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Good Linear Relationships (good + linear_relationships)
Selected AbstractsSimultaneous determination of 103 pesticide residues in tea samples by LC-MS/MSJOURNAL OF SEPARATION SCIENCE, JSS, Issue 9 2009Zhiqiang Huang Abstract A simple and sensitive method was developed and validated for the simultaneous determination of 103 pesticide residues in tea by LC-MS/MS. For the analysis of the pesticide with polarity, thermal lability or low volatility, this LC-MS/MS method has an advantage over GC. In this work, residual pesticides were extracted from the tea sample with ACN and then purified using Carb-NH2 SPE cartridges. Using the multiple reaction monitoring mode, the pesticides were quantified and identified by the most abundant and characteristic fragment ions. The recoveries obtained for each pesticide ranged between 65 and 114% at three spiked concentration levels. The intra-day precisions were lower than 19.6%. Good linear relationships were observed with the correlation coefficients r2 >0.996 for all analytes. The established method was successfully applied to the determination of pesticide residues in real tea samples. [source] Simple method for determination of five terpenoids from different parts of Tripterygium wilfordii and its preparations by HPLC coupled with evaporative light scattering detectionJOURNAL OF SEPARATION SCIENCE, JSS, Issue 9 2007Xiao-Ling Luo Abstract By optimizing the extraction, separation, and analytical conditions, a reliable and accurate high-performance liquid chromatography method coupled with evaporative light scattering detection (ELSD) was developed for simultaneous determination of five terpenoids, i. e., triptolide, tripchlorolide, demethylzelastral, wilforlide B, and wilforlide A, in root, stem, leaves, root bark, twig, and root without bark of Tripterygium wilfordii Hook. f and six of its herbal preparations. This approach would thus provide a more accurate and general method for evaluating the quality of the herb and its preparations. Separation of these five terpenoids was achieved on a ZORBAX Eclipse XDB-C8 column with gradient elution using water and acetonitrile as solvents, both containing 0.05% formic acid, at a temperature of 30°C and a flow rate of 0.8 mL/min. The drift tube temperature of ELSD was set at 100°C, and the nitrogen flow rate at 1.5 L/min. Good linear relationships were obtained with correlation coefficients for the analytes exceeding 0.992, and the LOD and LOQ were less than 0.149 ,g and 0.297 ,g on column, respectively. Intra-day and inter-day precision of the analytes were less than 1.25% and 5.97%, respectively, and the average recovery rates obtained were in the range of 95.9 ± 3.7% to 100.4 ± 5.0% for all terpenoids with RSDs below 4.99%. Quantitative analysis of the five terpenoids in different parts of Tripterygium wilfordii and its six preparations showed that the contents of the terpenoids varied significantly. The tender root contained higher concentrations of triptolide, tripchlorolide, demethylzelastral, and wilforlide B than any other part of the herb. Correspondingly, the root bark contained the greatest concentration of wilforlide A, and the stem and twig came in second and third. This suggested that we could infer whether the medicinal materials were absolute roots without bark or not from the comparative contents of these terpenoids in the tablets in view of the fact that only the roots without bark are the valid officinal part of the plant. This method and the quantitation results obtained can provide a scientific and general as well as simple and convenient approach for the product manufacturers to set up quality control standards and for informing the public about the quality and safety of the preparations. [source] A theoretical investigation on the structures, densities, detonation properties, and pyrolysis mechanism of the nitro derivatives of phenolsINTERNATIONAL JOURNAL OF QUANTUM CHEMISTRY, Issue 9 2010Guixiang Wang Abstract The nitro derivatives of phenols are optimized to obtain their molecular geometries and electronic structures at the DFT-B3LYP/6-31G* level. Detonation properties are evaluated using the modified Kamlet,Jacobs equations based on the calculated densities and heats of formation. It is found that there are good linear relationships between density, detonation velocity, detonation pressure, and the number of nitro and hydroxy groups. Thermal stability and pyrolysis mechanism of the title compounds are investigated by calculating the bond dissociation energies (BDEs) at the unrestricted B3LYP/6-31G* level. The activation energies of H-transfer reaction is smaller than the BDEs of all bonds and this illustrates that the pyrolysis of the title compounds may be started from breaking OH bond followed by the isomerization reaction of H transfer. Moreover, the CNO2 bond with the smaller bond overlap population and the smaller BDE will also overlap may be before homolysis. According to the quantitative standard of energetics and stability as a high-energy density compound, pentanitrophenol essentially satisfies this requirement. In addition, we have discussed the effect of the nitro and hydroxy groups on the static electronic structural parameters and the kinetic parameter. © 2009 Wiley Periodicals, Inc. Int J Quantum Chem, 2010 [source] Substituent effect on the [2,+,3] cycloaddition of (E)-,-Nitrostyrene with (Z)- C,N -Diarylnitrones,JOURNAL OF PHYSICAL ORGANIC CHEMISTRY, Issue 2 2002Andrzej Baranski Abstract The kinetics of the title reaction were studied in toluene at 80,°C by means of HPLC. The overall rate constant (ktotal) of the reaction of (E)-,-nitrostyrene (1) with (Z)- C -phenyl- N -arylnitrones (2a,g) was found to increase with increasing Hammett ,-constant, whereas in the case of (Z)- C -aryl- N -phenylnitrones (2g,p) and the same nitrostyrene the rate decreased. The substituent effect in these reactions is inconsistent with FMO treatments of cycloaddition rates. For both reaction series good linear relationships were obtained between log ktotal and the net charge on the carbon atom in the >CN(O), moiety of the nitrones calculated by the AM1 method. Copyright © 2001 John Wiley & Sons, Ltd. [source] Separation and determination of active components in Radix Salviae miltiorrhizae and its medicinal preparations by nonaqueous capillary electrophoresisJOURNAL OF SEPARATION SCIENCE, JSS, Issue 7-8 2004An Jia Chen Abstract A nonaqueous capillary electrophoresis (NACE) method was developed for simultaneous assay of three bioactive components (1: cryptotanshinone; 2: tanshinone IIA, and 3: tanshinone I) in Radix Salviae miltiorrhizae and in its herbal preparations for the first time. After optimization of separation conditions, a buffer of 250 mmol L,1 ammonium acetate containing 30% acetonitrile and 1.0% acetic acid (V : V) in methanol was selected for separating the three analytes, but baseline separation of tanshinon I and tanshinone IIA was not obtained. Therefore second-order derivative electropherograms were applied for resolving overlapping peaks. Regression equations revealed good linear relationships (correlation coefficients 0.9943,0.9991) between peak heights in second-order derivative electropherograms and concentrations of the three analytes. The relative standard deviations (RSD) of the migration times and the peak height of the three constituents were in the range of 0.81,0.88% and 0.34,1.13% (intra-day), 1.57,1.86% and 3.05,5.52% (inter-day), respectively. The recoveries of three constituents ranged from 90.2 to 108.5%. The results indicated that baseline separation of the analytes was sometimes hard to obtain and second-order derivative electropherograms were applicable for the resolving and analysis of overlapping peaks. [source] A new set of electronegativity scale for trivalent lanthanidesPHYSICA STATUS SOLIDI (B) BASIC SOLID STATE PHYSICS, Issue 6 2007Keyan Li Abstract A new set of electronegativity (EN) scale for all trivalent lanthanides (Ln) is proposed on the basis of effective ionic potential, from which the electron-attracting power of trivalent Ln can be well differentiated. This new scale can be used to qualitatively explain the valence stability and valence change of some typical trivalent Ln. Furthermore, the good linear relationships of the charge-transfer energy of Ln3+ and the first dehydroxylation temperature in the agardite to the current EN scale of Ln3+ show us the further reasonableness of our new EN scale. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Quantitative analyses of indoloquinazoline alkaloids in Fructus Evodiae by high-performance liquid chromatography with atmospheric pressure chemical ionization tandem mass spectrometryRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 20 2006Yan Zhou Fructus Evodiae (Wuzhuyu), the fruits of Evodia rutaecarpa and related varieties, is widely used in traditional Chinese medicine. The bioactive constituents include the indoloquinazoline alkaloids rutaecarpine, evodiamine and dehydroevodiamine. A new assay based on high-performance liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry (HPLC/UV/APCI-MS/MS) was developed for the measurement of the indoloquinazoline alkaloids in commercial Fructus Evodiae products. Initially, the MS/MS fragmentation pathways of indoloquinazoline alkaloids were investigated to identify fragment ions that might be useful for the sensitive and selective detection of trace indoloquinazoline alkaloids during LC/MS/MS. Then, quantitative MS analysis of five indoloquinazoline alkaloids in 12 commercial Fructus Evodiae products from different geographical sources was performed. Analyte recovery was in the range of 97.5,105.3% for all with relative standard deviations (RSDs) below 6%, the intra-assay and inter-assay RSDs were less than 7%, and good linear relationships were shown with correlation coefficients for the analytes exceeding 0.999. Therefore, this LC/MS/MS assay facilitated the rapid quantitative analysis of rutaecarpine, evodiamine, evodiamide, 14-formyldihydrorutaecarpine and dehydroevodiamine in 12 commercial Fructus Evodiae products with excellent recovery, repeatability, accuracy and sensitivity. This method is simple and specific and can be used for identification and quality control of this traditional Chinese remedy. Copyright © 2006 John Wiley & Sons, Ltd. [source] Fifteen-Count Breathlessness Score in adults with COPDRESPIROLOGY, Issue 5 2006Marie WILLIAMS Objective and background: The Fifteen-Count Breathlessness Score (15CBS) has been reported to quantify breathlessness. The aim of this study was to determine the reliability and validity of the 15CBS in adults with COPD. Methods: Using an observational correlation design, subjects with clinical signs and symptoms of COPD were videotaped performing the 15CBS at a self-selected (task 1) and an 8-s counting pace (task 2), on two occasions with 5-min rest between attempts. Respiratory-related quality of life questionnaires, self-report shortness of breath measures and pulmonary function tests were completed by all subjects. Results: Thirty subjects completed the protocol. No significant differences and good linear relationships were calculated for the 15CBS within subjects (task 1 P = 0.32, r = 0.75 and task 2 P = 1.00, r = 0.86) and between assessors (task 1 P = 0.57, r = 0.99 and task 2 P = 0.21, r = 0.75). No significant relationships were evident between the 15CBS and shortness of breath or quality of life scores. Significant relationships existed between the 15CBS and FVC (litres and per cent predicted). Conclusion: Most subjects completed the 15CBS using one breath, limiting discrimination between subjects with differing degrees of breathlessness. Although data from this study confirmed that the 15CBS is a reliable procedure within people with COPD, further modification is required to increase the validity and discriminative ability of this instrument. [source] Determination of halofantrine and its main metabolite desbutylhalofantrine in rat plasma by high-performance liquid chromatography with on-line UV irradiation and peroxyoxalate chemiluminescence detectionBIOMEDICAL CHROMATOGRAPHY, Issue 1 2009Abena Amponsaa-Karikari Abstract A sensitive, selective and reliable method has been developed and validated for the determination of halofantrine and its metabolite desbutylhalofantrine in rat plasma using 9,10-diphenylanthracene as an internal standard. The method is based on peroxyoxalate chemiluminescence detection of hydrogen peroxide produced from fused aromatic rings in the structures of halofantrine and desbutylhalofantrine upon UV irradiation. Using spiked rat plasma, good linear relationships were obtained for both halofantrine and desbutylhalofantrine between peak height ratios (vs internal standard) and their corresponding concentrations over a range of 0.01,0.8 µg/mL with correlation coefficients of at least 0.997. The detection limits at signal-to-noise ratio of 3 using 0.2 mL of rat plasma were 1.5 and 1.4 ng/mL for halofantrine and desbutylhalofantrine, respectively. Relative standard deviations (n = 3) intra- and inter-day were between 0.5 and 5.4% for all the studied concentrations. Using this method with simple sample treatment, halofantrine and desbutylhalofantrine in rat plasma could be precisely determined without interference from endogenous substances. The method was successfully applied to the measurement of the time courses of plasma halofantrine concentration after oral administration of the drug (7 mg/kg) to rats. Copyright © 2008 John Wiley & Sons, Ltd. [source] Simultaneous Determination of Epinephrine, Noradrenaline and Dopamine in Human Serum Samples by High Performance Liquid Chromatography with Chemiluminescence DetectionCHINESE JOURNAL OF CHEMISTRY, Issue 7 2007Fu-Nan Chen Abstract A simple, rapid and accurate high performance liquid chromatographic (HPLC) technique coupled with chemiluminescence (CL) detection was developed for the simultaneous determination of epinephrine (E), noradrenaline (NA) and dopamine (DA). It was based on the analyte enhancement effect on the CL reaction between luminol and potassium ferricyanide. The effects of various parameters, such as potassium ferricyanide concentration, luminol concentration, pH value and component of the mobile phase on chromatographic behaviors of the analytes (E, NA and DA) were investigated. The separation was carried out on C18 column using the mobile phase of 0.01 mol/L potassium hydrogen phthalate solution and methanol (92:8, V/V). Under the optimum conditions, E, NA and DA showed good linear relationships in the range of 1×10,8,5×10,6, 5.0×10,9,1.0×10,6 and 5.0×10,9,1.0×10,6 g/mL respectively. The detection limits for E, NA and DA were 4.0×10,9, 1.0×10,9 and 8.0×10,10 g/mL. The proposed method has been applied successfully to the analysis of E, NA and DA in human serum samples. [source] | ||||||||||