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.

我们通过柱交换系统（使用热图液体色谱仪谱机和光电二极管阵列阵列检测器），通过柱交换系统为苯二氮卓类药物（溴化物，estazolam和Triaselam）展示了一种自动的在线提取 - 分析测定法。使用凝胶柱（Asahipak GS-310H C18,4.6mm ID*250mm L）和流动阶段1（40％CH_3CN（含0.1 N NACIO_4）以0.1 N NACIO_4的流量为单位，将血清中的苯二氮卓类药物与血清含量分离为血清含量（Asahipak GS-310H C18,4.6mm ID*250mm L），以0.5ml/min的流速为0.5ml/min），然后将其置于Capell PakCl pak c18 mmm c18。在使用流动阶段2进行柱上进行柱进行洗涤（以1.5ml/min的蒸馏水为5分钟），使用第三列（STR ODS-2,4.6mm ID*250mm L）和3阶段3（50％CH__ <3cn>含有50 mm CH_3CoonH_4和0.05％CH_3COOH，在1.0ml/min）确定每种药物。检测到苯二氮卓类药物的热刺质谱仪QP1000EX和光电二极管阵列SPD-M10AVP。分别将蒸发器，块和尖端加热器的温度设置为144,305和315 c。溴化物，Estazolam和三唑仑的峰值分别为4.8,6.3和7.1分钟。水溶液中药物的回收率分别为90.9,97.2和90.9％。药物可重复性方差的系数分别为1.25,0.33和0.54％。当使用热喷雾电离时，分别获得了M/z 316,295和343的MH^+离子作为溴化物，Estazolam和Triasholam的基础峰。

项目成果

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。”

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)。

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）。

M.Yoshida: "Automatic extraction analysis for benzodiazepines in biological materials by column switching HPLC." Advances in Legal Medicine. 3. 532-534 (1997)

M.Yoshida：“通过柱切换 HPLC 自动萃取分析生物材料中的苯二氮卓类药物。”

Manabu Yoshida, Atsushi Akane, Sumitaka Yoshimura, Yutaka Okii, Takuma Tokiyasu and Toshimitsu Watabiki: "Determination of benzodiazepines, triazolam, nimetazepam, lormetazepam and flurazepam by thermospray liquid chromatography-mass spectrometry." Res.Pr

Manabu Yoshida、Atsushi Akane、Sumitaka Yoshimura、Yutaka Okii、Takuma Tokiyasu 和 Toshimitsu Watabiki：“通过热喷雾液相色谱-质谱法测定苯二氮卓类药物、三唑仑、尼美西泮、氯甲西泮和氟西泮。”