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31.
Two new applications using multiple ion isolations in the cell of a Fourier transform-ion cyclotron resonance mass spectrometer equipped with an electrospray ionization source are described. A procedure that uses multiple ion isolations of an analyte and calibrants for internal calibration at each stage in a MSn experiment, under high-resolution exact-mass conditions, for structural characterization/elucidation of angiotensin I and rapamycin is illustrated. Fragment ion mass accuracies < 1.0 ppm are demonstrated and routinely achieved. Purification of a mixture is illustrated by isolating multiple charge states of a protein-drug complex from residual protein for further MSn studies to elucidate the site of covalent drug bonding using IRMPD for a mixture of epidermal growth factor receptor (EGFr) protein and EGFr-drug complex. The procedure developed for multiple ion isolations is referred to as multi-CHEF, multiple correlated harmonic excitation fields, in which tailored waveforms are used to notch out multiple mass regions of a spectrum with minimal off-resonance excitation. 相似文献
32.
Theory is little used in the prediction of physician cancer screening stage of change. Structural equation modeling was used to evaluate the theoretical predictors of stage of change to recommend colonoscopy among 235 urban physicians. Constructs from the theory of planned behavior, social-cognitive theory, and the transtheoretical model were systematically tested. As predicted, contextual factors, such as the physicians' ages, their race-ethnicities, patient race-ethnicity, and office-related barriers to preventive care were associated with stage of change through self-efficacy, normative beliefs, and negative behavioral beliefs. The findings demonstrate the relevance of these models to studying the behavior of physicians and support the development of interventions that are tailored to normative beliefs and specific physician cognitions for colonoscopy recommendation. (PsycINFO Database Record (c) 2010 APA, all rights reserved) 相似文献
33.
34.
Suga K Mochizuki N Yamashita H 《Shokuhin eiseigaku zasshi. Journal of the Food Hygienic Society of Japan》2004,45(5):255-258
A simple method for analysis of fumonisin B1 (FB1) and fumonisin B2 (FB2) in beer and raw materials of beer using liquid chromatography-electrospray ionization tandem mass spectrometry (LC/MS/MS) was developed. Samples were prepared and purified by using solid-phase extraction columns (SAX). The LC separation was performed with an octadecylated silica column at a flow-rate of 0.2 mL/min, using a mobile phase consisting of water and acetonitrile. MS/MS was used in multiple reaction monitoring, employing electrospray ionization (ESI-MRM). Recoveries of spiked FB1 and FB2 from beer were 64% and 52%, respectively, at the level of 5 microg/kg. Recoveries of spiked FB1 and FB2 from malt, cornstarch, and corn grit, at the level of 50 microg/kg, were 87.9% and 86.4%, 89.5% and 87.9%, 86.6% and 81.1%, respectively. This method may have applications in quality assurance. 相似文献
35.
Suga K Mochizuki N Harayama K Yamashita H 《Shokuhin eiseigaku zasshi. Journal of the Food Hygienic Society of Japan》2004,45(6):307-312
A simple method for analysis of trichothecenes [Type A: diacetoxyscirpenol, neosolaniol, HT-2 toxin, and T-2 toxin, Type B: deoxynivalenol, nivalenol, fusarenon-X, 3-acetyldeoxynivalenol, 15-acetyldeoxynivarenol] in barley tea and beer using liquid chromatography tandem mass spectrometry (LC/MS/MS) was developed. Trichothecenes were extracted with ethyl acetate-methanol (19:1). The solvent was evaporated to dryness and the residue was dissolved in water-methanol (3:1) for injection into the LC/MS/MS. The LC separation was performed with an octadecylated silica column at a flow-rate of 0.2 mL/min, using a mobile phase consisting of water, methanol and acetonitrile. MS/MS was used in multiple reaction monitoring, employing electrospray ionization (ESI-MRM). The recoveries of trichothecenes from drinks at 1 microg/L (Type A) and 10 microg/L (Type B) were 52.5-115.2% (barley tea) and 68.1-127.5% (beer). Five barley tea and ten beer samples were analyzed by this method. Trichothecenes were not detected in them. This method may have applications in quality assurance. 相似文献
36.
The optical texture of cokes from two SRC pitches of different coking properties, from co-carbonizations of these materials and of hydrogenated and alkylated products has been studied. The objective, relative to formation of needle-cokes, is to correlate the optical texture of cokes with the chemical structure of the pitch materials using both benzene-soluble (BS) and insoluble (BI) fractions of the pitches. Hydrogenation improved the compatibility of the BS fraction of the inferior SRC pitch (No. 2) with the BI fractions of the two pitches (non-hydrogenated) using a ratio of only 1 to 9. Before hydrogenation, a ratio of BS to BI of 8 to 2 did not give a needle-coke. In contrast, alkylation destroyed the compatibility of the BS fraction of the superior SRC pitch (No. 1) with the BI fraction (non-alkylated) using a ratio of 6 to 4, and which gave a needle-coke before alkylation. Hydrogenation of the alkylated material restored the compatability. The relevance of these studies to industrial carbonization processes is discussed in terms of chemical treatment and the hydrogen economy. 相似文献
37.
The kinetic and thermodynamic constants of the hydrolytic polymerization of ?-caprolactam were determined by least-squares curve fitting. The calculations were carried out using observed kinetic data such as concentration of ?-caprolactam ([CL]), endgroup ([EG]), and ?-aminocaproic acid ([ACA]) and time derivatives of each concentration (rates) ?[CL]/?t, ?[EG]/?t, and ?[ACA]/?t. The sets of the converged constants are obtained for the initial water concentrations of 0.42, 0.82, and 1.18 mole/kg. An averaged set of the constants applicable for this range of the initial composition was also evaluated. The compatibility between observed and calculated concentration and rate curves was improved by the use of the newly developed sets of the constants. The mechanism of the polycondensation reaction is also discussed, based on the rate and kinetic constants obtained by this work. 相似文献
38.
Kanda M Ushiyama K Igusa K Murayama M Horie M Hirokado M Miyazaki T 《Shokuhin eiseigaku zasshi. Journal of the Food Hygienic Society of Japan》2003,44(2):110-113
A simple and rapid determination of anticoccidial drug residues, diclazuril (DCZ) and nicarbazin (NCZ), in chicken tissues has been developed. DCZ and NCZ were extracted with acetonitrile from chicken liver, muscle, and fat. The extract was rinsed with n-hexane saturated with acetonitrile and then evaporated. The residue was dissolved in 1.4 mL of acetonitrile-methanol (1:1), then 1.0 mL of n-hexane saturated with acetonitrile-methanol (1:1) was added, and the mixture was partitioned by the addition of 0.6 mL of water. DCZ and NCZ in the aqueous layers were determined by HPLC on an Xterra RP-18 column with acetonitrile-0.5% ammonium acetate containing 0.01 mol/L tetra-n-butylammonium hydrogen sulfate (43:57) as the mobile phase. The mean recoveries (n = 5) of DCZ and NCZ spiked in chicken tissues at the maximum residue levels were 92.0-95.6% (CV 2.4-3.0%) and 87.3-89.4% (CV 1.7-2.8%), respectively. The detection limits of DCZ and NCZ were 0.01 and 0.004 microgram/g, respectively. 相似文献
39.
Gunay NS Tadano-Aritomi K Toida T Ishizuka I Linhardt RJ 《Analytical chemistry》2003,75(13):3226-3231
A systematic approach was used to evaluate the electrospray ionization mass spectral (ESI-MS) analysis of sucrose octasulfate (SOS), an important pharmaceutical agent. SOS represents a model for other suffated carbohydrates, such as heparin and glycosaminoglycan-derived oligosaccharides that also are highly sulfated and pose difficult analytical problems. A survey of ammonium counterions showed that 1 degree, 2 degrees, and 3 degrees ammonium salts of SOS gave substantial fragmentation as a result of sulfate loss. In contrast, quaternary ammonium and phosphonium salts gave excellent ESI spectra, particularly in the positive ion mode. This represents the first report of the ESI-MS analysis of sulfated carbohydrates in the positive ion mode. 相似文献
40.
When a predatory mite, Amblyseius womersleyi is present, Tetranychus kanzawai takes refuge on its webs during a quiescent stage. To examine the factors responsible for the antipredator behavior of T. kanzawai, we exposed T. kanzawai to the odor of conspecifics, A. womersleyi, and both T. kanzawai and A. womersleyi. The proportion of T. kanzawai females that took refuge was significantly higher when they were exposed to the odor of `both T. kanzawai and A. womersleyi.' Furthermore, the proportion of T. kanzawai females that took refuge was significantly higher when they were exposed to injured conspecifics than to intact conspecifics. These results suggest that T. kanzawai assesses predation risk, at least in part, by using the odor of injured conspecifics. 相似文献