Rapid analysis of drugs by direct injection into thermospray mass spectrometer.

通过直接注入热喷雾质谱仪快速分析药物。

• 批准号: 07670509
• 负责人: YOSHIDA Manabu
• 金额: $ 1.09万
• 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 (C)
• 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-07670509/
• 关键词: Thermospray mass spectrometry; Flow injection method; Drug analysis

Increase of acute drug toxicosis caused by accidental or deliberate overdosage of sleeping drugs or tranquilizers has become a social problem. Establishment of quick and simple analysis for diagnosis of the toxicosis is thus required. In this research, rapid determination of the drugs by flow injection-thermospray mass spectrometry was investigated.Under the thermospray ionization mode and the filament-on ionization mode, MH^+ ions of most of the standard drugs were detected as base peaks. A semi-automatic drug extraction system was also applied, which consisted of Sep-Pak tCl8 column and a peristaltic pump controlled by personal computer, resulting in high reproduction rates.Gastric contents, which may contain large amounts of administered drugs, were expected to be the most suitable specimens for analysis. As the pretreatment, an equal volume of distillled water, ethanol or acetonitrile was added into the specimens, followed by centrifugation at 3,000rpm for 10 min. Drugs were extrac … More ted with ethyl acetate from the supernatants. When gastric contents containing no drugs were not pretealed, impurity ions were detected to some extent. Pretreatment with ethanol or acetonitrile enhanced intensities of the ions, interfering with the analysis. When gastric contents containing 1mug/ml benzodiazepines and dihydrocodeine were assayd, the drugs could not be detected well from non-pretreated samples but from samples treated with distillled water. Therefore, pretreatment with distillled water was most suitable for the determination.Since such drugs might be detected as ions of the same molecular weight, identification of each drug from their mixture by flow injection method would be difficult in some cases. To improve it, a simple separation column (a 1/16 inch * 1.0mm * 20 cm stainless-steel tube packed with Sep-Pak C18) was combined prior to the analysis system. The mobile phase used was acetonitrile-water (40 : 60, v/v) containing 0.1M ammonium acetate. By this modification, peaks representing the drugs were separated at retention time ranged 0.4-1.2 min, and each drug could be detected even from non-pretreated gastric contents containing the drugs. In combination with drug screening test devices such as Triage and Visualine, the flow injection method is a powerful measure for the rapid drug identification. Less

由于意外或故意过量的睡眠药物或镇静剂而导致的急性药物毒性增加已成为一个社会问题。因此，需要建立快速，简单的分析以诊断毒理症。在这项研究中，研究了通过流量注射 - 透明质量光谱法对药物进行快速测定。在热喷涂的电离模式和丝状电离模式下，大多数标准药物的MH^+离子被检测到基本峰。还采用了半自动药物提取系统，该系统由SEP-PAK TCL8色谱柱和由个人计算机控制的蠕动泵组成，导致较高的繁殖速率。胃含量可能包含大量的管理药物，预计将是最合适的标本。当预处理时，将等体积的蒸馏水，乙醇或乙腈添加到样品中，然后在3,000rpm下离心10分钟。药物是超级中清液中乙酸乙酯的外推。当未偶然发生含有不含药物的胃含量时，在一定程度上检测到杂质离子。对乙醇或乙腈的预处理增强了离子的强度，会干扰分析。当分析含有1mug/ml苯二氮卓类药物和二氢可爱苷的胃含量时，无法从未经培养的样品中很好地检测到这些药物，而是从用蒸馏水处理的样品中检测到的。因此，用蒸馏水进行预处理最适合确定。由于可以检测到这些药物为相同分子量的离子，因此在某些情况下很难通过流量注入方法从其混合物中鉴定每种药物。为了改善它，在分析系统之前将简单的分离柱（1/16英寸 * 1.0mm * 20 cm不锈钢管堆满了SEP-PAK C18）。所使用的流动相是含有0.1m乙酸铵的乙腈 - 水（40：60，V/V）。通过这种修饰，在保留时间分离代表药物的峰范围为0.4-1.2分钟，即使从含有该药物的非预测的胃含量中也可以检测到每种药物。结合药物筛查测试设备，例如分类和可视化，流动注射方法是快速药物鉴定的有力衡量标准。较少的

项目成果

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)。

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。”

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 Cl8 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 Cl8 柱开发半自动药物提取系统。”

Manabu Yoshida, Atsushi Akane, Yutaka Okii, Sumitaka Yoshimura, Takuma Tokiyasu and Toshimitsu Watabiki: "Automatic extraction-analysis system for benzodiazepines in biological materials by column-switching HPLC." Proceedings of The Third International Sy

Manabu Yoshida、Atsushi Akane、Yutaka Okii、Sumitaka Yoshimura、Takuma Tokiyasu 和 Toshimitsu Watabiki：“通过柱切换 HPLC 自动提取分析生物材料中苯二氮卓类药物的系统。”

Manabu Yoshida, Atsushi Akane, Eiichi Otsuki, Sumitaka Yoshimura, Yutaka Okii, Takuma Tokiyasu and Toshimitsu Watabiki: "Direct analysis of diazepam in biological materials by column-switching technique" Res.Pract.Forens.Med. 39. 101-106 (1995)

Manabu Yoshida、Atsushi Akane、Eiichi Otsuki、Sumitaka Yoshimura、Yutaka Okii、Takuma Tokiyasu 和 Toshimitsu Watabiki：“通过柱切换技术直接分析生物材料中的地西泮” Res.Pract.Forens.Med。