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| 1.
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Hayakawa, Kazuichi ; Miyoshi, Yasuko ; Kurimoto, Hiroaki ; Matzushima, Yuko ; Takayama, Nariaki ; Tanaka, Seishi ; Miyazaki, Motoichi ; 早川, 和一 ; 三好, 裕子 ; 栗本, 博昭 ; 松島, 優子 ; 高山, 成明 ; 田中, 星司 ; 宮崎, 元一
概要:
金沢大学理工研究域自然システム学系<br />A HPLC determination method for methamphetamine (MA) and its metabolites in the urine samples of
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abusers has been developed. MA, amphetamine (AP), norephedrine (NE), p-hydroxymethamphetamine (pOHMA), p-hydoroxyamphetamine (pOHAP) and an internal standard, namely β-phenylethylamine (PEA) were derivatized with dansyl chloride. They were separated on a reversed phase column with gradient elution using an acetonitrile/tetrahydrofuran/imidazole buffer mobile phase and chemilumigenically determined using bis(2, 4, 6-trichlorophenyl)-oxalate/hydrogen peroxide as post column reagents. The lower determination limits were as low as 1×10-14-3×10-14mol. AP, NE, pOHAP and PEA were derivatized with naphthalene-2, 3-dicarboxaldehyde, and were separated on a reversed phase column using an acetonitrile/imidazole buffer mobile phase and chemilumigenically determined. The lower determination limits were 3×10-16-1.5×10-15mol. Enzymatic hydrolysis of glucuronides of pOHMA (pOHMAG) and pOHAP (pOHAPG) allowed them to be determined as pOHMA and pOHAP, respectively. After adjusting the pH of the urine samples to 10.5 and adding PEA, all metabolites except glucuronides were extracted quantitatively into chloroform-isopropanol (3 : 1). Utilizing the two methods, MA and all metabolites were determined in urine samples of MA abusers. The tendency, in order of decreasing concentration was : [MA]>[A]>[pOHMAG]>[pOHMA]>[NE]>[pOHAPG]>[pOHAP]. Although ephedrine (EP) was detected in several samples, it was not considered to be a metabolite of MA but rather a component derived from cough medicine.
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| 2.
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早川, 和一 ; 山本 , 敦 ; 宮崎, 元一 ; Hayakawa, Kazuichi ; Yamamoto, Atsushi ; Miyazaki, Motoichi
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早川, 和一 ; 宮崎, 元一 ; Hayakawa, Kazuichi ; Miyazaki, Motoichi
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木津, 良一 ; 濱木, 路子 ; 下沢, 充子 ; 宮崎, 元一
概要:
A method for the determination of platinum in biological materials by using nickel as an internal standard was establish
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ed.Ten μg of nickel was added to samples which contained platinum.Nickel spiked sample was digested with nitric acid and hydrogen peroxide. Acid digest was evaporated to dryness and the residue was dissolved in 0.5ml of IM nitric acid. The amount of platinum was measured byflameless atomic absorption spectrophotometer using background correction with deuterium Iamp, Nickel was measured by flame atomic absorption spectrophotometer. The amount of platinum measured was corrected by the amount of nickel measured.Limit of detection of platinum in the proposed method was 0.05 ppm and the calibration curve showed good linearity in the range from 0.1 to 2.0 ppm. The method is advantageous in reducing sample size and making highly sensitive analysis of p-atinum possible.Correction for the loss of p-atinum resulted from bumping or pretreatment of sample is also easy.The method will be helpful in determining platinum in pharmacological and pharmacokinetic studies of various antineoplastic platinum complexes.
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| 5.
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今成, 登志男 ; 大久保, 登 ; 早川, 和一 ; 宮崎, 元一
概要:
生体試料中の金属を電気透析試料調製器によって陽イオンとして直接抽出する方法(A法)とEDTA-金属錯体として陰イオンとして抽出する方法(B法)について条件の検討を行った. A法の条件は泳動液0.05N酢酸,電流密度15mA/cm2,抽出時間
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(20～40)分,B法の条件は泳動液0.05N水酸化アンモニウム-1m M EDTA,電流密度20mA/cm2,抽出時問(20～40)分であった.A法では鉄(III),銅(II)の回収率80%,亜鉛(II)の回収率は90%,一方B法については鉄(III),亜鉛(II)の回収率100%,銅(II)の回収率は95%であった.たん白質として牛血清アルブミン,電解質として塩化ナトリウムの共存の影響を調べた後,B法を血しょう中のアルブミン結合亜鉛の分析に応用した. The extraction of metals from biological materials by an electrodialytic sample preparator was studied. Two procedures are proposed in this method : one depends on the extraction of metals as cationic ions (Mode A) and the other depends on the extraction of metal-EDTA complexes as anionic ions (Mode B). The basic conditions for Mode A are : carrier solution; 0.05 N CH3COOH, current density; 15 mA/cm2, extraction time; (2040) min. The conditions for Mode B are : carrier solution; 0.05 N NH4OH-1 mM EDTA, current density; 20 mA/cm2 and extraction time; (2040)min. The recoveries of Fe(III), Cu(II) and Zn(II) in Mode A were 90, 80 and 90%, and in Mode B the recoveries were 100, 95 and 100% respectively. The effects of electrolytes and proteins on the extraction of metals were examined, and the application of Mode B for the determination of albumin bound zinc in human plasma was carried out as follows : the supernatant containing albumin bound zinc was obtained by polyethylene glycol treatment and subjected to electrodialysis for 40 min according to the conditions described in Mode B. Albumin bound zinc in the extract was determined by atomic absorption spectrometry (AAS). Total plasma zinc was measured according to direct dilution method by AAS and α2-macroglobulin bound zinc was obtained by the difference.
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山本, 敦 ; 松永, 明信 ; 関口, 久義 ; 早川, 和一 ; 宮崎, 元一
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Photometric ion chromatography is a novel method by using the photometer as a detector. A feature of this method is the use of light absorbing ion in the mobil phase, and the appearance of transparent sample ion in the effluent is
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detected by "trough"in the base line absorbance. We applied this technique by using a conventional HPLC system equipped with a commercially available ion exchange separation column to the determination of bromate in such foodstuffs as bread and kamaboko. Sample solution was prepared by aqueous extraction and mixed with acetone for removal of proteins. After evaporation of the organic solvent, the aqueous solution was dechlorinated by a DOWEX column (Ag-form), and then was subjected to chromatography. Samples of bread and kamaboko were spiked with 5.4 ppm and 8.4 ppm of bromate, respectively, and examined by the above method. The average recoveries were 88.3% in bread and 82.9% in kamaboko, and the coefficients of variation were 7.7% and 7.9%, respectively. The detection limit was 1 ppm. The above findings indicate that bromate can be detected by HPLC using conventional instrumentation, and the sensitivity of this system is comparable to conductimetric detection.
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| 7.
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早川, 和一 ; 山本, 敦 ; 宮崎, 元一
概要:
Ion chromatography (IC), which was introduced in 1975, has become widely used for the sensitive and simultaneous determination of ions. In the early stage, the IC system consisted of two ion-exchange columns (separator and suppressor,
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respectively) and a conductivity detector. Although this combination is still the most popular, new forms of separation and suppression have been developed. On the other hand, an indirect photometric detection using a UV detector has become popular in IC and other detectors commonly used in HPLC also have been used. Each of them has specific advantages for different types of analyses. Thus, IC is now defined as a form of liquid chromatography of ions. This article reviews new developments of the different forms of IC and their applications, especially to environmental samples, foods, biological materials and drugs, from reports published since 1990.
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| 8.
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吉田, 育世 ; 早川, 和一 ; 宮崎, 元一
概要:
Simultaneous determination of carboxylic acids and inorganic anions was investigated by photometric ion chromatography w
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ith phthalate solution as an eluent. The retention time and the peak area of carboxylic acids changed remarkably with eluent pH. The optimum conditions at present were as follows : analytical column, OYOBUNKO ASA-4000 (4.6 mm i.d.×25 cm) ; eluent, 5×10-4 M disodium phthalate ; flow rate, 2 ml/min ; column temperature, 40°C ; detection wavelength, 240 nm ; injection volume, 100 μl. The detection limits for several carboxylic acids as 3 times noise were 0.05-0.07 mg/l in sample solution. Their calibration curves showed straight lines by the peak area method. The present method has an advantage to determine simultaneously not only carboxylic acids but also inorganic anions. Under the condition described above, both carboxylic acids and inorganic anions in several liquid foods were easily determined by direct injection of the sample prepared with only dilution.
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| 9.
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松永, 明信 ; 山本, 敦 ; 水上, 英一 ; 早川, 和一 ; 宮崎, 元一
概要:
A high-performance liquid chromatographic method using post column reaction system was established for the determination
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of polyphosphates (PP). Linear polyphosphates with the range of polymerization from 2 to 9 (P2-P9) could be separated on an anion exchange column, TSK GEL DEAE-5PW (Toyo Soda), with 0.01 M HNO3 containing NaNO3 as a mobile phase at flow rate of 1.0 ml/min, with a linear gradient in NaNO3 concentration at one hour intervals. PP were detected as the decrease of absorbance at 500 nm of ferric-sulfosalicylate complex by means of an on-line post column reaction at room temperature, with 0.5 mM FeCl3 containing 2.5 mM sulfosalicylic acid as reaction reagent at flow rate of 0.5 ml/min. The proposed method was applied to the analysis of 30 different commercial products of soft drinks. The pretreatment only necessary after mixing the sample with an equal volume of 0.01 M HNO3 was filtration through 0.45 μm pore size filter. P2-P6 (total 0.231 g/kg) and P2-P4 (0.070 g/kg) were found from 2 kinds of the samples, respectively. The determination limit was 0.02 m mol/kg for all of the PP.
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| 10.
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宮崎, 元一 ; 早川, 和一 ; 飯田, 寿恵 ; 藤井, ちず子
概要:
A simple method by using a column packed with Amberlyst-15 resin was established to remove metal ions which affect on PO
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V and TBA tests for lipid peroxidation. A methanol solution (2 ml) of lipid containing metal ions was applied to the column (0.5 cm×5 cm), and eluted with methanol (6 ml). Metal ions such as Cu2+, Fe3+ and Mn2+ were retained on the column, whereas linoleic acid, linolenic acid and methyl linolenate were completely recovered in the eluate (8 ml). By testing the peroxidized lipid with POV and TBA methods, the recoveries of the lipid mixture after the procedure were more than 85% (POV) and more than 99% (TBA). This pretreatment by using Amberlyst-15 column is available for the peroxidation tests of lipid.
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