The Tohoku Journal of Experimental Medicine
Online ISSN : 1349-3329
Print ISSN : 0040-8727
ISSN-L : 0040-8727
Volume 178, Issue 1
January
Displaying 1-10 of 10 articles from this issue
Sendai Symposium: Medico-Biological Application of Plasma Ionization Source Mass Spectrometry
  • Akiko Ejima, Chiho Watanabe, Hiroshi Koyama, Hiroshi Satoh
    1996 Volume 178 Issue 1 Pages 1-10
    Published: 1996
    Released on J-STAGE: November 21, 2006
    JOURNAL FREE ACCESS
    To investigate the roles of various elements in neurological disorders, multi-element analysis of limited quantities of samples in the central nervous system is required. Inductively coupled plasma-mass spectrometry (ICP-MS) analysis suits this requirement, but spectral and non-spectral interferences are inevitable. We studied correction methods for the non-spectral interferences by analyzing signals of 21 elements in various concentrations of HNO3 as well as 5 major elements (Na, K, P, Ca, and Cl). Using internal standards, the interferences caused by the major elements were corrected, but the interferences caused by HNO3 were impossible to correct for the elements with high ionization potentials. Thus, we decided to use a standard addition method to correct these interferences. The spectral interferences on Mn and Fe rising from HNO3 or major elements were compared with the signals of samples. Although the interferences on Mn were negligible, those on Fe were considerable and careful blank subtraction were needed. We measured concentrations of elements in the spinal cord of 4 controls and a patient with amyotrophic lateral sclerosis (ALS) using the standard addition method. The concentrations of Mn, Se, Fe, and Zn in the controls were nearly the same as previously reported values, whereas Mn concentrations in the ALS patient were higher.
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  • Takeshi Saito, Kazuo Saito
    1996 Volume 178 Issue 1 Pages 11-16
    Published: 1996
    Released on J-STAGE: November 21, 2006
    JOURNAL FREE ACCESS
    We examined the method of sample digestion and the analytical conditions for simultaneous multi-determination of trace element concentrations by inductively coupled plasma mass spectrometry (ICP-MS) in biological samples. In order to eliminate contaminations by extraneous elements from reagents and instruments, we chose plastic tubes and a Teflon decomposition vessel and super pure grade nitric acid for sample decomposition. Furthermore, standard solutions were prepared by mixing stock solutions of trace elements with a mixture of sample solutions to eliminate matrix interference. Quality control measurements using a standard reference material (SRM bovine liver) showed that the multi-analysis method established in the present study is very accurate and useful for determination of trace element concentrations in biological samples. Using this procedure, we determined the distribution of Zn, Cu, Rb, Mn and Mo in seven discrete regions of the rat brain and Zn and Mn in their synaptosomal fractions.
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  • Hiroshi Koyama, Yuichi Kasanuma, Choong-Yong Kim, Akiko Ejima, Chiho W ...
    1996 Volume 178 Issue 1 Pages 17-25
    Published: 1996
    Released on J-STAGE: November 21, 2006
    JOURNAL FREE ACCESS
    The distribution of selenium in human plasma has been investigated by high performance liquid chromatography (HPLC) connected directly to inductively coupled plasma mass spectrometry (ICP-MS). Human plasma was loaded on to a size exclusion column and eluted with 0.01 M sodium phosphate buffer (pH 7.0) at a flow rate of 0.6 ml/min. Four peaks of selenium were detected in the chromatogram. The first selenium peak was obtained in the void volume. The retention time of the third peak was in accord with that of bovine serum albumin as a standard. The forth peak was thought to be a ghost. The method was applied to identify the chemical form of selenium in blood plasma immediately after intestinal absorption. The chromatographic pattern of selenium in postprandial human plasma was compared with that in fasting plasma. The first and third peaks in the postprandial plasma sample were slightly higher than those in the fasting plasma sample. This finding suggests that absorbed selenium is associated with the high molecular weight fraction and mercaptalbumin in blood plasma.
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  • Kazuo T. Suzuki
    1996 Volume 178 Issue 1 Pages 27-35
    Published: 1996
    Released on J-STAGE: November 21, 2006
    JOURNAL FREE ACCESS
    High performance liquid chromatography (HPLC)/inductively coupled argon plasma-mass spectrometry (ICP-MS) was introduced to investigate the distributions of selenium (Se) in biological fluids. The method was to determine both the natural abundance of Se and an enriched stable isotope of Se used as a tracer. The distributions of Se in plasma and in urine specimens were determined in Wistar rats on various Se diets with and without an intravenous injection of 82Se-selenite. Although the distribution of natural abundance Se (endogenous Se) in the plasma was affected little by the nutritional status of Se, that in the urine gave a Se peak depending on the nutritional status of Se, and the peak was identified as methylselenol. When 82Se-selenite was injected in excess into rats given three different Se diets (Se-deficient, Se-adequate, Se-excessive), three Se peaks occurred in the HPLC chromatogram of the urine samples, corresponding to selenite, methylselenol and trimethylselenonium ion in the order of elution, and the intensities of the tracer peaks reflected the nutritional status. These results indicate that the HPLC/ICP-MS method is a powerful analytical tool for specifying Se-containing biological constituents, both natural abundance and enriched stable isotopes. Methylselenol in urine is proposed to be a sensitive and Se-specific biological indicator for diagnosing the nutritional status of Se. Furthermore, it was shown that an enriched stable isotope such as 82Se-selenite was shown to be used for the same purpose, and that 82Se-methylselenol and 82Se-trimethylselenonium ion in urine were more sensitive indicators of the Se status of the rats.
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  • Jun Yoshinaga
    1996 Volume 178 Issue 1 Pages 37-47
    Published: 1996
    Released on J-STAGE: November 21, 2006
    JOURNAL FREE ACCESS
    Inductively coupled plasma mass spectrometry (ICP-MS) allowed 0.2-0.3% imprecision (1 sigma) in 204Pb/206Pb, 207Pb/206Pb, and 208Pb/206Pb measurements at the 20-100 ppb level, which was precise enough to detect some of the isotopic variations observed in nature. Mass discrimination could be corrected within ±0.5% of the true value by periodical analysis of standard reference material of known lead isotopic composition. As a separation method for lead in human bone, which contains enormous amounts of calcium and phosphorus, anion exchange of the Pb-Br complex was found to be effective. Lead isotope ratios in bone, measured by ICP-MS after separation, were consistent with those measured by thermal ionization mass spectrometry. Hair matrix did not have any influence on the accuracy and precision of the analysis; a digested sample could be directly analyzed and this offered rapid sample throughput. Preliminary data on lead isotope ratios in bone and hair from prehistoric and contemporary Japanese are presented.
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  • Momoko Chiba, Atsuko Shinohara, Kazuko Matsushita, Hiromi Watanabe, Yu ...
    1996 Volume 178 Issue 1 Pages 49-62
    Published: 1996
    Released on J-STAGE: November 21, 2006
    JOURNAL FREE ACCESS
    Seventy male factory workers were studied. The lead concentrations in their blood (Pb-B) were 16.55±11.53 μg/100 ml (range 1.5 to 50.2 μg/100 ml). The subjects were divided into three groups according to Pb-B (in μg/100 ml): group A, Pb-B ≤10 (n=22); group B, 10<Pb-B ≤20 (n=30); group C, Pb-B >20 (n= 18). The mean±S.D. in each group was 5.57±2.53, 15.02±2.75, and 32.52±9.49 μg/100 ml, respectively. Pb in plasma was 0.011±0.010, 0.017±0.033, and 0.021±0.021 μg/liter, and Pb in the RBC was 0.281±0.246, 0.701±0.325, and 1.626±0.861 μg/g Hb, respectively. In addition to Pb concentration, the concentrations of 34 elements in the plasma or in the RBC were determined. Se concentrations in RBC in each group were 0.618±0.139, 0.670±0.207, and 0.728±0.200 μg/g Hb, and the mean values were significantly different between groups A and C (p<0.05). For Se concentrations in plasma, the mean±S.D. in each group was 0.132±0.035, 0.130±0.031, and 0.126±0.021 μ g/ml, respectively, and there was no significant difference between groups. On the other hand, when the activities of total SOD, Mn-SOD, Cu, Zn-SOD, and catalase in the plasma and the activities of GSR-Px both in the plasma and in the RBC were assayed, some differences were found. The activities in GSH-Px in RBC were 17.19±5.03, 17.59±3.95, and 15.25±3.18 μmol/g Hb/min, and those in plasma were 0.069±0.032, 0.081±0.023, and 0.080±0.028 μmol/ml/min. In group C, GSR-Px activity was lower in the RBC and higher in the plasma than those in group A, and it was observed that the Se concentration was higher in RBC, and that there was no remarkable change in the plasma. Catalase activity in group C was 3.58±0.81 mgH2O2/ml/30 min, which was significantly higher than that in group A (2.81±0.90 mg H2O2/ml/30 min). Further investigation is necessary in order to explain the above results. The regular indices used for evaluating lead exposure, showed significant correlations with Pb-B: r=−0.786 vs δ-Aminolevulinic acid (ALA) dehydratase activity in blood, r=0.927 vs. inhibition rate, and r=0.339 vs. ALA in urine.
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  • Eiji Fujimori, Yuko Tomosue, Hiroki Haraguchi
    1996 Volume 178 Issue 1 Pages 63-74
    Published: 1996
    Released on J-STAGE: November 21, 2006
    JOURNAL FREE ACCESS
    Rare earth elements (REEs) in a blood serum reference sample, which is a freeze-dried sample issued from the National Institute for Environmental Studies, Japan, have been determined by inductively coupled plasma mass spectrometry (ICP-MS) after sample digestion and concentration pretreatment. The freeze-dried serum sample (ca. 0.8 g), which corresponded to 10 ml of original blood serum, was digested with HNO3 with heating on a hot plate. The digested sample was then diluted with 100 ml of 0.1 M HNO3, and REEs in the diluted solution were adsorbed on chelating resin (Chelex® 100). The resin was then filtered with a glass filter. Finally, REEs on the resin were dissolved with 10 ml of 2 M HNO3 aqueous solution, and the sample solution was analyzed by ICP-MS. The concentrations of all the REEs were successfully determined by the present method. The recovery values for REEs were in the range of 70-80%, and the relative standard deviation of the recovery values in repeated experiments (n=3) was less than 5% for all REEs. In addition, 20 other elements were also determined by ICP-MS and ICP-AES.
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  • Ryuji Mizushima, Mitsuru Yonezawa, Akiko Ejima, Hiroshi Koyama, Hirosh ...
    1996 Volume 178 Issue 1 Pages 75-79
    Published: 1996
    Released on J-STAGE: November 21, 2006
    JOURNAL FREE ACCESS
    The analysis of trace elements in biological samples is essential to extend our knowledge on human health and disease. Inductively coupled plasma mass spectrometry (ICP-MS) makes it possible to simultaneously determine these elements in trace amounts. Before analysis, however, biological samples such as organs and tissues must be liquefied and extra organic materials must be decomposed by acid digestion. We established a method of microwave digestion using dual PTFE containers to minimize the amount of samples. Samples (35-45 mg) of standard reference materials, bovine liver (1577a, NIST) and fish flesh (MA-A-2, IAEA), were weighed in PTFE-PFA vials and a small amount of nitric acid (0.5 ml) was added. The vials were sealed and two PTFE-PFA vials were placed in a PTFE-TFM vessel containing 6 ml of pure water. Then the vessels were placed in a rotor and the samples were digested for 38 min in a microwave oven according to a pre-set program. After the program was completed, the samples were analyzed by ICP-MS. The determined values of elements of the microwave-digested samples matched the certified values of the standard reference materials. Therefore, the digestion using dual containers was successfully applied to small samples.
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  • Toshihiro Shirasaki, Jun Yoshinaga, Masatoshi Morita, Toyoharu Okumoto ...
    1996 Volume 178 Issue 1 Pages 81-90
    Published: 1996
    Released on J-STAGE: November 21, 2006
    JOURNAL FREE ACCESS
    Nitrogen microwave-induced plasma mass spectrometry was studied for its applicability to the isotope dilution analysis of selenium in biological samples. Spectroscopic interference by calcium, which is present in high concentrations in biological samples, was investigated. No detectable background spectrum was observed for the major selenium isotopes of 78Se and 80Se. No detectable interferences by sodium, potassium, calcium and phosphorus on the isotope ratio 80Se/78Se were observed up to concentration of 200 mg/ml. The method was applied to the analysis of selenium in biological reference materials of marine organisms. The results showed good agreement between the certified and found values.
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  • Nobuhiko Onda
    1996 Volume 178 Issue 1 Pages 91-99
    Published: 1996
    Released on J-STAGE: November 21, 2006
    JOURNAL FREE ACCESS
    By the use of a new simultaneous dual stage discrete detector for inductively coupled plasma-mass spectrometry (ICP-MS), a linear dynamic range of 8 orders of magnitude was achieved in a single spectral scan. The design of the detection system and its evaluation are described. The acquisition of the full spectrum of a human urine sample in a single scan is shown.
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