氯氮平的GC／MS／MS检验

目的建立苯二氮卓类药物氯氮平的串联质谱检验方法,以排除干扰物质,提高灵敏度。方法用串联质谱方法分析。结果以基峰m/z243为母离子,碰撞诱导电压(CID)为0.8v,进行MS/MS分析。结论与GC/MS相比,GC/MS/MS方法选择性好、灵敏度最高,排除干扰性能强。     

MALDI-TOF-IMS在蛋白质组学研究中的新进展

基质辅助激光解吸/电离-飞行时间质谱成像(matrix-assisted laser desorption/ionization time-of-flight imaging mass spectrometry,MALDI-TOF-IMS)技术已成为目前蛋白质组学研究中的经典技术,是一种研究生物组织切片中蛋白质和小分子物质分布的工具。MALDI-TOF-IMS通过单次扫描就能够同时分析生物组织切片中的各种未知组分,在保持组织中细胞和分子完整性的同时获取组织的分子成像图。近年来,质谱成像技术在生物医学各领域中有了较快发展,本文综合文献资料对MALDI-TOF-IMS技术目前的发展水平、质谱成像原理、方法学以及在法医病理学中的应用前景进行了综述。     

利用GC—CI—MS／MS时间编程技术分析混合农药

目的研究生物组织中两种混合农药(敌敌畏、克百威)的痕量确认方法;方法采用时间编程方法和GC-CI-MS/MS技术,选择在共振方式下,用CI化学源在4min~6.5min以敌敌畏的分子离子(M 1)221为母离子进行MS/MS分析;结果其碰撞诱导电压为0.5v,产生的二级质谱子离子为141,145;在6.5min~13min以克百威的分子离子(M 1)222为母离子进行MS/MS分析,其碰撞诱导电压为0.4v,产生的二级质谱子离子为165,123;结论排除背景干扰、定性快而准确。     

GC/MS/AMDIS在法医毒物分析中的应用

目的探索自动质谱去卷积定性系统(AMDIS)在法医毒物分析中的应用。方法利用自动质谱去卷积定性系统(AMDIS)、全扫描离子模式(FIM)和选择离子监测技术(SIM)对农药、毒品、安眠镇静类药等常见毒物进行检索分析,比较三种检索方式对不同质量浓度(40.0、4.0、0.4mg/L)毒物的检验结果。结果AMDIS与SIM具有相近的灵敏度,可以将GC/MS全扫描文件去卷积处理,解决杂质干扰问题,准确对目标化合物进行定性;AMDIS可以自动识别重叠的色谱峰并将其与目标谱库进行匹配,为重叠峰的定性提供了直观的鉴别依据。结论AMDIS检索自动快速,适用于GC/MS法快速鉴定毒物。     

应用SPE－GC／MS法检测艾司唑仑

采用固相萃取(SPE)分离富集水溶液中的安眠药,在气相色谱/质谱(GC/MS)联用仪上进行分析,从一起麻抢案的饮料中检出艾司唑仑,方法简单,结果可靠.     

苯二氮卓类新精神活性物质去氯依替唑仑的定性检验方法研究

目的建立苯二氮卓类新精神活性物质去氯依替唑仑的气相色谱-质谱(GC-MS)和超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF MS)定性检验方法。方法未知样品用甲醇和水提取,取上清液,采用GC-MS和UPLC-Q-TOF MS进行分析。结果经GC-MS检测,保留时间为17.73 min的未知组分的质谱碎片主要特征离子峰有m/z 279,308,239,252,225,77,126。经UPLC-Q-TOF MS检测,保留时间为4.781 min的未知组分的准分子离子峰为309.1173,碰撞诱导解离(CID)模式下二级质谱主要离子有m/z 280.0776,255.0952,240.0719,225.0604,206.0748。经缴获毒品分析科学工作组(Scientific Working Group for the Analysis of Seized Drugs,SWGDRUG)分析谱库检索和文献查询获得的信息资料进行比对,鉴定为去氯依替唑仑。结论该方法具有分析简便、快速的特点,可以用于实际案件的检测。     

LC-HRMS非靶标筛查8个地表水样品中有机污染物

目的 基于超高效液相色谱-四极杆-飞行时间串联质谱技术(UPLC-QTOF MS/MS),建立高分辨质谱(LC-HRMS)非靶标策略筛查地表水中潜在有机污染物的方法并应用于环境水样品中有机污染物识别.方法 地表水样品经固相萃取提取后,采用0.1％甲酸溶液和甲酸甲醇溶液作为流动相在C18色谱柱上进行洗脱.分别采用全扫描模...     

GC法和GC/MS法在地区毒品情报分析中的应用

目的探讨气相色谱法(GC)和气相色谱/质谱联用法(GC/MS)在地区毒品情报分析中的应用,并用于实际样品分析。方法采用GC/MS法定性分析毒品样品中的主成分、痕量杂质、掺假剂和稀释剂,并选择GC/FID法和内标标准曲线法定量分析上述各组分,通过定性和定量数据的统计和分析,推断该地区的毒品状况。结果用GC/MS定性分析、GC/FID定量分析,和数据的统计比对,获得了某省某年27起海洛因毒品大案样品主成分、痕量杂质、掺假剂和稀释剂组成及含量的特征,发现该省缴获的大宗海洛因毒品主要以掺假和稀释后的产品出现,且咖啡因和扑热息痛为两种主要的掺假剂和稀释剂。结论GC/MS和GC/FID法在地区毒品情报分析和打击毒品犯罪中可以发挥重要作用。     

利用GC-CI-MS／MS检验安定

目的研究生物组织中痕量安定的定性分析方法;方法采用CI化学源和串联质谱法分析;结果选择安定的分子离子(M 1)m/e285为母离子,CID电压为0.8v进行MS/MS分析;结论此检验方法能有效的排除干扰物质,定性快速、灵敏、准确。     

液相电喷雾离子质谱技术在法医DNA中的应用

生物质谱技术是近年来发展较为迅速的生物分析技术之一,在对大分子生物质量测定中,其以快速、准确、灵敏等优点受到研究者的青睐。其中,液相电喷雾离子电离质谱(LC-ESI-MS)在法医DNA分析中对STR以及SNP遗传标记的检测具有独特的应用价值和广阔的应用前景。本文对ESI-MS的现状和在法医DNA分析中的应用等方面进行了综述,分析了LC-ESI-MS技术在法医学DNA分析中的优缺点,以促进其在国内法医DNA分析中的应用与发展。     

Review of analytical methods for screening and quantification of fentanyl analogs and novel synthetic opioids in biological specimens

Fentanyl, fentanyl analogs, and other novel synthetic opioids (NSO), including nitazene analogs, prevail in forensic toxicology casework. Analytical methods for identifying these drugs in biological specimens need to be robust, sensitive, and specific. Isomers, new analogs, and slight differences in structural modifications necessitate the use of high-resolution mass spectrometry (HRMS), especially as a non-targeted screening method designed to detect newly emerging drugs. Traditional forensic toxicology workflows, such as immunoassay and gas chromatography mass spectrometry (GC–MS), are generally not sensitive enough for detection of NSOs due to observed low (sub-μg/L) concentrations. For this review, the authors tabulated, reviewed, and summarized analytical methods from 2010–2022 for screening and quantification of fentanyl analogs and other NSOs in biological specimens using a variety of different instruments and sample preparation approaches. Limits of detection or quantification for 105 methods were included and compared to published standards and guidelines for suggested scope and sensitivity in forensic toxicology casework. Methods were summarized by instrument for screening and quantitative methods for fentanyl analogs and for nitazenes and other NSO. Toxicological testing for fentanyl analogs and NSOs is increasingly and most commonly being conducted using a variety of liquid chromatography mass spectrometry (LC–MS)-based techniques. Most of the recent analytical methods reviewed exhibited limits of detection well below 1 μg/L to detect low concentrations of increasingly potent drugs. In addition, it was observed that most newly developed methods are now using smaller sample volumes which is achievable due to the sensitivity increase gained by new technology and new instrumentation.     

On the use of IRMS in forensic science: proposals for a methodological approach

The flourishing number of publications on the use of isotope ratio mass spectrometry (IRMS) in forensic science denotes the enthusiasm and the attraction generated by this technology. IRMS has demonstrated its potential to distinguish chemically identical compounds coming from different sources. Despite the numerous applications of IRMS to a wide range of forensic materials, its implementation in a forensic framework is less straightforward than it appears. In addition, each laboratory has developed its own strategy of analysis on calibration, sequence design, standards utilisation and data treatment without a clear consensus. Through the experience acquired from research undertaken in different forensic fields, we propose a methodological framework of the whole process using IRMS methods. We emphasize the importance of considering isotopic results as part of a whole approach, when applying this technology to a particular forensic issue. The process is divided into six different steps, which should be considered for a thoughtful and relevant application. The dissection of this process into fundamental steps, further detailed, enables a better understanding of the essential, though not exhaustive, factors that have to be considered in order to obtain results of quality and sufficiently robust to proceed to retrospective analyses or interlaboratory comparisons.     

油性圆珠笔字迹书写时间鉴定的研究综述

本文追述了油性圆珠笔问世以来,字迹书写时间的检验发展过程;总结了静态法,如标准样品比对法和基准物标记法,动态法,如如溶剂萃取法、色谱法、质谱法和光谱法用于鉴定圆珠笔字迹书写时间的研究成果;展望了非破坏性方法在鉴定书写时间上的发展趋势。     

Cyanide quantification in post-mortem biological matrices by headspace GC-MS

Cyanide is a powerful chemical asphyxiant found in some forensic cases following voluntary (suicide) or involuntary ingestion (fire, accidental exposure). A quantification method for cyanide that is specifically suited to post-mortem forensic purposes was developed. Determination was performed by headspace gas chromatography coupled to mass spectrometry using a GS-GASPRO column on an HP-6890 gas chromatograph with an HP-5973N mass detector. The biological sample was treated with an internal standard, frozen, glacial acetic acid was added and the sample was then incubated at 60°C for 15min. The headspace was sampled with a disposable syringe, and analyzed to quantify hydrogen cyanide. Isotopically labeled cyanide ((13)C(15)N) was used as the internal standard to minimize matrix effect and sampling error. The method produced an extended linear dynamic range (0.07-50μg/mL), and a method detection limit of 0.02μg/mL. Identical calibration curves were obtained when blood, gastric contents and aqueous solutions were used as the calibration standard matrix. This method was also successful in quantitating cyanide in gastric contents, one of the most variable biological fluids. The method has been validated and is being used for current forensic cases such as fire victims and suicides.     

乌头急性中毒死亡者乌头生物碱的体内分布

目的研究乌头急性中毒死亡者体液和组织中乌头生物碱的分布．为乌头中毒案的法医学鉴定取材和结果评价提供参考。方法用液相色谱一串联质谱法测定中毒死亡者体液和组织中乌头生物碱的含量。结果乌头碱在死者体液和组织中的含量从大到小依次为尿液、胆汁、胃内容物、心血、胰、心、肠、肝、肾、胃、肺、胆囊、脾，脑中未检出。结论尿液、胆汁和血液是检测体内鸟头生物碱的较佳检材。     

An investigation into the spatial elemental distribution within a pane of glass by time of flight secondary ion mass spectrometry

Advances in the technology employed for the manufacture of glass have resulted in a final glass product with little variability in terms of its physical and optical properties. For example, the refractive index of Australian float glass tends to lie between 1.5189 and 1.5194. It has therefore become necessary to complement physical and optical methods for forensic glass comparison with instrumental elemental analyses. In a previous study, time-of-flight secondary ion mass spectrometry has been shown to offer potential for the analysis of glass particles as small as a few tens of microns across. In this study, the three-dimensional homogeneity of a sheet of float glass is described, and consequences for forensic elemental analysis of glass particles of such size are explored. Variation in Si, Ca, Mg, and Na levels immediately under the nonfloat surface was observed, with the variance accompanied by a decrease in refractive index.     

Sample Mining and Data Mining: Combined Real-Time and Retrospective Approaches for the Identification of Emerging Novel Psychoactive Substances

Novel psychoactive substances (NPS) are synthetic drugs that pose serious public health and safety concerns. A multitude of NPS have been identified in the United States, often implicated in forensic investigations. The most common and effective manner for identifying NPS is by use of mass spectrometry and the true utility lies within nontargeted acquisition techniques. During this study, a liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) assay was developed, validated, and implemented for forensic toxicology testing. A SCIEX TripleTOF™ 5600 + with SWATH^® acquisition was used. Resulting data were compared against an extensive library database containing more than 800 compounds. The LC-QTOF-MS assay was applied to the reanalysis of biological sample extracts to discover emergent NPS. More than 3,000 sample extracts were analyzed, and more than 20 emerging NPS were detected for the first time. Among these were isopropyl-U-47700, 3,4-methylenedioxy-U-47700, fluorofuranylfentanyl, N-methyl norfentanyl, 2F-deschloroketamine, 3,4-methylenedioxy-alpha-PHP, eutylone, and N-ethyl hexedrone.     

MALDI-TOF-MS成像技术及其在法医损伤标志物筛选中的应用

传统的免疫学和分子生物学技术在寻找损伤分子标志物方面存在成果孤立、效价模糊以及相互间作用机制不明等缺点.质谱成像技术集筛选、分析和图像化于一体,更适合基于形态学的损伤分子标志物研究.本文综述了基于基质辅助激光解吸/电离-飞行时间质谱（matrix-assisted laser desorption/ionizationtime-of flight mass spectrometry,MALDI-TOF-MS）成像技术筛选并识别特征性蛋白质的方法和最新进展,阐述了其在法医学损伤研究中的应用价值.     

Simultaneous determination of trace benzodiazepines from drinks by using direct electrospray probe/mass spectrometry (DEP/MS).

This study presents a novel means of rapidly determining benzodiazepines in various drinks. Electrospray mass spectrometry with a direct probe design is used as the analytical instrument. Samples are treated only by a simple liquid-liquid extraction prior to direct electrospray probe/mass spectrometry (DEP/MS) analysis. The proposed method provides a relatively easy and efficient means of identifying the drugs in a very short time interval. On average, sample analysis is completed in less than five minutes including sample pretreatment. It is especially useful in forensic science since the technology can provide a rapid identification for unknown samples. Thus, the method proposed herein is highly appropriate for rapidly screening a large number of samples.