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論文

論文
木津, 良一 ; 東, 信一 ; 早川, 和一 ; 宮崎, 元一
出版情報: 分析化学 = Japan analyst.  35  pp.250-255,  1986-03-05.  The Japan Society for Analytical Chemistry = 日本分析化学会
URL: http://hdl.handle.net/2297/25011
概要: 金沢大学医薬保健研究域薬学系<br />血しょう及び尿中の制がん性白金錯体オキザラート(トランス-l-1,2-ジアミノシクロヘキサン)プラチニウム(II)(l-OHP)の分析法を研究した.種々検討した結果,分析条件は以下のように定めた.前処 理;Dowex 1-X8,Dowex 50 W-X4及びSep-Pak C_<18>カートリッジを一連のカラムとして構成する.この前処理カラムに血しょう及び尿の1mlと引き続き水を流す.前処理カラム溶出液の最初の6ml部分は捨て,次の10ml部分を分取し,高速液体クロマトグラフィー(HPLC)の試料とした.HPLC条件;カラム:Finepak SIL C_<18>(4.6mm i.d.×25cm),カラム温度:50℃,溶離液:水-メタノール(95:5),流速:1ml/min,検出波長:210nm,試料注入量:100μlピーク高さによる検量線は,原点を通る良い直線性を示した.定量下限は,血しょう及び尿中l-OHP濃度0.5μM,再現性はR.S.D.3%程度であった.血しょう及び尿中のl-OHPを高感度で精度良く定量することができた. A method for determination of (trans-l-1, 2-diaminocyclohexane) oxalatoplatinum (II) (l-OHP), introduced by Kidani et al. as one of the promising antineoplastic platinum complexes, in plasma and urine by high performance liquid chromatography (HPLC) was investigated in order to contribute for metabolic study of l-OHP. The recommended pretreatment procedures and HPLC conditions are as follows. Pretreatment of plasma and urine ; pretreatment column is composed of Dowex 1-X8 (5mm i. d.×6cm), Dowex 50W-X4 (5 mm i. d.×3 cm) and Sep-Pak C_<18> cartridge. Blood samples are centrifuged at 1000 g for 3 min to obtain plasma. One ml of plasma or urine is immediately placed on the pretreatment column and is eluted with water at the flow rate of 1.2 ml/min. The initial 6 ml portion of effluent is discarded and subsequent 10 ml portion is collected. An aliquot (100 μl) of the effluent collected is subjected to HPLC. All of these pretreatment procedures are carried out at 5±2℃. HPLC conditions ; column : Finepak SIL C_<18> (4.6 mm i. d.×25cm), eluent : H_2O-MeOH (95 : 5), column temperature : 40℃, flow rate : 1 ml/min, detection wavelength : 210 nm, injection volume : 100 μl. Under the conditions described above, a linear relationship was obtained between peak height and l-OHP concentration in plasma and urine. Determination limit was 0.5 μM l-OHP in sample solutions. Recovery of l-OHP in pretreatment was 86±3% in plasma and 83±2% in urine. A sensitive and precise determination of l-OHP in plasma and urine will be possible by this method. 続きを見る
2.

論文

論文
早川, 和一 ; 蛯名, 令子 ; 松本, 美枝子 ; 宮崎, 元一
出版情報: 分析化学 = Japan analyst.  33  pp.390-392,  1984-07-05.  The Japan Society for Analytical Chemistry = 日本分析化学会
URL: http://hdl.handle.net/2297/24891
概要: 金沢大学医薬保健研究域薬学系<br />Determination of inorganic anions and cations in some vegetable juices was examined by ultraviolet p hotometric ion chromatography with a conventional HPLC system equipped with a UV monitor and a separating column packed with popular ion exchangers. Inorganic anions such as Cl^-, NO_3^-, and SO_4^<2-> in sample solution were completely separated on a Zipax SAX packed column (50 cm × 2.1 mm I. D.) with 5 × 10^<-3> M disodium phthalate as an eluent and detected at 240 nm. Inorganic cations such as Na^+, NH_4^+, K^+, Mg^<2+>, and Ca^<3+> in sample solution were completely separated on a Zipax SCX packed column (25 cm × 4.6 mm I. D.) with 2.5 × 10^<-3> M copper sulfate as an eluent and detected at 220 nm. Under the conditions described above, the three anions in juices of Chinese cabbage, tomato, and radish, and the five cations in Sep-pak C_<18> treated juice of Chinese cabbage were determined. 続きを見る
3.

論文

論文
早川, 和一 ; 西島, 美知子 ; 宮崎, 元一
出版情報: 分析化学 = Japan analyst.  31  pp.160-161,  1982-03-05.  The Japan Society for Analytical Chemistry = 日本分析化学会
URL: http://hdl.handle.net/2297/24888
概要: 金沢大学医薬保健研究域薬学系<br />A novel method for the separation of halogenated anion complexes of platinum metals by reversed-phas e ion-pair partition chromatography has been developed. The separation of RhBr_5^<2->, PdBr_4^<2->,and PtBr_6^<2-> was accomplished on a Hitachi #3050 packed column (3mm×30cm), where 30 % (v/v) acetonitrile-0.02 M phosphate buffer (pH 7) mixture containing 0.1 M tetrabutylammonium bromide and 0.025 M sodium bromide was used as a mobile phase. These anion complexes can be determined at 310nm, and as low as 5×10^<-11> mol of PtBr_6^<-2> can be determined with the peak height method which gave a straight calibration curve. Detecting wavelengths and retention times of the complexes can be altered if the complexes are formed with other halogen ions. This analytical method for micro amounts of platinum metals can remove the mutual metal interferences. 続きを見る