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Spiked Samples (spiked + sample)
Selected AbstractsAnalysis of aristolochic acids by CE-MS with carboxymethyl chitosan-coated capillaryELECTROPHORESIS, Issue 10 2009Xiaofang Fu Abstract A CE-MS method for rapid determination of aristolochic acid-I and aristolochic acid-II (AA-II) in traditional Chinese medicines and biological samples was described in the present paper. AA-I and AA-II can be baseline separated within 6,min by CE-MS with carboxymethyl-chitosan-coated capillary. CZE conditions including pH, concentration of buffer, applied voltage, and capillary temperature were systematically investigated, and the composition and flow rate of sheath liquid were also optimized for CE-MS. Furthermore, the CE-UV method without any additives in BGE solution was established and compared with the CE-MS method. The results showed that the two methods could achieve satisfactory separation efficiency, repeatability, and linearity, while the LOD was 0.6,,g/mL for CE-UV and 0.05,,g/mL for CE-MS. Compared with the CE-UV method, the sensitivity of CE-MS was significantly improved, in addition to the structure information provided by MS detection at the same time. As an application example, a spiked sample in human serum was analyzed by the CE-MS method, indicating that the new CE-MS method can be applied to analyze AAs in biological samples. [source] Solid-phase microextraction for the determination of benzoylureas in orange juice using liquid chromatography combined with post-column photochemically induced fluorimetry derivatization and fluorescence detectionJOURNAL OF SEPARATION SCIENCE, JSS, Issue 1 2008Piedad Parrilla Vázquez Abstract A solid-phase microextraction (SPME) method has been developed for the determination of six benzoylureas (diflubenzuron, triflumuron, hexaflumuron, teflubenzuron, lufenuron, and flufenoxuron) in natural orange juice based on the direct immersion mode of a 60 ,m polydimethylsiloxane/divinylbenzene fiber. An orange juice was obtained from blended, homogenized, and diluted ecological natural orange juice samples. An aliquot of 3 mL of a spiked sample was extracted under optimum SPME conditions. The determination of benzoylureas was carried out using HPLC combined with post-column photochemically induced fluorimetry derivatization and fluorescence detection. The limits of quantification obtained in matrix were within the range of 0.02 to 0.04 mg/kg and these limits are lower than the maximum residue levels established in Spanish regulations for all pesticides in this study. Recoveries in juice samples ranged between 85 and 110% and relative standard deviations between 1.8 and 7.4%. [source] New supported liquid membrane-capillary electrophoresis in-line arrangement for direct selective analysis of complex samplesELECTROPHORESIS, Issue 15 2006Leonor Nozal Abstract An in-line coupling of a micro-membrane extraction unit, based on supported liquid membrane, with commercially available capillary electrophoresis equipment is described. A main characteristic of this micro-membrane device, made from a simple Eppendorf tube, is that it permits the application of voltage in the acceptor solution to be applied during the extraction process. This has been shown as an alternative to enhance sensitivity, as the analytical signal achieved by applying 10,kV for 20,min was similar to that obtained without the application of voltage and with extraction time of 60,min. In addition, the design has been made permitting both in-line hydrodynamic and electrokinetic sample introduction into the electrophoretic capillary. The analytical potential of the proposed system has been demonstrated by the direct determination of nitroimidazoles from pig liver tissue. The high efficiency of the proposed system allowed the extraction and the determination of the analytes to be performed from a simple tissue homogenate obtained in water. The precision of the analysis of spiked samples, expressed in terms of relative standard deviation, was better than 4.8%. [source] Urtica dioica agglutinin: Separation, identification, and quantitation of individual isolectins by capillary electrophoresis and capillary electrophoresis,mass spectrometryELECTROPHORESIS, Issue 9 2005Markus Ganzera Abstract With benign prostatic hyperplasia (BPH) being a major health problem in ageing men, alternative therapeutic approaches (e.g., with phytopharmaceuticals) are of great interest. Based on pharmacological evidences, one of the most promising options in that respect are the lectins found in Urtica dioica (stinging nettle) roots. In this study the qualitative and quantitative analysis of individual isolectins in U. dioica extracts is described, which is the first report on using capillary electrophoresis (CE) for the analysis of lectins in plant material at all. By utilizing a 200 mM sodium acetate buffer (pH 3.75) a baseline separation and determination of four closely related isolectins was feasible within 20 min in the aqueous plant extracts. The individual compounds were identified based on reference compounds as well as data obtained from CE-mass spectrometry (MS) experiments. After modifying the optimized CE conditions to 100 mM ammonium formate buffer with pH 3.75 and a voltage of 15 kV, the isolectins were clearly assignable in positive electrospray ionization (ESI) mode. The quantitative results obtained by CE (the total lectin content varied from 0 to 0.42% in the samples) were accurate (recovery rates of spiked samples between 92.5 and 96.2%), precise (relative standard deviation < 5%) and in good agreement to those obtained by High-performance liquid chromatography (HPLC). As for peak resolution, assignable compounds and required separation time the newly developed CE method was clearly advantageous over the determination achieved by LC. [source] Indirect identification of isoprenoid quinones in Escherichia coli by LC-MS with atmospheric pressure chemical ionization in negative modeJOURNAL OF BASIC MICROBIOLOGY, Issue 6 2004Mengchun Gao Dr. A novel analytical method was applied for identification of isoprenoid quinones in Escherichia coli by liquid chromatography atmospheric press chemical ionization mass spectrometry in negative mode (LC-NI-APCI-MS). Extraction and clean-up of sample were carried out on Sep-Pak Plus Silica solid-phase extraction cartridges. Ubiquinone-7 (UQ-7), Ubiquinone-8 (UQ-8) and Mequinone-8 (MK-8) were determined directly using combined information on retention time, molecular ion mass, fragment ion masses and UV characteristic spectrometry without any standard reagent. It was found that UQ-8 was the major component of isoprenoid quinones in Escherichia coli under aerobic condition. Compared with UQ-8, the relative abundance of UQ-7 and MK-8 is only 15% and 14%, respectively. The average recoveries of UQ-6, UQ-10 and vitamin K1 in Escherichia coli were investigated by standard spiking experiment. The recoveries were achieved in the range from 94 to 106%, and the relative standard deviations (RSD) of the triplicate analysis of the spiked samples (UQ-6, UQ-10 and vitamin K1) ranged from 3 to 8%. The detection limits of LC-NI-APCI-MS were estimated to be 5, 40 and 0.8 ,g/g dry cell for UQ-6, UQ-10 and vitamin K1, respectively. (© 2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] A STUDY ON SUITABILITY OF FOUR ENRICHMENT BROTHS FOR PCR-BASED DETECTION OF LISTERIA MONOCYTOGENES FROM RAW MEATJOURNAL OF FOOD SAFETY, Issue 1 2006J. BALAMURUGAN ABSTRACT Four enrichment broths were evaluated for their compatibility with the polymerase chain reaction (PCR) for detection of Listeria monocytogenes from raw meat after single-step enrichment. Standardized PCR protocols for listeriolysin O (hlyA) gene were used for the species-specific identification of L. monocytogenes. Four broths, namely, modified University of Vermont broth (MUVM), Listeria enrichment broth (LEB), Fraser broth (FB) and polymyxin, acriflavin, lithium chloride, ceftazidime, aesculin, mannitol, egg yolk broth (PALCAM) , were inoculated with L. monocytogenes. The enriched cultures were subjected for PCR. Similarly, meat samples were artificially spiked with various concentrations of L. monocytogenes, these spiked samples were enriched in the above-mentioned four broths and subjected to PCR to determine the medium that was most compatible for PCR-based detection of L. monocytogenes. The aliquots taken during different incubation periods were subjected to three different procedures for the concentration of the target organism for use in PCR. Results revealed that MUVM was better than other broths for the detection of L. monocytogenes by both PCR and cultural method; moreover, it was able to support the growth of as low as 10 cfu/g of meat. Concentration of the target organisms by centrifugation and washing with PCR buffer was the most suitable method for improving PCR performance for detection of L. monocytogenes. Goat (n = 67) and buffalo (n = 45) meat samples from local markets were also screened by both PCR and cultural method to validate the results obtained from the spiking studies. Both results were in agreement in spiking studies as well as screening of market meat samples. [source] Determination of 17,-estradiol in bovine plasma: development of a highly sensitive technique by ion trap gas chromatography,tandem mass spectrometry using negative chemical ionization,JOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 12 2002Giancarlo Biancotto Abstract A novel approach to the determination of 17,-estradiol in bovine plasma is presented. The observed enhanced sensitivity is gained by the application of tandem mass spectrometry (MS) fragmentation to a stable, well characterized negative ion produced by chemical ionization (methane as reagent gas). A specific derivatizing reactant is employed (pentafluorobenzyl bromide), combined with bis-trimethylsilyltrifluoroacetamide, to favor the formation of a diagnostic precursor negative ion. Plasma samples are purified through a C18 solid phase extraction column and derivatized before gas chromatography,MS analysis. The accuracy and the precision of the method, tested over a set of spiked samples, were satisfactory. The limit of detection was found to be 5 pg ml,1 and the limit of quantification was fixed at 20 pg ml,1. The fragmentation pattern is fully explained and the method is applicable for the official analysis of bovine plasma for the detection of 17,-estradiol according to the European criteria 256/93 and to the draft SANCO/1805/2000 rev. 3. The quantification of incurred positive samples was performed according to the proposed procedure and compared with the results obtained by standardized radio immuno assay; the estimated concentrations were significantly similar. Copyright © 2002 John Wiley & Sons, Ltd. [source] Rapid quantification of sucrose esters in oriental tobacco by liquid chromatography-ion trap mass spectrometryJOURNAL OF SEPARATION SCIENCE, JSS, Issue 1 2007Li Ding Abstract A rapid and sensitive LC-MS/MS method was developed for the quantitative determination of sucrose esters (SEs) in Oriental tobacco samples. The sample preparation involved a 10-min sonication extraction procedure with acetone and five-fold dilution of the extract with methanol. The experiment was carried out in positive ion mode by ESI IT mass spectrometer. Because of lack of authentic standards of SEs, sucrose octa-acetate (internal standard, IS) was used as a surrogate to validate the proposed method. Matrix-matched standard calibration was used for quantification of IS in the spiked samples. Under optimized MS/MS conditions, an LOQ of 3.9 ,g/g was achieved for IS, with an LOD of about 1.2 ,g/g. Recoveries for IS were 95,97%. Among 19 monitored SEs, the contents of 11 SEs had RSDs lower than 13.7%. The method, with very little sample handling and good sensitivity, was applied to the rapid quantification of SEs in four Oriental tobacco samples. It appears that the sum of contents of the five SEs with MW 650, 664, and 678 Da occupied approximately 80% of the total content of SEs. [source] Evaluation of PetrifilmÔ EC method for enumeration of E. coli from soilLETTERS IN APPLIED MICROBIOLOGY, Issue 5 2010A.D. Samarajeewa Abstract Aims:, To evaluate the suitability of commercially available PetrifilmÔ EC plates for enumeration of Escherichia coli from soil. Methods and Results:, A confirmed E. coli strain isolated from liquid swine manure was inoculated into sterilized sandy clay loam and loam soils at the concentrations of 102, 103, 105 CFU g,1 of soil. The efficiency of recovery on PetrifilmÔ EC plates for soils spiked with E. coli was compared with standard membrane filtration techniques on m-FC basal medium supplemented with 3-bromo-4-chloro-5-indoyl-,- d -glucopyranoside (BCIG) and most probable numbers (MPN) techniques in E. coli medium with 4-methylumbelliferyl-,- d -glucuronide (EC-MUG) broth. PetrifilmÔ EC and m-FC (BCIG) methods were then assessed for the ability to recover E. coli from field soils applied with swine manure. No significant differences (P > 0·05) were observed between PetrifilmÔ EC, m-FC (BCIG) and MPN methods for the recovery of E. coli from spiked samples, irrespective of soil type. However, recovery of E. coli from manure-applied field soil samples showed a significant difference (P < 0·05) between the PetrifilmÔ EC method and the m-FC method in enumerating E. coli possibly as a result of false positives on m-FC. Conclusion:, The PetrifilmÔ EC method is suitable for the enumeration of E. coli from soil with a detection limit of 10 CFU g,1 soil. Significance and Impact of the Study:, The commercially available PetrifilmÔ EC method is comparatively low cost, easy to use method for the enumeration of E. coli from soil without the need for further confirmation tests. [source] Cloud point extraction combined with electrothermal vaporization inductively coupled plasma mass spectrometry for the speciation of inorganic selenium in environmental water samplesRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 19 2006Beibei Chen A new method based on cloud point extraction (CPE) separation and electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICPMS) detection has been proposed for the speciation of inorganic selenium in environmental waters. When the temperature of the system is higher than the cloud point temperature (CPT) of the selected surfactant Triton X-114, the complex of Se(IV) with ammonium pyrrolidine dithiocarbamate (APDC) seems to be extracted into the surfactant-rich phase, whereas the Se(VI) remains in aqueous solutions. Thus, an insitu separation of Se(IV) and Se(VI) could be realized. The concentrated analyte was introduced into the ETV-ICP mass spectrometer for determination of Se((IV) after dilution with 200,µL methanol. Se(VI) was reduced to Se(IV) prior to determining total selenium, and its assay was based on subtracting Se(IV) from total selenium. The main factors affecting the CPE and the vaporization behavior of the analyte were investigated in detail. Under the optimized experimental conditions, the limit of detection (LOD) for Se(IV) was 8.0,ng/L with an enhancement factor of 39 when 10,mL of sample solution was preconcentrated to 0.2,mL. The relative standard deviation (RSD) was found to be 3.9% (CSe(IV),=,1.0,µg/L, n,=,7). The proposed method was applied to the speciation of inorganic selenium in different environmental water samples with the recovery for the spiked samples in the range of 82,102%. Copyright © 2006 John Wiley & Sons, Ltd. [source] Method validation for measurement of hair nicotine level in nonsmokersBIOMEDICAL CHROMATOGRAPHY, Issue 3 2009Sung Roul Kim Abstract The development of strategies to address the growing worldwide burden of exposure to secondhand smoke (SHS) would be facilitated by sensitive and accurate methods for assessing SHS exposure. Hair provides a readily available matrix for assessing biomarkers of typical SHS exposure. We developed and applied an optimized analytical method using an isotope dilution gas chromatography,mass spectrometry (GC/MS) for hair nicotine measurement. The utility of this optimized method is illustrated by presenting data on SHS exposure of women and children from 31 countries. Using this isotope dilution method with spiked samples (3.3 ng/mg), we found that the greatest hair nicotine extraction efficiency was obtained with a 60 min shaking time. In the field study (n = 2400), a positive association was evident between hair nicotine concentrations from nonsmokers and higher numbers of cigarettes smoked per day in a household. Copyright © 2008 John Wiley & Sons, Ltd. [source] | |||||||||||||