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

因意外或故意过量使用安眠药物或镇定剂而引起的急性药物中毒日益增多，已成为一个社会问题。因此，需要建立快速和简单的分析来诊断中毒。本研究建立了流动注射-热喷雾质谱联用快速测定药物的方法。在热喷雾电离模式和离子束电离模式下，大多数标准药物的MH^+离子作为基峰被检测到。采用Sep-Pak tCl8色谱柱和微机控制的蠕动泵组成的半自动药物提取系统，重现率高。胃内容物可能含有大量给药药物，预计是最适合分析的标本。在样品中加入等体积的蒸馏水、乙醇或乙腈作为预处理，3000rpm离心10 min。用上清液中的乙酸乙酯提取药物未预处理不含药物的胃内容物时，可检出一定程度的杂质离子。乙醇或乙腈预处理可增强离子强度，干扰分析。当胃内容物中苯二氮卓类药物和二氢可待因含量为1杯/毫升时，未经预处理的样品不能很好地检测到药物，而蒸馏水处理的样品则不能很好地检测到药物。因此，蒸馏水预处理是最合适的测定方法。由于这些药物可能被检测为具有相同分子量的离子，因此在某些情况下，用流动注射方法从它们的混合物中识别每种药物是困难的。为了改进它，在分析系统之前，将一个简单的分离柱（1/16英寸* 1.0mm * 20 cm不锈钢管，填充Sep-Pak C18）组合在一起。流动相为含0.1M乙酸铵的乙腈-水（40∶60,v/v）。通过这种修饰，代表药物的峰在保留时间为0.4-1.2 min的范围内被分离出来，并且即使在含有药物的未预处理的胃内容物中也可以检测到每种药物。与Triage、Visualine等药物筛选试验装置相结合，流动注射法是快速鉴别药物的有力手段。少

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, 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。

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。”