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Hayakawa, Kazuichi ; Miyazaki, Motoichi
概要:
A HPLC method with peroxyoxalate-chemiluminescence (CL) detection has been developed for the determination of dinitropyrenes (DNPs) and nitropyrene (NP). Both DNPs and NP, which are CL-insensitive, were initially reduced to the
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corresponding amino-derivatives with sodium hydrosulfide. They were separated on a reversed-phase column and chemilumigenically determined with detection limits in the subfmol range. Utilizing this method, DNPs and NP were determined in gasoline and diesel particulate samples.
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| 2.
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Hayakawa, Kazuichi ; Kitamura, Ryuichi ; Butoh, Mizuka ; Imaizumi, Noriko ; Miyazaki, Motoichi
概要:
A high performance liquid chromatographic (HPLC) method with chemiluminescence (CL) detection was developed for the sens
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itive determination of 1, 3-diaminopyrene (1, 3-DAP), 1, 6-DAP, 1, 8-DAP and 1-aminopyrene (1-AP). The HPLC conditions were as follows: column, Cosmosil 5C18 (4.6mm i.d.×250mm); mobile phase, 10mM imidazole- perchloric acid buffer(pH 7.6)-acetonitrile (1:1, v/v); CL reagent, 0.02mM bis(2, 4, 6-trichlorophenyl)oxalate (TCPO) and 15mM hydrogen peroxide in acetonitrile. The oxidative degradation of DAPS and AP in the presence of metals was prevented by adding ascorbic acid to sample solutions. The calibration curves were straight over 2 orders of magnitude for all analytes, and their detection limits (as S/N was 3) were in the sub-fmol range. Dinitro- and nitropyrenes in sooty emissions of diesel- and gasoline-engine cars could be determined by this HPLC after reductive conversion into DAPs and AP, respectively, by refluxing the samples in the presence of sodium hydrosulfide.
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Imaizumi, Noriko ; Hayakawa, Kazuichi ; Okubo, Noboru ; Miyazaki, Motoichi
概要:
A selective, sensitive and accurate determination of sulfite was proposed by high performance liquid chromatography (HPL
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C). The sulfite was converted quantitatively to an adduct by reacting with a triphenylmethane dye, malachite green (MG). The formation of adduct was complete, and the adduct was stable at the experimental conditions. Then, the adduct was submitted to HPLC. The working curve for sulfite was linear in the range from 2.0×10-12 mol upto 1.2×10-9 mol.
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| 4.
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早川, 和一 ; 平木, 博美 ; 宮崎, 元一
概要:
金沢大学医薬保健研究域薬学系<br />入手が容易なイオン交換カラムを備えた普及型HPLC装置で可能な,無機陰イオンの微量分析条件を検討した.無機陰イオン(炭酸イオン,塩化物イオン,亜硝酸イオン,リン酸イオン,臭化物イオン,硝酸イオン,硫酸
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イオン,ヨウ化物イオン)は,フタル酸二ナトリウム溶液を溶離液として,陰イオン交換カラムで分離溶出された後,ベースラインの谷として紫外検出される.炭酸イオン,塩化物イオン,リン酸イオン,臭化物イオン,硝酸イオン,硫酸イオンの同時分析の最適条件は,カラム:Zipax SAX (2.1 mm i.d.×50cm):溶離液:5×10^<-4> Mフクル酸二ナトリウム;流速:1 ml/min; 温度:室温;検出波長:240 nm;注入量:100μlであった.この条件で,検出下限はppbレベルであり,ピーク高さ法と面積法のいずれでも検量線は直線となった.本法を用いると,環境試料中の主要無機陰イオンが短時間に一斉分析でき,しかも本法の分析値は,他法の結果ともよく一致した. A photometric determination method of microamounts of inorganic anions has been developed by conventional high performance liquid chromatography using a popular ion exchange column. Inorganic anions (HCO_3^-, Cl^-, NO_2^-, H_2PO_4^-, Br^-, NO_3^-, SO_4^<2->, and I^-) were separated on an anoin exchange column by using disodium phthalate solution as an eluent, and detected as troughs in the base line absorbance by a UV monitor. The optimum conditions for the determination of HCO_3^-, C1^-, H_2PO_4^-, Br^-, NO_3^-, and SO_4^<2-> were as follows : column, Zipax SAX (2.1 mm i.d. ×50cm) ; eluent, 5×10^<-4>M disodium phthalate ; flow rate, 1 ml/min ; column temperature, ambient ; detection wavelength, 240 nm. Under the conditions described above, detection limits of these anions were at levels as low as ppb. The calibration curves gave straight lines by either peak height or peak area method. Main inorganic anions contained in environmental samples could be simultaneously determined by the proposed method, and their analytical results were close to those obtained by other methods.
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| 5.
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Hayakawa, Kazuichi ; Miyazaki, Motoichi
概要:
A HPLC method with peroxyoxalate-chemiluminescence (CL) detection has been developed for the determination of dinitropyr
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enes (DNPs) and nitropyrene (NP). Both DNPs and NP, which are CL-insensitive, were initially reduced to the corresponding amino-derivatives with sodium hydrosulfide. They were separated on a reversed-phase column and chemilumigenically determined with detection limits in the subfmol range. Utilizing this method, DNPs and NP were determined in gasoline and diesel particulate samples. © 1991, The Japan Society for Analytical Chemistry. All rights reserved.
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Oe, Tomoyuki ; Mizuguchi, Tatsuhito ; Shimada, Kazutake
概要:
One of the Cookson-type reagents, 4-(1-anthryl)-1,2,4-triazoline-3,5-dione, has been applied to the determination of 7-d
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ehydrocholesterol in human skin surface. The extract from human skin surface was derivatized with the reagent and the obtained adduct was selectively detected using a UV detector. © 1991, The Japan Society for Analytical Chemistry. All rights reserved.
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| 7.
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村上, 新 ; 龍村, 俊樹 ; 清水, 岑雄 ; 森田, 直賢
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