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

因意外或故意过量服用安眠药或镇静剂而导致的急性药物中毒增加已成为一个社会问题。因此，需要建立快速、简单的分析方法来诊断中毒。本文研究了流动注射-热喷雾-质谱法快速测定药物，在热喷雾电离模式和灯丝开启电离模式下，大多数标准药物的MH~++离子被检测为基峰。采用Sep-Pak tCl8色谱柱和由个人计算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，有望成为最适合分析的标本。作为前处理，在样品中加入等量的蒸馏水、乙醇或乙腈，然后以3000转/分的速度离心10分钟。毒品被排除在…之外更多的是用上清液中的乙酸乙酯。不含药物的胃内容物未经预检时，有不同程度的杂质离子检出。用乙醇或乙腈进行前处理会增强离子的强度，干扰分析。当检测含有1mug/ml苯二氮卓类和双氢可待因的胃内容物时，未经前处理的样品不能很好地检出药物，而经蒸馏水处理的样品则不能很好地检出这些药物。由于这些药物可能被检测为相同分子量的离子，流动注射方法在某些情况下很难将每种药物从其混合物中分离出来。为了改进它，在分析系统之前结合了一个简单的分离柱(1/16英寸*1.0 mm*20厘米不锈钢管，填充有Sep-Pak C18)。流动相为含0.1M醋酸铵的乙腈-水(40：60，v/v)。通过这种改进，代表药物的峰在保留时间为0.4-1.2min的范围内分离，即使从含有药物的未处理的胃内容物中也能检测到每种药物。流动注射技术与Triage、Visualine等药物筛选检测设备相结合，是实现药物快速鉴定的有力手段。较少

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。”