand was evaluated in four column experiments. Residual PCE was emplaced by injecting 14C-labeled PCE into water-saturated soil columns and displacing the free product ...

  7. A Better Method for Filling Pasteur Pipet Chromatography Columns

    ERIC Educational Resources Information Center

    Ruekberg, Ben

    2006-01-01

    An alternative method for the preparation of Pasteur pipet chromatography columns is presented that allows the column to be filled with solvent without bubbles and allows greater control of fluid flow while the materials to be separated are added. Students are required to wear gloves and goggles and caution should be used while handling glass…

  8. COLUMN EXPERIMENTS AND ANOMALOUS CONDUCTIVITY IN HYDROCARBON-IMPACTED SOILS

    EPA Science Inventory

    A laboratory experiment was designed to increase the understanding of the geoelectric effects of microbial " degradation of hydrocarbons. Eight large columns were were paired to provide a replicate of each of four experiments. These large-volume columns contained "sterilized" soi...

  9. Measurement of the axial and radial temperature profiles of a chromatographic column. Influence of thermal insulation on column efficiency.

    PubMed

    Gritti, Fabrice; Guiochon, Georges

    2007-01-01

    The temperatures of the metal wall along a chromatographic column (longitudinal temperature gradients) and of the liquid phase across the outlet section of the column (radial temperature gradients) were measured at different flow rates with the same chromatographic column (250 mm x 4.6 mm). The column was packed with 5 microm C18-bonded silica particles. The measurements were carried out with surface and immersion thermocouples (all junction Type T, +/-0.1 K) that measure the local temperature. The column was either left in a still-air bath (ambient temperature, T(ext) = 295-296 K) or insulated in a packing foam to avoid air convection around its surface. The temperature profiles were measured at several values of the inlet pressure (approximately = 100, 200, 300 and 350 bar) and with two mobile phases, pure methanol and a 2.5:97.5 (v/v, %) methanol:water solution. The experimental results show that the longitudinal temperature gradients never exceeded 8 K for a pressure drop of 350 bars. In the presence of the insulating foam, the longitudinal temperature gradients become quasi-linear and the column temperature increases by +1 and +3 K with a water-rich (heat conductivity approximately = 0.6 W/m/K) and pure methanol (heat conductivity approximately = 0.2 W/m/K), respectively. The radial temperature gradients are maximum with methanol (+1.5 K at 290 bar inlet pressure) and minimum with water (+0.8 K at 290 bar), as predicted by the solution of the heat transfer balance in a chromatographic column. The profile remains parabolic all along the column. Combining the results of these measurements (determination of the boundary conditions on the wall, at column inlet and at column outlet) with calculations using a realistic model of heat dispersion in a porous medium, the temperature inside the column could be assessed for any radial and axial position.

  10. HEAT TRANSFER ANALYSIS FOR FIXED CST AND RF COLUMNS

    SciTech Connect

    Lee, S

    2007-10-17

    In support of a small column ion exchange (SCIX) process for the Savannah River Site waste processing program, transient and steady state two-dimensional heat transfer models have been constructed for columns loaded with cesium-saturated crystalline silicotitanate (CST) or spherical Resorcinol-Formaldehyde (RF) beads and 6 molar sodium tank waste supernate. Radiolytic decay of sorbed cesium results in heat generation within the columns. The models consider conductive heat transfer only with no convective cooling and no process flow within the columns (assumed column geometry: 27.375 in ID with a 6.625 in OD center-line cooling pipe). Heat transfer at the column walls was assumed to occur by natural convection cooling with 35 C air. A number of modeling calculations were performed using this computational heat transfer approach. Minimal additional calculations were also conducted to predict temperature increases expected for salt solution processed through columns of various heights at the slowest expected operational flow rate of 5 gpm. Results for the bounding model with no process flow and no active cooling indicate that the time required to reach the boiling point of {approx}130 C for a CST-salt solution mixture containing 257 Ci/liter of Cs-137 heat source (maximum expected loading for SCIX applications) at 35 C initial temperature is about 6 days. Modeling results for a column actively cooled with external wall jackets and the internal coolant pipe (inlet coolant water temperature: 25 C) indicate that the CST column can be maintained non-boiling under these conditions indefinitely. The results also show that the maximum temperature of an RF-salt solution column containing 133 Ci/liter of Cs-137 (maximum expected loading) will never reach boiling under any conditions (maximum predicted temperature without cooling: 88 C). The results indicate that a 6-in cooling pipe at the center of the column provides the most effective cooling mechanism for reducing the

  11. THERMAL MODELING OF ION EXCHANGE COLUMNS WITH SPHERICAL RF RESIN

    SciTech Connect

    Lee, S.; King, W.

    2009-12-30

    Models have been developed to simulate the thermal performance of RF columns fully loaded with radioactive cesium. Temperature distributions and maximum temperatures across the column were calculated during Small Column Ion Exchange (SCIX) process upset conditions with a focus on implementation at Hanford. A two-dimensional computational modeling approach was taken to include conservative, bounding estimates for key parameters such that the results will provide the maximum centerline temperatures achievable under the design configurations using a feed composition known to promote high cesium loading on RF. The current full-scale design for the SCIX system includes a central cooling tube, and one objective of these calculations was to examine its elimination to simplify the design. Results confirmed that a column design without a central cooling tube is feasible for RF, allowing for the possibility of significant design simplifications if it can be assumed that the columns are always filled with liquid. With active cooling through the four outer tubes, the maximum column diameter expected to maintain the temperature below the assumed media and safety limits is 26 inches, which is comparable to the current design diameter. Additional analysis was conducted to predict the maximum column temperatures for the previously unevaluated accident scenario involving inadvertent drainage of liquid from a cesium-saturated column, with retention of the ion exchange media and cesium in the column. As expected, much higher maximum temperatures are observed in this case due to the poor heat transfer properties of air versus liquid. For this hypothetical accident scenario involving inadvertent and complete drainage of liquid from a cesium-saturated column, the modeling results indicate that the maximum temperature within a 28 inch diameter RF column with external cooling is expected to exceed 250 C within 2 days, while the maximum temperature of a 12 inch column is maintained below

  12. Experimental study of wave propagation dynamics of multicomponent distillation columns

    SciTech Connect

    Ting, J.; Helfferich, F.G.; Hwang, Y.L.; Graham, G.K.; Keller, G.E. II

    1999-10-01

    Distillation columns with sharp separations exhibit severely nonlinear behavior, which has been known to cause difficulties in column control and design. Such a column is characterized by sharp composition and temperature variations in the column. Previously, the binary distillation case was thoroughly analyzed using a nonlinear wave theory and such an analysis was experimentally validated. For multicomponent distillation, the complicated nonlinear dynamics of the movement and interference of multiple sharp composition variations can be elucidated with a coherent-wave theory developed earlier for general countercurrent separation processes. With a ternary alcohol mixture, the present study has experimentally verified the theory by demonstrating the existence and propagation of constant-pattern coherent waves in a 50-tray stripping column in response to a step disturbance of feed composition, feed flow rate, or reboiler heat supply. The study has also tested the theory's predictions of composition profile, wave velocities, and asymmetric dynamics.

  13. Experimental study of wave propagation dynamics of binary distillation columns

    SciTech Connect

    Hwang, Y.L.; Graham, G.K.; Keller, G.E. II; Ting, J.; Helfferich, F.G.

    1996-10-01

    High-purity distillation columns are typically difficult to control because of their severely nonlinear behavior reflected by their sharp composition and temperature profiles. The dynamic behavior of such a column, as characterized by the movement of its sharp profile, was elucidated by a nonlinear wave theory established previously. With binary alcohol mixtures, this study provides an experimental observation of such wave-propagation dynamics of a 40-tray stripping column and a 50-tray fractionation column in response to step disturbances of feed composition, feed flow rate, and reboiler heat supply. These experimental results have verified that the sharp profile in a high-purity column moves as a constant-pattern wave and that the nonlinear wave theory predicts its velocity satisfactorily with very simple mathematics. Results also demonstrate the asymmetric dynamics of the transitions between two steady states.

  14. Mitigation of Liquefaction in Sandy Soils Using Stone Columns

    NASA Astrophysics Data System (ADS)

    Selcuk, Levent; Kayabalı, Kamil

    2010-05-01

    Soil liquefaction is one of the leading causes of earthquake-induced damage to structures. Soil improvement methods provide effective solutions to reduce the risk of soil liquefaction. Thus, soil ground treatments are applied using various techniques. However, except for a few ground treatment methods, they generally require a high cost and a lot of time. Especially in order to prevent the risk of soil liquefaction, stone columns conctructed by vibro-systems (vibro-compaction, vibro-replacement) are one of the traditional geotechnical methods. The construction of stone columns not only enhances the ability of clean sand to drain excess pore water during an earthquake, but also increases the relative density of the soil. Thus, this application prevents the development of the excess pore water pressure in sand during earthquakes and keeps the pore pressure ratio below a certain value. This paper presents the stone column methods used against soil liquefaction in detail. At this stage, (a) the performances of the stone columns were investigated in different spacing and diameters of columns during past earthquakes, (b) recent studies about design and field applications of stone columns were presented, and (c) a new design method considering the relative density of soil and the capacity of drenage of columns were explained in sandy soil. Furthermore, with this new method, earthquake performances of the stone columns constructed at different areas were investigated before the 1989 Loma Prieta and the 1994 Northbridge earthquakes, as case histories of field applications, and design charts were compiled for suitable spacing and diameters of stone columns with consideration to the different sandy soil parameters and earhquake conditions. Key Words: Soil improvement, stone column, excess pore water pressure

  15. HEAT TRANSFER ANALYSIS FOR ION-EXCHANGE COLUMN SYSTEM

    SciTech Connect

    Lee, S.; King, W.

    2011-05-23

    Models have been developed to simulate the thermal characteristics of Crystalline Silicotitanate (CST) ion exchange media fully loaded with radioactive cesium in a column configuration and distributed within a waste storage tank. This work was conducted to support the Small Column Ion Exchange (SCIX) program which is focused on processing dissolved, high-sodium salt waste for the removal of specific radionuclides (including Cs-137, Sr-90, and actinides) within a High Level Waste (HLW) storage tank at the Savannah River Site. The SCIX design includes CST columns inserted and supported in the tank top risers for cesium removal. Temperature distributions and maximum temperatures across the column were calculated with a focus on process upset conditions. A two-dimensional computational modeling approach for the in-column ion-exchange domain was taken to include conservative, bounding estimates for key parameters such that the results would provide the maximum centerline temperatures achievable under the design configurations using a feed composition known to promote high cesium loading on CST. The current full-scale design for the CST column includes one central cooling pipe and four outer cooling tubes. Most calculations assumed that the fluid within the column was stagnant (i.e. no buoyancy-induced flow) for a conservative estimate. A primary objective of these calculations was to estimate temperature distributions across packed CST beds immersed in waste supernate or filled with dry air under various accident scenarios. Accident scenarios evaluated included loss of salt solution flow through the bed, inadvertent column drainage, and loss of active cooling in the column. The modeling results demonstrate that the baseline design using one central and four outer cooling tubes provides a highly efficient cooling mechanism for reducing the maximum column temperature.

  16. Novel techniques for slurry bubble column hydrodynamics

    SciTech Connect

    Dudukovic, M.P.

    1999-05-14

    The objective of this cooperative research effort between Washington University, Ohio State University and Exxon Research Engineering Company was to improve the knowledge base for scale-up and operation of slurry bubble column reactors for syngas conversion and other coal conversion processes by increased reliance on experimentally verified hydrodynamic models. During the first year (July 1, 1995--June 30, 1996) of this three year program novel experimental tools (computer aided radioactive particle tracking (CARPT), particle image velocimetry (PIV), heat probe, optical fiber probe and gamma ray tomography) were developed and tuned for measurement of pertinent hydrodynamic quantities, such as velocity field, holdup distribution, heat transfer and bubble size. The accomplishments were delineated in the First Technical Annual Report. The second year (July, 1996--June 30, 1997) was spent on further development and tuning of the novel experimental tools (e.g., development of Monte Carlo calibration for CARPT, optical probe development), building up the hydrodynamic data base using these tools and comparison of the two techniques (PIV and CARPT) for determination of liquid velocities. A phenomenological model for gas and liquid backmixing was also developed. All accomplishments were summarized in the Second Annual Technical Report. During the third and final year of the program (July 1, 1997--June 30, 1998) and during the nine months no cost extension, the high pressure facility was completed and a set of data was taken at high pressure conditions. Both PIV, CT and CARPT were used. More fundamental hydrodynamic modeling was also undertaken and model predictions were compared to data. The accomplishments for this period are summarized in this report.

  17. Statistical heterospectroscopy, an approach to the integrated analysis of NMR and UPLC-MS data sets: application in metabonomic toxicology studies.

    PubMed

    Crockford, Derek J; Holmes, Elaine; Lindon, John C; Plumb, Robert S; Zirah, Severine; Bruce, Stephen J; Rainville, Paul; Stumpf, Chris L; Nicholson, Jeremy K

    2006-01-15

    Statistical heterospectroscopy (SHY) is a new statistical paradigm for the coanalysis of multispectroscopic data sets acquired on multiple samples. This method operates through the analysis of the intrinsic covariance between signal intensities in the same and related molecules measured by different techniques across cohorts of samples. The potential of SHY is illustrated using both 600-MHz 1H NMR and UPLC-TOFMS data obtained from control rat urine samples (n = 54) and from a corresponding hydrazine-treated group (n = 58). We show that direct cross-correlation of spectral parameters, viz. chemical shifts from NMR and m/z data from MS, is readily achievable for a variety of metabolites, which leads to improved efficiency of molecular biomarker identification. In addition to structure, higher level biological information can be obtained on metabolic pathway activity and connectivities by examination of different levels of the NMR to MS correlation and anticorrelation matrixes. The SHY approach is of general applicability to complex mixture analysis, if two or more independent spectroscopic data sets are available for any sample cohort. Biological applications of SHY as demonstrated here show promise as a new systems biology tool for biomarker recovery. PMID:16408915

  18. Chiral PCB 91 and 149 Toxicity Testing in Embryo and Larvae (Danio rerio): Application of Targeted Metabolomics via UPLC-MS/MS

    NASA Astrophysics Data System (ADS)

    Chai, Tingting; Cui, Feng; Yin, Zhiqiang; Yang, Yang; Qiu, Jing; Wang, Chengju

    2016-09-01

    In this study, we aimed to investigate the dysfunction of zebrafish embryos and larvae induced by rac-/(+)-/(‑)- PCB91 and rac-/(‑)-/(+)- PCB149. UPLC-MS/MS (Ultra-performance liquid chromatography coupled with mass spectrometry) was employed to perform targeted metabolomics analysis, including the quantification of 22 amino acids and the semi-quantitation of 22 other metabolites. Stereoselective changes in target metabolites were observed in embryos and larvae after exposure to chiral PCB91 and PCB149, respectively. In addition, statistical analyses, including PCA and PLS-DA, combined with targeted metabolomics were conducted to identify the characteristic metabolites and the affected pathways. Most of the unique metabolites in embryos and larvae after PCB91/149 exposure were amino acids, and the affected pathways for zebrafish in the developmental stage were metabolic pathways. The stereoselective effects of PCB91/149 on the metabolic pathways of zebrafish embryos and larvae suggest that chiral PCB91/149 exposure has stereoselective toxicity on the developmental stages of zebrafish.

  19. Metabolites identification of Huo Luo Xiao Ling Dan in rat urine by UPLC coupled with electrospray ionization time-of-flight mass spectrometry.

    PubMed

    Wang, Fenrong; Wu, Yun; Ai, Yu; Bian, Qiaoxia; Ma, Wen; Lee, David Y-W; Dai, Ronghua

    2016-03-01

    Huo Luo Xiao Ling Dan (HLXLD), a Chinese herbal formula, is used in folk medicine for the treatment of arthritis and other chronic inflammatory diseases. However, the in vivo integrated metabolism of its multiple components remains unknown. In this paper, an ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS) method was developed for detection and identification of HLXLD metabolites in rat urine at high and normal clinical dosages. The prototype constituents and their metabolites in urine were analyzed. The mass measurements were accurate within 8 ppm, and subsequent fragment ions offered higher quality structural information for interpretation of the fragmentation pathways of various compounds. A total of 85 compounds were detected in high dosages urine samples by a highly sensitive extracted ion chromatograms method, including 31 parent compounds and 54 metabolites. Our results indicated that phase 2 reactions (e.g. glucuronidation, glutathionidation and sulfation) were the main metabolic pathways of lactones, alkaloids and flavones, while phase I reactions (e.g. hydrogenation and hydroxylation) were the major metabolic reaction for coumarins, paeoniflorin and iridoids. This investigation provided important structural information on the metabolism of HLXLD and provided scientific evidence to obtain a more comprehensive metabolic profile.

  20. UPLC-HRMS based metabolomics reveals the sphingolipids with long fatty chains and olefinic bonds up-regulated in metabolic pathway for hypoxia preconditioning.

    PubMed

    Zhou, Tao; Wang, Mingming; Cheng, Haiting; Cui, Can; Su, Su; Xu, Pingxiang; Xue, Ming

    2015-12-01

    Hypoxia preconditioning (HPC) could protect cells, tissues, organs and systems from hypoxia injury, but the molecular mechanism still remained unclear. The ultra-high performance liquid chromatography coupled high resolution mass spectrometry (UPLC-HRMS) based metabolomics method was utilized to explore the key endogenous metabolites and metabolic pathways related to HPC. Our results clearly showed that the HPC mice model was established and refined, suggesting that there were significant differences between the control group and 6 × HPC group at the molecular levels. A serious of statistical analyses, including univariate analysis and multivariate analysis, were performed by the Progenesis QI software package and MetaboAnalyst web-server. The sphingolipid metabolic pathways were noticed due to the low p-value and high pathway impact calculated by the MetaboAnalyst and the pathways were altered under HPC condition. Especially, the sphingolipid compound sphingomyelin, ceramide, glucosylceramide, galactosylceramide and lactosylceramide were mapping in this metabolic pathway. Interestingly, these sphingolipid metabolites with olefinic bond in the long fatty chain were up-regulated, while those sphingolipids without olefinic bond were down-regulated. The results indicated that C24:1-Cers played a critical role in HPC and had potential in endogenous protective mechanism. Our data provided an insight to further reveal the protection mechanism of HPC. PMID:26433137

  1. HPLC-PDA method for quinovic acid glycosides assay in Cat's claw (Uncaria tomentosa) associated with UPLC/Q-TOF-MS analysis.

    PubMed

    Pavei, Cabral; Kaiser, Samuel; Verza, Simone Gasparin; Borre, Gustavo Luis; Ortega, George Gonzalez

    2012-03-25

    Uncaria tomentosa (Willd.) is a medicinal plant largely used in folk medicine due to its wide range of biological activities, many of which are usually ascribed to the two main classes of secondary metabolites, namely, alkaloids and quinovic acid glycosides. In this work, a reversed phase HPLC-PDA method was developed and validated for the assay of quinovic acid glycosides in crude and dried extracts of Uncaria tomentosa (Cat's claw) bark. The validation comprised tests of specificity, accuracy, linearity, intermediate precision, repeatability and limits of detection and of quantification. Alpha-hederin was used as the external standard. High coefficients of determination with lower R.S.D. were achieved for both external standard and crude extract. The structural characterization of the main quinovic acid glycosides presented in the crude extract was carried out through UPLC/Q-TOF-MS. The identities of the compounds were obtained through the comparison of their fragmentation patterns with those reported in the literature. The analytical method was successfully applied for quantifying quinovic acid glycosides in two different dried extracts from U. tomentosa and in one quinovic acid glycosides purified fraction.

  2. A pre-classification strategy based on UPLC-Triple-TOF/MS for metabolic screening and identification of Radix glehniae in rats.

    PubMed

    Wang, Shuang; Qi, Pengcheng; Zhou, Na; Zhao, Minmin; Ding, Weijing; Li, Song; Liu, Minyan; Wang, Qiao; Jin, Shumin

    2016-10-01

    Traditional Chinese Medicines (TCMs) have gained increasing popularity in modern society. However, the profiles of TCMs in vivo are still unclear owing to their complexity and low level in vivo. In this study, UPLC-Triple-TOF techniques were employed for data acquiring, and a novel pre-classification strategy was developed to rapidly and systematically screen and identify the absorbed constituents and metabolites of TCMs in vivo using Radix glehniae as the research object. In this strategy, pre-classification for absorbed constituents was first performed according to the similarity of their structures. Then representative constituents were elected from every class and analyzed separately to screen non-target absorbed constituents and metabolites in biosamples. This pre-classification strategy is basing on target (known) constituents to screen non-target (unknown) constituents from the massive data acquired by mass spectrometry. Finally, the screened candidate compounds were interpreted and identified based on a predicted metabolic pathway, well - studied fragmentation rules, a predicted metabolic pathway, polarity and retention time of the compounds, and some related literature. With this method, a total of 111 absorbed constituents and metabolites of Radix glehniae in rats' urine, plasma, and bile samples were screened and identified or tentatively characterized successfully. This strategy provides an idea for the screening and identification of the metabolites of other TCMs. PMID:27592348

  3. Evaluation of the Effects of Ketoconazole and Voriconazole on the Pharmacokinetics of Oxcarbazepine and Its Main Metabolite MHD in Rats by UPLC-MS-MS.

    PubMed

    Chen, Xinxin; Gu, Ermin; Wang, Shuanghu; Zheng, Xiang; Chen, Mengchun; Wang, Li; Hu, Guoxin; Cai, Jian-ping; Zhou, Hongyu

    2016-03-01

    Oxcarbazepine (OXC), a second-generation antiepileptic drug, undergoes rapid reduction with formation of the active metabolite 10,11-dihydro-10-hydroxy-carbazepine (MHD) in vivo. In this study, a method for simultaneous determination of OXC and MHD in rat plasma using ultra-performance liquid chromatography with tandem mass spectrometry (UPLC-MS-MS) was developed and validated. Under given chromatographic conditions, OXC, MHD and internal standard diazepam were separated well and quantified by electrospray positive ionization mass spectrometry in the multiple reaction monitoring transitions mode. The method validation demonstrated good linearity over the range of 10-2,000 ng/mL for OXC and 5-1,000 ng/mL for MHD. The lower limit of quantification was 5 ng/mL for OXC and 2.5 ng/mL for MHD, respectively. The method was successfully applied to the evaluation of the pharmacokinetics of OXC and MHD in rats, with or without pretreatment by ketoconazole (KET) and voriconazole (VOR). Statistics indicated that KET and VOR significantly affected the disposition of OXC and MHD in vivo, whereas VOR predominantly interfered with the disposition of MHD. This method is suitable for pharmacokinetic study in small animals. PMID:26499119

  4. Analysis of the Enantioselective Effects of PCB95 in Zebrafish (Danio rerio) Embryos through Targeted Metabolomics by UPLC-MS/MS

    PubMed Central

    Xu, Nana; Mu, Pengqian; Yin, Zhiqiang; Jia, Qi; Yang, Shuming; Qian, Yongzhong; Qiu, Jing

    2016-01-01

    As persistent organic pollutants, polychlorinated biphenyls (PCBs) accumulate in the bodies of animals and humans, resulting in toxic effects on the reproductive, immune, nervous, and endocrine systems. The biological and toxicological characteristics of enantiomers of chiral PCBs may differ, but these enantioselective effects of PCBs have not been fully characterized. In this study, we performed metabolomics analysis, using ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) to investigate the enantioselective toxic effects of PCB95 in zebrafish (Danio rerio) embryos after exposure to three dose levels of 0.1, 1, and 10 μg/L for 72 h. Multivariate analysis directly reflected the metabolic perturbations caused by PCB95. The effects of (-)-PCB95 and (+)-PCB95 were more prominent than those of the racemate in zebrafish embryos. A total of 26 endogenous metabolites were selected as potential marker metabolites with variable importance at projection values larger than 1 and significant differences (p<0.05). These metabolites included amino acids, organic acids, nucleosides, betaine, and choline. The changes in these biomarkers were dependent on the enantiomer-specific structures of PCB95. Fifteen metabolic pathways were significantly affected, and several nervous and immune system-related metabolites were significantly validated after exposure. These metabolic changes indicated that the toxic effects of PCB95 may be associated with the interaction of PCB95 with the nervous and immune systems, thus resulting in disruption of energy metabolism and liver function. PMID:27500732

  5. The Effect of Temperature on Pressurised Hot Water Extraction of Pharmacologically Important Metabolites as Analysed by UPLC-qTOF-MS and PCA

    PubMed Central

    Khoza, B. S.; Chimuka, L.; Mukwevho, E.; Steenkamp, P. A.; Madala, N. E.

    2014-01-01

    Metabolite extraction methods have been shown to be a critical consideration for pharmacometabolomics studies and, as such, optimization and development of new extraction methods are crucial. In the current study, an organic solvent-free method, namely, pressurised hot water extraction (PHWE), was used to extract pharmacologically important metabolites from dried Moringa oleifera leaves. Here, the temperature of the extraction solvent (pure water) was altered while keeping other factors constant using a homemade PHWE system. Samples extracted at different temperatures (50, 100, and 150°C) were assayed for antioxidant activities and the effect of the temperature on the extraction process was evaluated. The samples were further analysed by mass spectrometry to elucidate their metabolite compositions. Principal component analysis (PCA) evaluation of the UPLC-MS data showed distinctive differential metabolite patterns. Here, temperature changes during PHWE were shown to affect the levels of metabolites with known pharmacological activities, such as chlorogenic acids and flavonoids. Our overall findings suggest that, if not well optimised, the extraction temperature could compromise the “pharmacological potency” of the extracts. The use of MS in combination with PCA was furthermore shown to be an excellent approach to evaluate the quality and content of pharmacologically important extracts. PMID:25371697

  6. High-throughput screening of inhibitory effects of Bo-yang-hwan-o-tang on human cytochrome P450 isoforms in vitro using UPLC/MS/MS.

    PubMed

    Lee, Miran; Park, Jeonghyeon; Lim, Mi-sun; Seong, Sook Jin; Lee, Joomi; Seo, Jeong Ju; Park, Yong-Ki; Lee, Hae Won; Yoon, Young-Ran

    2012-01-01

    Bo-yang-hwan-o-tang (BHT) is an oriental herbal medicine for treating brain disorders such as cerebral ischemia. The objective of this study was to develop an economically feasible and time-saving high-throughput screening method to monitor the potential inhibitory effects of BHT on human cytochrome P450 (CYP) enzymes in vitro. Two cocktail sets were used for incubation of human liver microsomes: Cocktail A: 6 probe substrates for CYP1A2, CYP2A6, CYP2C8, CYP2C19, CYP2D6, CYP3A4; Cocktail B: 3 for CYP2B6, CYP2C9, CYP2E1. The concentrations of the substrate metabolites were simultaneously analyzed using UPLC/MS/MS. The BHT extract had almost negligible inhibitory effects on the nine human CYP isoforms tested, with the half-maximal inhibitory concentration value ranged from 3624.99 to 45412.44 μg/ml. The results suggest that BHT extract has no inhibitory effects on CYP isoforms within the clinically recommended dosage range. We conclude that BHT might be free of drug-herb interactions when co-administered with other medicines. However, more in vivo human studies are needed to confirm these results. The high-throughput screening method can be a useful tool for drug discovery and for understanding drug interactions. PMID:23232241

  7. HILIC-UPLC-MS/MS combined with hierarchical clustering analysis to rapidly analyze and evaluate nucleobases and nucleosides in Ginkgo biloba leaves.

    PubMed

    Yao, Xin; Zhou, Guisheng; Tang, Yuping; Guo, Sheng; Qian, Dawei; Duan, Jin-Ao

    2015-02-01

    Ginkgo biloba leaf extract has been widely used in dietary supplements and more recently in some foods and beverages. In addition to the well-known flavonol glycosides and terpene lactones, G. biloba leaves are also rich in nucleobases and nucleosides. To determine the content of nucleobases and nucleosides in G. biloba leaves at trace levels, a reliable method has been established by using hydrophilic interaction ultra performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (HILIC-UPLC-TQ-MS/MS) working in multiple reaction monitoring mode. Eleven nucleobases and nucleosides were simultaneously determined in seven min. The proposed method was fully validated in terms of linearity, sensitivity, and repeatability, as well as recovery. Furthermore, hierarchical clustering analysis (HCA) was performed to evaluate and classify the samples according to the contents of the eleven chemical constituents. The established approach could be helpful for evaluation of the potential values as dietary supplements and the quality control of G. biloba leaves, which might also be utilized for the investigation of other medicinal herbs containing nucleobases and nucleosides.

  8. Spectrum-Effect Relationships Between Chemical Fingerprints and Antibacterial Effects of Lonicerae Japonicae Flos and Lonicerae Flos Base on UPLC and Microcalorimetry

    PubMed Central

    Shi, Zhilong; Liu, Zhenjie; Liu, Chunsheng; Wu, Mingquan; Su, Haibin; Ma, Xiao; Zang, Yimei; Wang, Jiabo; Zhao, Yanling; Xiao, Xiaohe

    2016-01-01

    The traditional Chinese medicines Lonicerae Japonicae Flos (LJF, Jinyinhua in Chinese) and Lonicerae Flos (LF, Shanyinhua in Chinese) refer to the flower buds of five plants belonging to the Caprifoliaceae family. Until 2000, all of these were officially listed as a single item, LJF (Jinyinhua), in the Chinese Pharmacopoeia. However, there have recently been many academic controversies concerning the separation and combination of LJF and LF in administrative regulation. Till now there has been little work completed evaluating the relationships between biological activity and chemical properties among these drugs. Microcalorimetry and UPLC were used along with principal component analysis (PCA), hierarchical cluster analysis (HCA), and canonical correlation analysis (CCA) to investigate the relationships between the chemical ingredients and the antibacterial effects of LJF and LF. Using multivariate statistical analysis, LJF and LF could be initially separated according to their chemical fingerprints, and the antibacterial effects of the two herbal drugs were divided into two clusters. This result supports the disaggregation of LJF and LF by the Pharmacopoeia Committee. However, the sample of Lonicera fulvotomentosa Hsu et S. C. Cheng turned out to be an intermediate species, with similar antibacterial efficacy as LJF. The results of CCA indicated that chlorogenic acid and 3,4-Dicaffeoylquinic acid were the major components generating antibacterial effects. Furthermore, 3,4-Dicaffeoylquinic acid could be used as a new marker ingredient for quality control of LJF and LF. PMID:26869929

  9. CYP450 phenotyping and metabolite identification of quinine by accurate mass UPLC-MS analysis: a possible metabolic link to blackwater fever

    PubMed Central

    2013-01-01

    Background The naturally occurring alkaloid drug, quinine is commonly used for the treatment of severe malaria. Despite centuries of use, its metabolism is still not fully understood, and may play a role in the haemolytic disorders associated with the drug. Methods Incubations of quinine with CYPs 1A2, 2C9, 2C19, 2D6, and 3A4 were conducted, and the metabolites were characterized by accurate mass UPLC-MSE analysis. Reactive oxygen species generation was also measured in human erythrocytes incubated in the presence of quinine with and without microsomes. Results The metabolites 3-hydroxyquinine, 2’-oxoquininone, and O-desmethylquinine were observed after incubation with CYPs 3A4 (3-hydroxyquinine and 2’-oxoquininone) and 2D6 (O-desmethylquinine). In addition, multiple hydroxylations were observed both on the quinoline core and the quinuclidine ring system. Of the five primary abundance CYPs tested, 3A4, 2D6, 2C9, and 2C19 all demonstrated activity toward quinine, while 1A2 did not. Further, quinine produced robust dose-dependent oxidative stress in human erythrocytes in the presence of microsomes. Conclusions Taken in context, these data suggest a CYP-mediated link between quinine metabolism and the poorly understood haemolytic condition known as blackwater fever, often associated with quinine ingestion. PMID:23800033

  10. Removal of malathion from aqueous solution using De-Acidite FF-IP resin and determination by UPLC-MS/MS: equilibrium, kinetics and thermodynamics studies.

    PubMed

    Naushad, Mu; Alothman, Z A; Khan, M R

    2013-10-15

    In the present study, De-Acidite FF-IP resin was used to remove a highly toxic and persistent organophosphorus pesticide (malathion) from the aqueous solution. Batch experiments were performed as a function of various experimental parameters such as effect of pH (2-10), contact time (10-120 min), resin dose (0.05-0.5 g), initial malathion concentration (0.5-2.5 µg mL(-1)) and temperature (25-65°C). The concentration of malathion was determined using a sensitive, selective and rapid ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method. The uptake rate of malathion on De-Acidite FF-IP resin was rapid and equilibrium established within 40 min. Kinetics studies showed better applicability for pseudo-second-order model. The equilibrium data was fitted to Langmuir and Freundlich isotherm models and the isotherm constants were calculated for malathion. The values of thermodynamic parameters (ΔG(0), ΔH(0) and ΔS(0)) were computed from the Van't Hoff plot of lnKC vs. 1/T which showed that the adsorption of malathion was feasible, endothermic and spontaneous. The regeneration studies were carried out which demonstrated a decrease in the recovery of malathion from 95% to 68% after five consecutive cycles. Breakthrough and exhaustive capacities of malathion were found to be 1.25 mg g(-1) and 3.5 mg g(-1), respectively.

  11. Comparative characterization of nucleotides, nucleosides and nucleobases in Abelmoschus manihot roots, stems, leaves and flowers during different growth periods by UPLC-TQ-MS/MS.

    PubMed

    Du, Le-yue; Qian, Da-wei; Jiang, Shu; Shang, Er-xin; Guo, Jian-ming; Liu, Pei; Su, Shu-lan; Duan, Jin-ao; Zhao, Min

    2015-12-01

    Nucleotides, nucleosides and nucleobases have been proven as important bioactive compounds related to many physiological processes. Abelmoschus manihot (L.) Medicus from the family of Malvaceae is an annual herbal plant of folk medicine widely distributed in Oceania and Asia. However, up to now, no detailed information could be available for the types and contents of nucleotides, nucleosides and nucleobases contained in A. manihot roots, stems, leaves as well as the flowers. In the present study, an UPLC-TQ-MS/MS method was established for detection of the twelve nucleotides, nucleosides and nucleobases. The validated method was successfully applied to identify the 12 analytes in different parts of A. manihot harvested at ten growth periods. 2'-deoxyinosine was not detected in all of the A. manihot samples. The data demonstrated that the distribution and concentration of the 12 compounds in A. manihot four parts were arranged in a decreasing order as leaf>flower>stem>root. Based on the results, the leaves and flowers of A. manihot could be developed as health products possessed nutraceutical and bioactive properties in the future. This method might also be utilized for the quality control of the A. manihot leaves and other herbal medicines being rich in nucleotides, nucleosides and nulecobases.

  12. Quantitative evaluation of berberine subcellular distribution and cellular accumulation in non-small cell lung cancer cells by UPLC-MS/MS.

    PubMed

    Yuan, Zhong-Wen; Leung, Elaine Lai-Han; Fan, Xing-Xing; Zhou, Hua; Ma, Wen-Zhe; Liu, Liang; Xie, Ying

    2015-11-01

    Berberine, an isoquinoline alkaloid, has been demonstrated to be a safe anti-cancer agent with multiple effects on mitochondria. Intracellular concentration and distribution around the targeting sites are determinants of efficacy, but subcellular distribution of berberine has not been fully elucidated yet, which relies on the sensitive and robustness assay. In this study, a sensitive and robust UPLC-MS/MS method has been developed and validated with optimized extraction solvents and detection conditions. Key factors such as the purity and integrity of isolated organelle fractions, and the effects of isolation procedures on the subcellular concentration of berberine were systemically evaluated. With the developed assay, we found that the intracellular accumulations of berberine in two gefitinib resistant NSCLC cell lines H1650 and H1975 were 2-3 folds higher than that of normal epithelial cells BEAS-2B. Moreover, significantly different subcellular distribution profiles in NSCLC cancer cells from that of BEAS-2B cells with a striking increase in content in most organelles may contribute to its selective cytotoxicity to cancer cells. Furthermore, a predominant accumulation of berberine was observed for the first time in microsomal fraction for all three cell lines. Therefore, this method could be used for quantitative evaluation of subcellular distribution and cellular accumulation of berberine and for further evaluation of the concentration-effects relationship.

  13. A highly sensitive quantification method for the accumulation of alarmone ppGpp in Arabidopsis thaliana using UPLC-ESI-qMS/MS.

    PubMed

    Ihara, Yuta; Ohta, Hiroyuki; Masuda, Shinji

    2015-05-01

    Recently, a bacterial second messenger, guanosine 5'-diphosphate 3'-diphosphate (ppGpp), has been detected in chloroplasts. However, because ppGpp concentration in plants is much lower than that in bacteria, detailed analysis of ppGpp in plants has not been performed. A highly sensitive quantification method is required for further characterization of ppGpp function in chloroplasts. Here, we report a new method that allows for the highly sensitive and selective high-throughput quantification of ppGpp by ultra-performance liquid chromatography (UPLC) coupled with a tandem quadrupole mass spectrometer (qMS/MS) equipped with an electrospray interface (ESI). This method requires only ~100 mg of plant tissue for ppGpp quantification. We used this method to measure ppGpp levels in Arabidopsis thaliana under different light conditions. A. thaliana accumulated ppGpp during dark periods. This method will be helpful to further characterize the stringent response in higher plants.

  14. Chiral PCB 91 and 149 Toxicity Testing in Embryo and Larvae (Danio rerio): Application of Targeted Metabolomics via UPLC-MS/MS

    PubMed Central

    Chai, Tingting; Cui, Feng; Yin, Zhiqiang; Yang, Yang; Qiu, Jing; Wang, Chengju

    2016-01-01

    In this study, we aimed to investigate the dysfunction of zebrafish embryos and larvae induced by rac-/(+)-/(−)- PCB91 and rac-/(−)-/(+)- PCB149. UPLC-MS/MS (Ultra-performance liquid chromatography coupled with mass spectrometry) was employed to perform targeted metabolomics analysis, including the quantification of 22 amino acids and the semi-quantitation of 22 other metabolites. Stereoselective changes in target metabolites were observed in embryos and larvae after exposure to chiral PCB91 and PCB149, respectively. In addition, statistical analyses, including PCA and PLS-DA, combined with targeted metabolomics were conducted to identify the characteristic metabolites and the affected pathways. Most of the unique metabolites in embryos and larvae after PCB91/149 exposure were amino acids, and the affected pathways for zebrafish in the developmental stage were metabolic pathways. The stereoselective effects of PCB91/149 on the metabolic pathways of zebrafish embryos and larvae suggest that chiral PCB91/149 exposure has stereoselective toxicity on the developmental stages of zebrafish. PMID:27629264

  15. Analysis of the Enantioselective Effects of PCB95 in Zebrafish (Danio rerio) Embryos through Targeted Metabolomics by UPLC-MS/MS.

    PubMed

    Xu, Nana; Mu, Pengqian; Yin, Zhiqiang; Jia, Qi; Yang, Shuming; Qian, Yongzhong; Qiu, Jing

    2016-01-01

    As persistent organic pollutants, polychlorinated biphenyls (PCBs) accumulate in the bodies of animals and humans, resulting in toxic effects on the reproductive, immune, nervous, and endocrine systems. The biological and toxicological characteristics of enantiomers of chiral PCBs may differ, but these enantioselective effects of PCBs have not been fully characterized. In this study, we performed metabolomics analysis, using ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) to investigate the enantioselective toxic effects of PCB95 in zebrafish (Danio rerio) embryos after exposure to three dose levels of 0.1, 1, and 10 μg/L for 72 h. Multivariate analysis directly reflected the metabolic perturbations caused by PCB95. The effects of (-)-PCB95 and (+)-PCB95 were more prominent than those of the racemate in zebrafish embryos. A total of 26 endogenous metabolites were selected as potential marker metabolites with variable importance at projection values larger than 1 and significant differences (p<0.05). These metabolites included amino acids, organic acids, nucleosides, betaine, and choline. The changes in these biomarkers were dependent on the enantiomer-specific structures of PCB95. Fifteen metabolic pathways were significantly affected, and several nervous and immune system-related metabolites were significantly validated after exposure. These metabolic changes indicated that the toxic effects of PCB95 may be associated with the interaction of PCB95 with the nervous and immune systems, thus resulting in disruption of energy metabolism and liver function. PMID:27500732

  16. Search for over 2000 current and legacy micropollutants on a wastewater infiltration site with a UPLC-high resolution MS target screening method.

    PubMed

    Wode, Florian; van Baar, Patricia; Dünnbier, Uwe; Hecht, Fabian; Taute, Thomas; Jekel, Martin; Reemtsma, Thorsten

    2015-02-01

    A target screening method using ultra high performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS) was developed. The method was applied to 14 groundwater and 11 surface water samples of a former wastewater infiltration site, where raw wastewater was applied until 1985 and treated wastewater is applied since 2005. The measured data are compared with mass spectrometric data of over 2000 organic micropollutants (OMPs), including pharmaceuticals, personal care products, pesticides, industrial chemicals and metabolites of these classes. A total number of 151 and 159 OMPs were detected in groundwater and surface water, respectively, of which 12 have not been reported before in these matrices. Among these 12 compounds were 11 pharmaceuticals and one personal care product. The identity of 55 of the detected OMPs (35%) was verified by analysis of standard compounds. Based on the distribution in the study area, two groups of OMPs were clearly distinguished: current OMPs introduced with treated municipal wastewater since 2005 and legacy OMPs originating from infiltration of untreated wastewater until 1985. A third group included OMPs contained in historic as well as in current wastewater. During infiltration, OMPs with molecular mass >500 g/mol and log DOW > 3.9 were preferentially removed. Speciation had a strong impact with cationic OMPs showing high, neutral OMPs medium and anionic OMPs lowest elimination during infiltration. This target screening method proved useful to study a wide range of compounds, even in retrospect and at sites with poorly documented history and with a complex and variable hydrological situation. PMID:25497426

  17. A reversed-phase capillary ultra-performance liquid chromatography-mass spectrometry (UPLC-MS) method for comprehensive top-down/bottom-up lipid profiling

    PubMed Central

    Gao, Xiaoli; Zhang, Qibin; Meng, Da; Issac, Giorgis; Zhao, Rui; Fillmore, Thomas L.; Chu, Rosey K.; Zhou, Jianying; Tang, Keqi; Hu, Zeping; Moore, Ronald J.; Smith, Richard D.; Katze, Michael G.; Metz, Thomas O.

    2012-01-01

    Lipidomics is a critical part of metabolomics and aims to study all the lipids within a living system. We present here the development and evaluation of a sensitive capillary UPLC-MS method for comprehensive top-down/bottom-up lipid profiling. Three different stationary phases were evaluated in terms of peak capacity, linearity, reproducibility, and limit of quantification (LOQ) using a mixture of lipid standards representative of the lipidome. The relative standard deviations of the retention times and peak abundances of the lipid standards were 0.29% and 7.7%, respectively, when using the optimized method. The linearity was acceptable at >0.99 over 3 orders of magnitude, and the LOQs were sub-fmol. To demonstrate the performance of the method in the analysis of complex samples, we analyzed lipids extracted from a human cell line, rat plasma, and a model human skin tissue, identifying 446, 444, and 370 unique lipids, respectively. Overall, the method provided either higher coverage of the lipidome, greater measurement sensitivity, or both, when compared to other approaches of global, untargeted lipid profiling based on chromatography coupled with MS. PMID:22354571

  18. Comparative characterization of nucleotides, nucleosides and nucleobases in Abelmoschus manihot roots, stems, leaves and flowers during different growth periods by UPLC-TQ-MS/MS.

    PubMed

    Du, Le-yue; Qian, Da-wei; Jiang, Shu; Shang, Er-xin; Guo, Jian-ming; Liu, Pei; Su, Shu-lan; Duan, Jin-ao; Zhao, Min

    2015-12-01

    Nucleotides, nucleosides and nucleobases have been proven as important bioactive compounds related to many physiological processes. Abelmoschus manihot (L.) Medicus from the family of Malvaceae is an annual herbal plant of folk medicine widely distributed in Oceania and Asia. However, up to now, no detailed information could be available for the types and contents of nucleotides, nucleosides and nucleobases contained in A. manihot roots, stems, leaves as well as the flowers. In the present study, an UPLC-TQ-MS/MS method was established for detection of the twelve nucleotides, nucleosides and nucleobases. The validated method was successfully applied to identify the 12 analytes in different parts of A. manihot harvested at ten growth periods. 2'-deoxyinosine was not detected in all of the A. manihot samples. The data demonstrated that the distribution and concentration of the 12 compounds in A. manihot four parts were arranged in a decreasing order as leaf>flower>stem>root. Based on the results, the leaves and flowers of A. manihot could be developed as health products possessed nutraceutical and bioactive properties in the future. This method might also be utilized for the quality control of the A. manihot leaves and other herbal medicines being rich in nucleotides, nucleosides and nulecobases. PMID:26551204

  19. Metabolite profiling in 18 Saudi date palm fruit cultivars and their antioxidant potential via UPLC-qTOF-MS and multivariate data analyses.

    PubMed

    Farag, Mohamed A; Handoussa, Heba; Fekry, Mostafa I; Wessjohann, Ludger A

    2016-02-01

    Date palm fruit (Phoenix dactylifera) is not only one of the most economically significant plants in the Middle East, but also valued for its nutritional impact, and for which development of analytical methods is ongoing to help distinguish its many cultivars. This study attempts to characterize the primary and secondary metabolite profiles of 18 date cultivars from Saudi Arabia. A total of 44 metabolites extracted from the fruit peel were evaluated in a UPLC-qTOF-MS based metabolomics analysis including flavonoids, phenolic acids and fatty acids. The predominant flavones were glycosides of luteolin and chrysoeriol, as well as quercetin conjugates, whereas caffeoyl shikimic acid was the main hydroxycinnamic acid conjugate. GC-MS was further utilized to identify the primary metabolites in fruits (i.e. sugars) with glucose and fructose accounting for up to 95% of TIC among most cultivars. PCA and OPLS analyses revealed that flavone versus flavonol distribution in fruit were the main contributors for cultivar segregation. The antioxidant activity of date fruit samples was correlated with their total phenolics as determined by DPPH and CUPRAC assays. Dkheni Saudi and Shalabi Madina cultivars, appearing as the most distant in clustering analyses exhibited the strongest antioxidant effect suggesting that multivariate data analysis could help determine which date cultivars ought to be prioritized for future agricultural development. PMID:26781334

  20. Identification of Iridoids in Edible Honeysuckle Berries (Lonicera caerulea L. var. kamtschatica Sevast.) by UPLC-ESI-qTOF-MS/MS.

    PubMed

    Kucharska, Alicja Z; Fecka, Izabela

    2016-09-01

    Iridoid profiles of honeysuckle berry were studied. Compounds were identified by ultra-performance liquid chromatography coupled with electrospray ionization mass spectrometry UPLC-ESI-qTOF-MS/MS in positive and negative ions mode. The MS fragmentation pathways of detected iridoid glycosides were also studied in both modes. In the negative ESI mass spectra, iridoids with a methyl ester or lactone structure have preferentially produced adduct [M + HCOOH - H](-) ions. However, protonated ions of molecular fragments, which were released by glycosidic bond cleavage and following fragmentation of aglycone rings, were more usable for iridoid structure analysis. In addition, the neutral losses of H₂O, CO, CO₂, CH₃OH, acetylene, ethenone and cyclopropynone have provided data confirming the presence of functional substituents in the aglycone. Among the 13 iridoids, 11 were identified in honeysuckle berries for the first time: pentosides of loganic acid (two isomers), pentosides of loganin (three isomers), pentosyl sweroside, and additionally 7-epi-loganic acid, 7-epi-loganin, sweroside, secologanin, and secoxyloganin. The five pentoside derivatives of loganic acid and loganin have not been previously detected in the analyzed species. Honeysuckle berries are a source of iridoids with different structures, compounds that are rarely present in fruits.