Development of automatic extraction-analysis system for thermospray mass spectrometer.

热喷雾质谱仪自动萃取分析系统的研制。

• 批准号: 07557042
• 负责人: YOSHIDA Manabu
• 金额: $ 4.1万
• 依托单位: Kansai Medical University
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (B)
• 财政年份: 1995
• 资助国家: 日本
• 起止时间: 1995 至 1996
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-07557042/
• 关键词: Thermospray mass spectrometry; Column-Switching; Drug analysis; sample pretreatment; benzodiazepine; Alkyldipyridylium herbicide; カラムスイッチング法

We demonstrate an automatic, on-line extraction-analysis assay for benzodiazepines (bromazepam, estazolam and triazolam) by the column-switching system for three columns using thermospray liquid chromatograph-mass spectrometer and photodiode array detector. The benzodiazepines in serum were separated from the serum contents using a gel column (ASAHIPAK GS-310H C18,4.6mm ID*250mm L) and the mobile phase 1 (40% CH_3CN containing 0.1 N NaCIO_4 at a flow rate of 0.5ml/min), and then trapped to the second column (CAPCELL PAK C18,4.6mm ID*35mm L). Following the column-wash with the mobile phase 2 (distillled water at 1.5ml/min, for 5min), each drug was identified using the third column (STR ODS-2,4.6mm ID*250mm L) and the mobile phase 3 (50% CH_<3CN> containing 50 mM CH_3COONH_4 and 0.05% CH_3COOH,at 1.0ml/min). The benzodiazepines were detected thermospray mass spectrometer QP1000EX and photodiode array detector SPD-M10AVP.The temperature of the vaporizer, block and tip heater of the ion source block were set at 144,305 and 315 ﾟC,respectively. Peaks of bromazepam, estazolam and triazolam were represented 4.8,6.3 and 7.1 min, respectively. The recovery rates of the drugs in aqueous solution were 90.9,97.2 and 90.9%, respectively. The coefficients of variance for reproducibility of the drugs were 1.25,0.33 and 0.54%, respectively. When thermospray ionization was used, MH^+ ions of m/z 316,295 and 343 were obtained as base peak for bromazepam, estazolam and triazolam, respectively.

采用三柱切换系统，采用热喷雾液质联用仪和光电二极管阵列检测器，建立了苯二氮类药物(溴氮卓、艾司唑仑和三唑仑)的自动在线萃取分析方法。采用凝胶色谱柱(ASAHIPAK GS-310H C18，4.6 mM ID*250 mM L)和流动相1(40%CH3CN含0.1N NaClO_4，流速0.5ml/min)从血清中分离苯二氮卓类药物，然后固定到第二柱(CAPCELL PAK C18，4.6 mM ID*35 mm L)。用流动相2(蒸馏水1.5ml/min，5min)洗脱后，使用第三柱(STR ods-2，4.6 mM ID*250 mM L)和流动相3(50%CH_3COONH_4和0.05%CH_3COOH，1.0ml/min)进行鉴别。采用热喷雾质谱仪QP1000EX和光电二极管阵列检测器SPD-M10VP检测苯二氮类药物，离子源块的气化器、块和尖端加热器的温度分别设置为144、305和315ﾟC。溴西潘、艾司唑仑和三唑仑的峰时间分别为4.8min、6.3 min和7.1min。水溶液中药物的回收率分别为90.9%、97.2%和90.9%。重现性变异系数分别为1.25、0.33和0.54%。当采用热喷雾电离时，分别获得了m/z为316、295和343的MH~+离子作为溴西潘、艾司唑仑和三唑仑的基峰。

项目成果

吉田 学: "Sep-Pak tC18カラムを用いた半自動薬物抽出装置の開発" 法医学の実際と研究. 38. 121-128 (1995)

Manabu Yoshida：“使用 Sep-Pak tC18 柱开发半自动药物提取装置”法医学实践与研究 38. 121-128 (1995)。

M.Yoshida: "Automatic extraction-analysis system for benzodiazepines in biological materials by column-switching HPLC." Proceedings of The Third International Symposium ADVANCES IN LEGAL MEDICINE.1996.(IN PRESS).

M.Yoshida：“通过柱切换 HPLC 自动提取生物材料中苯二氮卓类药物的分析系统。”

吉田 学: "カラムスイッチング法を用いたHPLCによるベンゾジアゼピン系薬物の直接分析" 第80次日本医学会総会講演要旨(日本法医学雑誌). 50(補冊号). (1996)

Manabu Yoshida：“使用柱切换法通过 HPLC 直接分析苯二氮卓类药物”日本医学会第 80 届大会摘要（日本法医学杂志）50（增刊）。

吉田 学: "カラムスイッチング法による生体試料中のジアゼパムの直接分析." 法医学の実際と研究. 39. 101-106 (1996)

Manabu Yoshida：“使用柱切换法直接分析生物样品中的地西泮。”法医实践与研究 39. 101-106 (1996)。

Manabu Yoshida, Atsushi Akane, Toshimitsu Watabiki, Sumitaka Yoshimura, Yutaka Okii, Takuma Tokiyasu and Eiichi Otsuki: "Development of semi-automatic drug extraction system using a Sep-Pak C18 column." Res.Pract.Forens.Med.38. 121-128 (1995)

Manabu Yoshida、Atsushi Akane、Toshimitsu Watabiki、Sumitaka Yoshimura、Yutaka Okii、Takuma Tokiyasu 和 Eiichi Otsuki：“使用 Sep-Pak C18 色谱柱开发半自动药物提取系统。”