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The methods of the α-proton chemical shift index (CSI) and the amide proton (NH) chemical shift temperature coefficient (Δδ/ΔT) were found experimentally by a number of studies on proton NMR chemical shifts of peptides and proteins in an aqueous solution, and have been widely accepted. They provide an insight into secondary structures and intra-molecular hydrogen bonds in peptides and proteins without complex calculation. Our question is whether the methods are applicable to helical peptides in methanol. Melittin, a peptide of 26 amino acid residues found in bee venom, has been known to consist of two helices (the residues 2-11 and 13-26) connected by a kink section (the residues 11-13). Employing the methods for melittin in methanol, we have shown that most of the CSI's for the residues 3-10 and 14-26 are - 1, and the Δδ/ΔT's for the residues 5-26 except 6 and 14 are more positive than - 6 ppb/℃. If the methods are applicable to melittin in methanol, these results indicate that helix structures are formed in the regions of the residues 3-10 and 14-26 and NH's in the residues 5-26 except 6 and 14 are involved in intra-molecular hydrogen bonds. The helical structure evaluated from the methods, hence, agrees nearly with the known helix structure. We also apply the methods to D-Pro14 melittin (synthetic melittin) and alamethicin (a peptide of 20 amino acid residues) in methanol, and show that they virtually work well.

Background In vitro diagnostic bilirubin reagents based on oxidation with bilirubin oxidase or vanadic acid for total and direct-reacting bilirubin are widely used in Japan; however, their reactivity to unconjugated and conjugated bilirubin and delta bilirubin has not been completely disclosed by manufacturers. We used artificially prepared bilirubin materials to investigate the reactivity with four in vitro diagnostic bilirubin reagents. Methods Porcine unconjugated bilirubin solution, chemically synthesized ditaurobilirubin solution, and chemically synthesized delta bilirubin solution were used as surrogates of naturally occurring unconjugated bilirubin, conjugated bilirubin, and delta bilirubin, respectively. The total bilirubin and direct-reacting bilirubin concentrations were measured by three bilirubin oxidase methods and one vanadic acid method, and the observed concentrations were compared with those obtained by the diazo-based reference measurement procedure. Results The unconjugated bilirubin and delta bilirubin concentrations were similar when any of the four in vitro diagnostic bilirubin reagents were used during total bilirubin measurement. This was consistent with reference measurement procedure and exhibited a converged inter-method variation. Compared with reference measurement procedure, significantly low ditaurobilirubin concentrations were observed by the in vitro diagnostic bilirubin reagents despite the converged inter-method variation. In delta bilirubin measurement, some reagents reacted doubtfully with unconjugated bilirubin, while showed lower ditaurobilirubin concentrations than its corresponding total bilirubin concentration. Reactivity with delta bilirubin was different for each method including reference measurement procedure. Some reagents were developed to react less with delta bilirubin and others to strongly react with delta bilirubin. Conclusions We revealed the reactivity of IVD-TB and IVD-DB reagents to artificially prepared bilirubin materials, and their consistency with reference measurement procedure. The delta bilirubin data results vary depending on the reagents used.

IMPORTANCE: A delayed large local reaction (DLLR) is a delayed-onset adverse skin reaction that may occur after injection of the mRNA-1273 vaccine against SARS-CoV-2. OBJECTIVE: To examine the associations between sex and age and susceptibility of DLLRs after mRNA-1273 vaccination. DESIGN, SETTING, AND PARTICIPANTS: This retrospective cross-sectional study was conducted at the Self-Defense Forces large-scale vaccination center in Tokyo, Japan, from May 24 to November 30, 2021. Participants were recipients of the second dose of the mRNA-1273 vaccine who had received the first dose 4 to 6 weeks earlier. Five experienced dermatologists interviewed participants to assess whether they had experienced symptoms of DLLR after administration of the first dose of the vaccine. EXPOSURE: Receipt of the first dose of the mRNA-1273 vaccine. MAIN OUTCOMES AND MEASURES: The primary outcome was the incidence rate of DLLR stratified by sex and age group. Odds ratios (ORs) were calculated to evaluate the differences between groups. Outcomes were tested for significance using the Pearson χ(2) test with 95% CIs. RESULTS: Of 5893 participants in the study, 3318 (56.3%) were male (median age, 55 years [IQR, 38-68 years]) and 2575 (43.7%) were female (median age, 50 years [IQR, 34-67 years]). A total of 747 participants (12.7%) experienced DLLR symptoms after the first dose of the mRNA-1273 vaccine. Symptoms were mild and not considered as contraindications to the vaccine. The incidence rate was significantly higher among females (22.4% [577 participants]; OR, 5.30; 95% CI, 4.42-6.34) than among males (5.1% [170 participants]; reference). Moreover, the incidence rate was significantly higher among participants aged 30 to 39 years (14.3% [129 participants]; OR, 1.68; 95% CI, 1.25-2.26), 40 to 49 years (15.8% [136 participants]; OR, 1.89; 95% CI, 1.41-2.53), 50 to 59 years (14.9% [104 participants]; OR, 1.76; 95% CI, 1.29-2.40), and 60 to 69 years (12.6% [182 participants]; OR, 1.45; 95% CI, 1.10-1.91) than among participants aged 18 to 29 years (9.0% [81 participants]; reference). CONCLUSIONS AND RELEVANCE: In this cross-sectional study, the first dose of the SARS-CoV-2 mRNA-1273 vaccine was associated with a higher incidence of DLLR among females and among individuals aged 30 to 69 years. The findings suggest that DLLR may be a type IV allergic skin reaction.

Tailoring the elemental doping of inorganic nanowires remains an important challenge due to complex dopant incorporation pathways. Here we report that the face-selectivity of tungstate ions controls growth direction and dopant incorporation of hydrothermal zinc oxide nanowires. The introduction of tungstate ions on nanowire surface during synthesis unexpectedly enhances nucleation at sidewall $$\left\{ {10\bar 10} \right\}$$ 10 1 ¯ 0 planes, while dopant incorporation occurs only on (0001) planes. This conflicting face-selective behavior leads to inhomogeneous dopant distribution. Density functional theory calculations reveal that the face-selective behavior can be interpreted in terms of the effect of coordination structure of the tungstate ions on each zinc oxide crystal plane. In addition, we demonstrate a rational strategy to control the morphology and the elemental doping of tungsten-doped zinc oxide nanowires.

Porcine unconjugated bilirubin solution, chemically synthesized ditaurobilirubin solution, and chemically synthesized delta bilirubin solution were used as surrogates of naturally occurring unconjugated bilirubin, conjugated bilirubin, and delta bilirubin, respectively. The total bilirubin and direct-reacting bilirubin concentrations were measured by three bilirubin oxidase methods and one vanadic acid method, and the observed concentrations were compared with those obtained by the diazo-based reference measurement procedure.The unconjugated bilirubin and delta bilirubin concentrations were similar when any of the fourWe revealed the reactivity of IVD-TB and IVD-DB reagents to artificially prepared bilirubin materials, and their consistency with reference measurement procedure. The delta bilirubin data results vary depending on the reagents used.

Mastoparan is a small peptide composed of 14 amino acid residues found in wasp venom. It penetrates into cytoplasm through the cell membranes and then binds to a G protein to stimulate the release of histamine. Conformation and its thermal stability of mastoparan from Vespula lewisi (MP) in methanol are investigated by using proton nuclear magnetic resonance (NMR) spectroscopy. On the basis of data on NOESY cross peaks, spin-spin coupling constants between an amide proton (NH) and an α-proton, NH chemical shift analyses, and temperature dependence of integrated intensity of NH resonance lines, we found that MP forms the helix between the 5th and 12th residues at low temperatures and the helix segment is maintained even at 54°C. This conformation is similar to that of MP bound to detergent micelles, and hence, methanol is considered to be appropriate as a membrane mimetic for MP. In connection with the function of the venom peptide, significance of high stability of the helical conformation is discussed.

The gelation process of methylcellulose (MC) in light (H2O) and heavy (D2O) waters was investigated using NMR and DSC to elucidate solvent isotope effect on the process. As temperature is raised, MC chains in both solvents undergo the aggregation and subsequent gelation; however, their onset temperatures are lower in D2O than H2O. This demonstrates that D2O enhances the hydrophobic attractive force, which is the driving force for the aggregation and gelation. We propose that the excluded volume effect of the hydrophobic segments in MC chains should play a pivotal role for the enhancement, while, prior to the above investigation, chemical shift assignments of proton and carbon resonances are performed, and six resonances are newly assigned.

The response of a radiation detector fabricated from piezoelectric lead zirconate titanate (PZT) was studied. The response signal due to a single 400 MeV/n xenon (Xe) ion was assumed to have a simple form that was composed of two variables, the amplitude and time constant. These variables were estimated by comparing two output waveforms obtained from a computer simulation and an experiment on Xe beam irradiation. Their values appeared to be dependent on the beam intensity.

Alamethicin is an antibiotic peptide comprising 20 amino acid residues and functions as an ion channel in biological membranes. Natural alamethicins have a variety of amino acid sequences. Two of them, used as a mixed sample in this study, are: UPUAUAQUVUGLUPVUUQQO and UPUAUUQUVUGLUPVUUQQO, where U and O represent α-aminoisobutyric acid and phenylalaninol, respectively. As indicated, only the amino acid at position six differs, and the two alamethicins are referred to as alamethicin-A6 and -U6, respectively. The conformation and thermal stability of alamethicin-A6 and -U6 in methanol were examined using proton nuclear magnetic resonance (NMR) spectroscopy. Both alamethicins form an α-helix between the 2nd and 11th residues. The N-terminal, 19th and C-terminal residues take a non-helical conformation. The structure between the 12th and 18th residues has not been well determined due to the absence of cross peaks in the two-dimensional NMR data. The α-helices are maintained up to 54 °C at least. In contrast to these similarities, it has been found that the length of the α-helix of alamethicin-U6 is somewhat shorter than that of alamethicin-A6, the intra-molecular hydrogen bonds formed by the amide proton of the seventh residue is much more thermally stable for alamethicin-U6 than for alamethicin-A6, and the C-terminal residue of alamethicin-U6 has higher mobility than that of alamethicin-A6. The mobility of the N- and C-terminal residues is discussed on the basis of a model chain which consists of particles connected by rigid links, and the physiological significance of the mobility is emphasized.

Methylcellulose (MC), a hydrophobically modified cellulose derivative, in an aqueous solution undergoes sol-to-gel and gel-to-sol transitions on heating and cooling, respectively. Using differential scanning calorimetry, MC in light (H2O) and heavy (D2O) water solutions has been investigated to elucidate the solvent isotope effect on the transitions. As a result, their transition temperatures are higher in H2O by about 4 °C than D2O. This phenomenon is rationalized in terms of the strength of the hydrophobic attractive interaction; the strength is enhanced by D2O. We discuss the reason for the enhancement and the difference in the isotope effect between MC and a poly(N-isopropylacrylamide) polymer which shows an opposite trend to MC.

This study describes a user-friendly and rapid detection system of oral bacteria in the liquid phase for point of care testing based on magnetic immunoassay. We focused on the dependence of the strength of external magnetic field required to switch the magnetic moments of nanoparticles bound to bacteria on the bacteria concentration. The results obtained indicate that the required field strength increases linearly as a function of log concentration of Porphyromonas gingivalis cultured in the range of 103–109 CFU/mL. Similarly, the required field strengths for Streptococcus mutans and Pseudomonas aeruginosa increase monotonically when their concentrations increase, whereas the required field strength for Escherichia coli decreases monotonically when its concentration increases. We then measured the concentration of Porphyromonas gingivalis in the saliva collected from elderly people in a geriatric health services facility and the results using the developed system had a correlation with those using a commercial bacteria counter.

The precursor protein of localized cutaneous amyloidosis (LCA) is believed to be cytokeratins on the basis of previous immunohistochemical studies. To identify the candidate amyloid protein biochemically, amyloid proteins were extracted with distilled water from lesional skin of LCA associated with Bowen's disease. The proteins were resolved on one- or two-dimensional polyacrylamide gel electrophoresis followed by characterization with immunoblot analysis. The proteins with multiple molecular weights of 50-67 kDa and two proteins with 25 and 35 kDa were identified as keratins, serum amyloid P component and apolipoprotein E, respectively. The unknown 14-kDa (pI = 7.0) and 42-kDa (pI = 5.4) proteins reacted with the antibody against galectin-7 and actin, respectively. The protein with the molecular weight of 14 kDa was identified as galectin-7 by MALDI-TOF mass spectrometer. Their electrophoretic mobilities were identical with normal counterparts extracted from cultured normal human keratinocytes. Galectin-7 and actin were detected by immunoblot assay in the water-soluble fractions prepared from the lesional skins of two patients with primary LCA. Immunohistochemical studies of tumor-associated (n = 9) and primary (n = 10) LCA revealed various degrees of positive immunoreactivities with the antibodies for galectin-7 and F-actin. Galectin-7 and actin, which contain considerable amount of β-sheet structure, may be candidate amyloidogenic proteins of primary and secondary LCA.

Melittin, a peptide of 26 amino acid residues, has been used as a model peptide for protein folding and unfolding, and extensive research has been done into its structure and conformational stability. Circular dichroism (CD) studies have demonstrated that melittin in an aqueous solution undergoes a transition from a helical tetramer to a random coil monomer not only by heating but also by cooling from room temperature (i.e., heat- and cold-denaturation, respectively). The heat-denaturation has been also examined by nuclear magnetic resonance (NMR) experiments, however, no NMR data have been presented on the cold-denaturation. In this paper, using proton ((1)H) NMR spectroscopy, we show that melittin undergoes conformational transitions from the monomer to the tetramer to the monomer by elevating temperature from 2 to 70 °C. Only melittin including a trans proline peptide bond participates in the transitions, whereas melittin including a cis proline one does not. The tetramer has maximum conformation stability at around 20 °C, and cooperativity of the heat-denaturation is extremely low.

The present study examined the index of absorption of trace element ( Fe , Cu , and Zn ) in different semi-solid nourishment medicines. Various mineral compositions were administered to 7-week-old male rats and semi-solid nourishment medicine from three companies, each using a different gelling agent, were orally administered for two weeks (5 per group). Five rats that were that were fed the standard diet were used as a control group. The rats' excrement excreted after the administration the nutritional supplement was gathered, and the density of trace elements was measured by the PIXE method. The trace element value of each semi-solid nourishment medicine and the standard diet were measured before the experiment, and the intake of trace elements was calculated based on these values. The amount of gut absorption was subtracted from the amount excreted. The groups were compared by the index of absorption.

In order to understand the behavior of radionuclides released from the Fukushima Daiichi nuclear power plant, the depth distributions of radiocesium and radioiodine were investigated in a wheat field, a rice paddy, an orchard, and a cedar forest in Koriyama, Fukushima Prefecture. Our results demonstrate that, following the nuclear power plant disaster, more than 90% of the radionuclides were distributed in the upper 6 cm of the soil column in the wheat field and within 4 cm of the surface in the rice paddy, orchard, and cedar forest. According to the measurement of radionuclides in the three adjacent agricultural fields, the variation of deposition densities in the wheat field was smaller than that of the orchard and rice paddy, suggesting that the low permeability of the orchard and paddy soils may cause horizontal migration of radionuclides during the initial deposition. This result indicates that the deposition densities in the wheat field should be appropriate for estimating the amount of fallout in the area. The deposition densities of 134 Cs, 137 Cs, and 131 I in this area were estimated to be 512 ± 76 (SD, n = 5), 522 ± 80 (SD, n = 5), and 608 ± 79 (SD, n = 5) kBq/m 2 (decay corrected to April 1, 2011), respectively. A comparison of the deposition density between the wheat field and the cedar forest suggests that more than half of the radionuclides are distributed in the tree canopies of the evergreen forestland.

Thermal stability of the α-helix conformation of melittin in pure ethanol and ethanol–water mixture solvents has been investigated by using NMR spectroscopy. With increase in water concentration of the mixture solvents (from 0 wt% to ~71.5 wt%) as well as temperature (from room temperature to 60 °C), the intramolecular hydrogen bonds formed in melittin are destabilized and the α-helix is partially uncoiled. Further, the hydrogen bonds are found to be more thermally stable in pure ethanol than in pure methanol, suggesting that their stability is enhanced with increase in the size of the alkyl groups of alcohol molecules. Copyright © 2011 European Peptide Society and John Wiley & Sons, Ltd.

Temperature dependence of the α-helix conformation of bee venom melittin in methanol-water mixed solvents has been examined by NMR, in order to elucidate conformation stability and a phase diagram. At high methanol concentration of 100 - ca. 80 wt.%, melittin forms a full α-helix conformation in the temperature range from 25 °C to 60 °C. At intermediate methanol concentration of ca. 80 - ca. 25 wt.%, it undergoes a thermal transformation from a full α-helix to a partial α-helix. In solutions of low methanol concentrations of ca. 25 - 0 wt.%, partial α-helix monomers and their self-aggregated conformers coexist at low temperatures, and the relative number of the monomers increases with increase in temperature. The monomers turn to a random coil state at high temperatures only below ca. 10 wt. % methanol concentrations. The thermal transitions are discussed from the viewpoint of stability of intra-molecular hydrogen bonds and inter-molecular hydrophobic interactions.

A rapid simultaneous multi-element analysis method for soils and environmental samples has been established using polarizing energy dispersive X-ray fluorescence (EDXRF) spectrometry. The pressed powder pellet technique was adopted because it is simple and requires no specialized skills for sample preparation. The analytes examined were: Na2O, MgO, Al2O3, SiO2, P2O5, K2O, CaO, TiO2, MnO, Fe2O3, V, Cr, Co, Ni, Cu, Zn, Rb, Sr, Y, Zr, Nb, Sn, Sb, Cs, Ba, La, Ce, Pr, Nd, Pb and Th. Twenty-six reference samples were used for the calibrations. Compton scatter radiation was used as an internal standard to compensate for variations in the sample matrix, particle size, packing density and operating characteristics of the instrument. The correlation coefficients of the linear regression lines were >0.98, with the exception of Na2O, MgO, Al2O3, SiO2, P2O5, Co, Pr and Nd. The values obtained using the proposed EDXRF spectrometry were compared with the values obtained using other methods. Out of the 31 analyt...

Serum trace elements were analyzed by PIXE method in a patient with acute aortic dissection during the supportive process by a Nutrition support team (NST). The patient was a 53-year old male who suffered from acute aortic dissection on March 1, 2007. He received emergent Bentall operation and bow pars total displacement. Since he suffered from diarrhea as a result of hypoalbuminemia and bowel dysfunction, enteral nutrition was not sufficient to maintain adequate intake. Therefore, we also used parenteral nutrition until the 97th disease day. Afterwards, the patient managed only with enteral nutrition. We measured serum trace elements during these periods. Serum trace elements such as Fe , Zn and Se were preserved within normal ranges. On the other hand, Cu gradually decreased until the 54th disease day (44 μg/l) and stayed in the lower levels around the detection limit until the 109th disease day. Thereafter, Cu slightly increased and reached 117 μg/l on the 131st disease day (reference range of serum Cu in adult males: 700~1,300 μ g/l ). It was suggested that the serum levels of these trace elements might reflect the nutritional stages of the patient and could be useful as clinical markers for nutritional therapies.

Recently, Nutrition Support Teams (NSTs) has been spreading throughout Japan. Nutritional assessment is important as an initial step among NST activities, since the patients can be identified based on this assessment whether they needs supports by NST or not. Serum trace element is one of the most useful and convenient nutritional indices. The aim of this study is to analyze the relationships between serum trace element values and clinical backgrounds in NST patients by data mining. The subjects of this study consisted of 29 NST patients who were admitted to our hospital between January 2005 and October 2006. Serum trace elements in patients were analyzed by PIXE method. The data were analyzed by a data mining software, i.e. "ICONS Miner" (Koden Industry Co., Ltd.). The significant "if-then rules" were extracted from the decision trees. The target variable of the decision trees is whether nutritional conditions of the patients are improved or not (Yes/No). The explanatory variables of the decision trees are the values in serum trace elements (Fe, Cu, Zn, Se, Mn) and TTR (transthyretin). The analyses demonstrated that the first node of the decision tree was Zn. Therefore, serum Zn value might be the most significant factor among these trace elements in estimating the improvement of nutritional conditions of the patients. In the decision, the second branch was the Fe value, and the Cu the third. The following significant "If-then rules" were extracted from the decision trees. If-then rule 1: If serum Zn value >758.6 µg/l, then improvement of nutritional condition = Y. (1.00 = 9/9) If-then rule 2: If serum Zn value ≤758.6 µg/l and Fe ≤653.2 µg/l and Cu ≤682.5 µg/l, then improvement of nutritional condition = Y. (1.00 = 5/5) If-then rule 3: If serum Zn value ≤758.6 µg/l and Fe ≤653.2 µg/l and Cu >682.5 µg/l and Se >119.8 µg/l, then improvement of nutritional condition = Y. (1.00 = 3/3) In conclusion, data mining analysis of serum trace elements was found to be an effective method in assessing the nutritional conditions in NST patients.

It is known that melittin in an aqueous solution undergoes a conformational transition between the monomer and tetramer by variation in temperature. The transition correlates closely with isomers of the proline residue; monomeric melittin including a trans proline peptide bond (trans-monomer) is involved directly in the transition, whereas monomeric melittin having a cis proline peptide bond (cis-monomer) is virtually not. The transition has been explored by using nuclear magnetic resonance spectroscopy in order to clarify the stability of the tetrameric conformation and the cooperativity of the transition. In the light of temperature dependence of chemical shifts of resonances from the isomeric monomers, we qualitatively estimate the temperature-, salt-, and concentration-dependence of the relative equilibrium populations of the trans-monomer and tetramer, and show that the tetramer has a maximum conformational stability at 30-45 °C and that the transition cooperativity is very low.

Aim: To evaluate surgical indications for combined partial rectosigmoidectomy in ovarian cancer with direct invasion of the rectum and sigmoid colon or dissemination into the pouch of Douglas. Methods: Subjects comprised 25 patients with ovarian cancer who underwent primary surgery and rectosigmoidectomy between 1990 and 2002 at our hospital. Federation of Obstetrics and Gynecology staging of tumors was II (n = 6), III (n = 17) or IV (n = 2). The histologic type was serous adenocarcinoma (n = 18), clear cell adenocarcinoma (n = 4), and others (n = 3). Bowel resection was performed during primary surgery in 18 patients, and after neoadjuvant chemotherapy (NAC) in seven patients. Cumulative survival rate was compared between NAC and non-NAC groups. Patients were divided into three groups based on extent of surgical resection to compare survival rates: no residual tumor (n = 19); maximum residual tumor diameter

Complex formation between vanadate and various ethanolamine derivatives (ethanolamine, diethanolamine, methyldiethanolamine, triethanolamine and ECTEOLA–Cellulose) has been examined in detail by using 51V NMR spectroscopy. Vanadate binds with ethanolamine to form 1:1 (O)-monodentate and (N,O)-bidentate complexes which are protonated and deprotonated forms, respectively. Ethanolamine undergoes a comparatively weak interaction with vanadate relative to the other ligands. 51V NMR spectra clearly show that vanadate reacts with the functional group of ECTEOLA–Cellulose, as well as diethanolamine, methyldiethanolamine and triethanolamine, which are analogues of the functional groups of ECTEOLA–Cellulose, to form the −1 charged 1:1 (N,O,O)-tridentate complex. In addition to anion exchange interaction of monovanadate and isopolyvanadate anions with the protonated functional group, in the alkaline region the adsorbability of vanadium(V) onto ECTEOLA–Cellulose is a consequence of the complexation of vanadate with the functional group. The formation constant of the (N,O,O) complex with ECTEOLA–Cellulose was estimated to be log β ¯ ( N , O , O ) = 3 . 6 , which was almost the same as those with the analogues of the functional group.

We have developed standard-free methods for PIXE analysis of hair, nail, urine and serum, and they have widely been applied to studies on human exposure to some toxic elements caused by pollution in many countries. Although these samples are known to be quite suited for evaluating human exposure to toxic elements, there is a case where it is required to quantitatively analyze other samples taken from people. We have examined sweat, saliva, snivel and tear, which are expected to be useful for estimating concentration of various elements in a human body. However, sufficient quantities of them are difficult to be taken from a human body and it is required to establish standard-free methods for these samples. In the present work, standard-free methods for sweat and saliva were established and its accuracy and reproducibility are confirmed. It becomes possible to quantitatively analyze only a drop of sweat and saliva by means of this method. For snivel and tear, potassium concentration is obtained by the internal-standard method for a small-spot sample and the conversion coefficient required for the standard-free method was evaluated. It is found that analyses of these samples give us useful information about some specific elements. As the standard-free methods are free from dryness of samples, which becomes a serious problem in the case where the internal-standard method is applied, it is expected to give more essential information about elemental concentration in a human body.

Background: Biologically uncommon d-aspartyl residues have been reported in the elderly tissues such as tooth, eye lens, aorta, and brain. We have previously prepared the antibody against d-aspartyl residue-containing peptide and found that it reacted with elastotic material of actinic elastosis. Methods: Immunoreactivity of the normal skins obtained from sun-exposed and sun-protected skins of varied ages with this antibody was studied. Results: In the sun-exposed skins, the antibody showed negative reaction with the skin specimens of young donors, whereas it reacted with elastotic materials of actinic elastosis of the elderly. In the sun-protected skins, the antibody recognized elastic fiber-like structures and inner layer of vessels found from the mid to lower dermis of old donors but showed no positive reaction to skin specimens of young donors. Conclusions: The results suggest that the antibody is a potent marker for chronological and ultraviolet (UV)-induced skin aging. Unusual eosinophilic bodies seen in the superficial dermis in the sun-exposed area of the elderly skins were also immunoreactive with the antibody, suggesting that the eosinophilic bodies resulted from UV-induced skin damage.

The complexation of borate with linear dextrans consisting of pyranoside residues and their monomer derivatives (α-methyl- d -glucopyranoside and α-methyl- d -mannopyranoside) was investigated in detail by using 11 B NMR spectroscopy. For the monomer systems five kinds of borate complexes with α,β-diols and α,γ-diols of the pyranosides were present: that is, (α,β)-monochelate, (α,γ)-monochelate, (α,β)(α,β)-bischelate, (α,γ)(α,γ)-bischelate and (α,β)(α,γ)-bischelate complexes. Borate reacts with dextran to form inter-chain (α,β)(α,β)- and (α,β)(α,γ)-bischelate complexes in the 1:2-complexation in addition to the (α,β)- and (α,γ)-monochelate complexes. The formation of intra-chain bischelate complexes can be negligible for a rather stiff polymer as dextran. Formation constants of the (α,γ)-monochelate complex are almost constant among dextrans with different chain lengths except Dextran 3000 which is the shortest polymer examined. On the other hand, the stability of (α,β)-monochelate complexes decreases with an increase in the chain length. The complexation behavior for polysaccharides with various chain lengths was discussed in correlation with hydrodynamic and steric hindrance of the polymer ligands.

Ion exchange distribution of the phenylphosphoric acid has been studied on various types of chloride form strong base resins as a function of pH at 25 degrees C, at 0.1 M ionic strength. Equilibrium measurements were supplemented by the study of pH dependence of the (31)P NMR spectra of the resin-phase phenylphosphate species. Equations were derived to describe the pH dependence of the overall distribution coefficient and the chemical shift of the resin-phase solute species. Experimental data were evaluated by using these model equations and the values of the individual distribution coefficients, ion exchange selectivity coefficients and the resin-phase (31)P chemical shifts of the mono- and divalent ions have been calculated. Comparison of distribution data of the individual species corroborated the significance of the role of hydrophobic interaction in the selectivity of organic ion exchange processes. A well-defined correlation between the ion exchange selectivity and the resin-phase (31)P NMR chemical shift data has been pointed out.

A number of considerations suggest that trace element disturbances might occur in patients with renal disease and in hemodialysis (HD) patients. Using particle induced X-ray emission, we demonstrated the relations between serum concentration, urinary excretion of the trace elements and creatinine clearance (Ccr) in randomized 50 patients. To estimate the effects of HD, we also observed the changes of these elements in serum and dialysis fluids during HD. Urinary silicon excretion decreased, and serum silicon concentration increased as Ccr decreased, with significant correlation ( r =0.702, p r =0.676, p r =0.452, p

In 30 healthy persons (control), 17 renal cell carcinoma (RCC) patients, 30 hemodialysis patients (HD) and 15 healthy persons in the Takko town (Aomori prefecture), the selenium concentration in serum was determined by PIXE. The mean serum selenium concentration in healthy controls was 1.4 ± 0.6 μ mol/l , in RCC patients 1.1 ± 0.4 μ mol/l , in HD patients 1.3 ± 0.9 μ mol/l and in healthy persons in the Takko town 1.7 ± 0.7 μ mol/l . There was a significant statistical difference between RCC patients and healthy persons in the Takko town ( p < 0.05). Takko town is famous for the production of garlic. Epidemiological studies have established an inverse relationship between garlic consumption and incidence of gastric, colon, and laryngeal cancers. Garlic is a rich source of selenium in the food. Contents of selenium in normal and carcinoma fractions in kidneys of RCC patients were determined by PIXE. The results indicate that RCC patients caused significant decrease of selenium contents in the carcinoma fraction ( p < 0.05).

A standard-free method of quantitative analysis, which is based on the fact that the total yield of continuous x-rays from the sample approximately corresponds to effective weight of the sample, was developed and has been applied to some typical bio-samples such as serum, whole blood, hair and untreated bone. In this work, the standard-free method was applied to untreated urine samples. This method allows us to perform sample preparation only by dropping 5 μl of urine sample onto a backing film. It requires neither a large amount of urine nor the internal standard. As the results, values of concentration of potassium for 4 samples agree well with the value obtained by the internal standard method within an error of 10%. The present method was also applied to 21 urine samples containing excess amount of urinary protein and / or sugar, and it is found that the present method is applicable to such abnormal urines. Owing to this method, target preparation can be performed at the place and time of sampling. It is quite convenient to environmental studies.

The complex formation of aluminum(III) with phosphinate and phosphite ions in acidic solutions (pH 1–3) has been investigated by 27 Al NMR spectroscopy. The formation of a 2:2 complex was established in addition to ordinary stepwise complexes in both Al 3+ -PH 2 O 2 − and –PHO 3 2− systems. Formation constants of these complexes formed in both systems, and thermodynamic quantities for the complexation in the Al 3+ -PH 2 O 2 − system were determined at an ionic strength of 1.0 mol dm −3 NaClO 4 . The stepwise complexation up to 1:3 becomes more exothermic and less entropy-productive in a regular manner. Both Δ H ° and Δ S ° values for the 2:2 complexation are quite large and positive due to the dimerization.

In hemodialysis (HD) patients, an accumulation of trace elements such as aluminum, copper, silicon and vanadium has been reported. Aluminum-caused encephalopathy and aluminum-related bone diseases are important trace element-related complications. Using particle induced X-ray emission (PIXE) we determined concentrations of aluminum, silicon, copper, zinc, selenium and bromine in sera of 29 patients with HD, 14 nondialysis patients with renal disease (RD) and 27 normal controls. The concentration of serum silicon of the patients with HD was 107.4 ± 61.3 μmol/l, which is markedly higher than that of normal controls (48.3 ± 25.8 μmol/l, p p p p

Silicon levels in dialysis patients are markedly increased. Using PIXE we determined the relationship between silicon concentration and creatinine clearance in 30 samples. Urine silicon concentration were significantly correlated to creatinine clearance (p

Emissions of trace gases (CO2, CO, CH4, N2O) resulting from rice straw burning were measured by using the open chamber method. The carbon contained in rice straw was mainly released to the atmosphere as CO2. The percentage of CO2-C emitted in total C in rice straw was in the range of 57–81%, followed by CO-C (5–9%). The percentages of CH4-C and N2O-N in total C and N in rice straw were in the range of 0.43–0.90 and 1.16–1.50%, respectively. In the case of the rice straw which had been left in the field for a period of one month after harvest, emission of imperfect combustible gases such as CO and CH4 during burning increased slightly, while that of perfect combustible gas, CO2, was reduced. The amount of CH4 emission from rice straw burning was comparable to that from paddy fields.

Internal Standard Method, which has been widely used for quantitative analysis of general bio-samples, requires certain skill in sample preparation since it sometimes accompanies a noticeable error due not only to inaccuracy of weight measurement both of a sample and of an internal standard but also to nonuniformity of the internal standard in the target. In this work, a standard-free method of quantitative analysis, based on the fact that the total yield of continuous x-rays from the sample approximately corresponds to effective weight of the sample, has been developed and applied to some typical bio-samples (NIST Bovine liver, a rat liver and a human serum). As a result, values of concentration obtained by the present method present good agreement with those obtained by the internal standard method. Further, in a case where target preparation is performed by unskilled person, the present method gives better results than those obtained by the internal standard method. It is also found that this method is applicable to almost all soft-tissue samples and, moreover, to targets prepared by a different method.

Little information is available regarding the influence of non-ionic low-osmolar iodinated contrast medium (CM) in stored blood on the quality of blood components. We sought to evaluate the quality of such CM-contaminated blood in terms of the degree of hemolysis, production of microaggregates, level of iodine concentration, and RBC shape, and to identify the pros and cons of autologous blood donation immediately after X-ray examination using CM. In conclusion, contamination by such CM in blood collected around 2h after the completion of X-ray examination appears unlikely to induce deleterious effects on blood components.

BACKGROUND The angiotensin I-converting enzyme (ACE) is a key component of the renin-angiotensin system thought to be important in the pathogenesis of hypertension and cardiovascular disease. Deletion polymorphism in the ACE gene may be a risk factor for myocardial infarction in the Caucasian population. However, this finding has not yet been investigated in the Japanese population. METHODS AND RESULTS A 287-bp insertion/deletion polymorphism in intron 16 of the ACE gene was examined by polymerase chain reaction in a cross-sectional study of 100 healthy subjects and 178 patients with coronary artery disease (CAD) (70 angina pectoris, 108 myocardial infarction), whose serum ACE levels were concomitantly measured. Polymorphism of the ACE gene was characterized by three genotypes: two deletion alleles (genotype DD), two insertion alleles (genotype II), and heterozygous alleles (genotype ID). No differences could be detected among the three genotypes for total cholesterol, HDL cholesterol, and body mass index. Serum ACE levels were 11.4 +/- 2.7, 14.5 +/- 3.5, and 16.6 +/- 4.6 IU/mL for genotypes II, ID, and DD, respectively. In the study population, the genotype DD was more closely associated with CAD than the other two genotypes (ID and II). The frequency of deletion alleles was higher (0.58) in the CAD group than in healthy control subjects (0.42) (P < .05). Furthermore, multivessel disease was more strongly associated with deletion alleles than with insertion alleles (P < .05). CONCLUSIONS A deletion polymorphism of the ACE gene is associated with serum ACE activity and increased risk for CAD in the Japanese.

Using PIXE we determined concentrations of iron, nickel, copper, zinc, selenium, and rubidium in sera of 24 patients with acute myocardial infarction and 12 healthy controls. Rubidium*, selenium*, zinc**, nickel** and iron** concentrations are significantly (P

The effects of the application level of rice straw and percolation rate on the leaching amounts of methane, total water soluble organic carbon (TOC), hexose, Fe2+, and Mn2+ with percolating water were investigated in a soil column experiment. The amount of methane in the leachate was larger as the application level of rice straw (0.3–1.0 × 10-2 kg kg-1) increased. The methane concentration in the leachate reached a saturation level around the 18th day after incubation in the 0.6 and 1.0 × 10-2 kg kg-1 rice straw treatments, and remained at the same level afterwards. In the treatments with percolation rates of 0.26, 0.52, and 1.0 cm/d, the methane concentration in the leachate did not change. The total amounts of methane percolated during a 30 d period corresponded to ca. 3, 7, and 15% of the estimated methane production from rice straw in a whole crop season, respectively. The amounts of percolated TOC, hexose, Fe2+, and Mn2+ also increased with the increase of the application level of rice straw...