{"title":"结合乙酸盐的多种分析物加合物形成在液相色谱-串联质谱法法医毒理学信号分离定量中的应用。基于水杨酸作为模型药物应用的讨论","authors":"Marek Dziadosz","doi":"10.1016/j.forsciint.2019.02.025","DOIUrl":null,"url":null,"abstract":"<div><p>In this work the examination of analyte adduct formation by the application of both sodium acetate and lithium acetate was performed with salicylic acid used as a model drug. Additionally, on the basis of combined acetate salt based multiple analyte adduct ions it was aimed to investigate the generation of different analyte precursor ions and their application in signal separated quantification with liquid chromatography–tandem mass spectrometry. Adduct identification experiments were performed by infusion experiments and resulted in an optimised detection of analyte adduct ions with lithium acetate, sodium acetate and combined lithium acetate/sodium acetate. Sample preparation based on a fast protein precipitation with a methanol solution containing lithium acetate and sodium acetate. A Luna 5 μm C18 (2) 100 A, 150 mm × 2 mm analytical column and a mobile phase composed of an H<sub>2</sub>O/methanol = 3%/97% (v/v) solution with 10 mmol l<sup>-1</sup> ammonium acetate and 0.1% acetic acid were used for chromatographic purposes. The linearity was investigated in the range of 5–500 μg/ml. The limit of detection (LOD of 1.2 μg/ml) and quantification (LOQ 4.0 μg/ml) together with other results of validation experiments revealed that this strategy can be applied for salicylic acid quantification.</p></div>","PeriodicalId":12341,"journal":{"name":"Forensic science international","volume":"297 ","pages":"Pages 249-253"},"PeriodicalIF":2.5000,"publicationDate":"2019-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.forsciint.2019.02.025","citationCount":"0","resultStr":"{\"title\":\"Application of combined acetate salt based multiple analyte adduct formation in signal separated quantification performed for the purposes of forensic toxicology with liquid chromatography–tandem mass spectrometry — Discussion on the basis of salicylic acid applied as a model drug\",\"authors\":\"Marek Dziadosz\",\"doi\":\"10.1016/j.forsciint.2019.02.025\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>In this work the examination of analyte adduct formation by the application of both sodium acetate and lithium acetate was performed with salicylic acid used as a model drug. Additionally, on the basis of combined acetate salt based multiple analyte adduct ions it was aimed to investigate the generation of different analyte precursor ions and their application in signal separated quantification with liquid chromatography–tandem mass spectrometry. Adduct identification experiments were performed by infusion experiments and resulted in an optimised detection of analyte adduct ions with lithium acetate, sodium acetate and combined lithium acetate/sodium acetate. Sample preparation based on a fast protein precipitation with a methanol solution containing lithium acetate and sodium acetate. A Luna 5 μm C18 (2) 100 A, 150 mm × 2 mm analytical column and a mobile phase composed of an H<sub>2</sub>O/methanol = 3%/97% (v/v) solution with 10 mmol l<sup>-1</sup> ammonium acetate and 0.1% acetic acid were used for chromatographic purposes. The linearity was investigated in the range of 5–500 μg/ml. The limit of detection (LOD of 1.2 μg/ml) and quantification (LOQ 4.0 μg/ml) together with other results of validation experiments revealed that this strategy can be applied for salicylic acid quantification.</p></div>\",\"PeriodicalId\":12341,\"journal\":{\"name\":\"Forensic science international\",\"volume\":\"297 \",\"pages\":\"Pages 249-253\"},\"PeriodicalIF\":2.5000,\"publicationDate\":\"2019-04-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://sci-hub-pdf.com/10.1016/j.forsciint.2019.02.025\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Forensic science international\",\"FirstCategoryId\":\"3\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S037907381830937X\",\"RegionNum\":3,\"RegionCategory\":\"医学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"2019/2/22 0:00:00\",\"PubModel\":\"Epub\",\"JCR\":\"Q1\",\"JCRName\":\"MEDICINE, LEGAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Forensic science international","FirstCategoryId":"3","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S037907381830937X","RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"2019/2/22 0:00:00","PubModel":"Epub","JCR":"Q1","JCRName":"MEDICINE, LEGAL","Score":null,"Total":0}
引用次数: 0
摘要
在这项工作中,以水杨酸为模型药物,研究了醋酸钠和醋酸锂的应用对分析物加合物形成的影响。此外,以复合乙酸盐为基础,研究了不同分析物前体离子的生成及其在液相色谱-串联质谱信号分离定量中的应用。加合物鉴定实验采用输注实验,优化了醋酸锂、醋酸钠和醋酸锂/醋酸钠复合对分析物加合物离子的检测。用含有醋酸锂和醋酸钠的甲醇溶液快速蛋白沉淀制备样品。色谱柱为Luna 5 μm C18 (2) 100 A, 150 mm × 2mm,流动相为H2O/甲醇= 3%/97% (v/v)溶液,10 mmol l-1醋酸铵和0.1%醋酸。在5 ~ 500 μg/ml范围内考察其线性关系。检出限(LOD为1.2 μg/ml)和定量限(LOQ为4.0 μg/ml)以及其他验证实验结果表明,该策略可用于水杨酸的定量分析。
Application of combined acetate salt based multiple analyte adduct formation in signal separated quantification performed for the purposes of forensic toxicology with liquid chromatography–tandem mass spectrometry — Discussion on the basis of salicylic acid applied as a model drug
In this work the examination of analyte adduct formation by the application of both sodium acetate and lithium acetate was performed with salicylic acid used as a model drug. Additionally, on the basis of combined acetate salt based multiple analyte adduct ions it was aimed to investigate the generation of different analyte precursor ions and their application in signal separated quantification with liquid chromatography–tandem mass spectrometry. Adduct identification experiments were performed by infusion experiments and resulted in an optimised detection of analyte adduct ions with lithium acetate, sodium acetate and combined lithium acetate/sodium acetate. Sample preparation based on a fast protein precipitation with a methanol solution containing lithium acetate and sodium acetate. A Luna 5 μm C18 (2) 100 A, 150 mm × 2 mm analytical column and a mobile phase composed of an H2O/methanol = 3%/97% (v/v) solution with 10 mmol l-1 ammonium acetate and 0.1% acetic acid were used for chromatographic purposes. The linearity was investigated in the range of 5–500 μg/ml. The limit of detection (LOD of 1.2 μg/ml) and quantification (LOQ 4.0 μg/ml) together with other results of validation experiments revealed that this strategy can be applied for salicylic acid quantification.
期刊介绍:
Forensic Science International is the flagship journal in the prestigious Forensic Science International family, publishing the most innovative, cutting-edge, and influential contributions across the forensic sciences. Fields include: forensic pathology and histochemistry, chemistry, biochemistry and toxicology, biology, serology, odontology, psychiatry, anthropology, digital forensics, the physical sciences, firearms, and document examination, as well as investigations of value to public health in its broadest sense, and the important marginal area where science and medicine interact with the law.
The journal publishes:
Case Reports
Commentaries
Letters to the Editor
Original Research Papers (Regular Papers)
Rapid Communications
Review Articles
Technical Notes.