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1.
三唑仑(Triazolam)为苯二氮卓类安定药,该药具有抗惊厥、抗癫痫、抗焦虑、镇静催眠作用。加大用量可导致昏迷,目前尚未见致死量的报道。人口服三唑仑后尿液含量的检验已有一些报道,但选择的服药量均在治疗量范围内(1—2片),药量偏低。本实验采用GC/ECD、GC/MS/NCI,GC/MS/EI法,分析口服0—4片三唑仑后72h内尿液中药物的排泄规律,以期为实际案件收集尿液检材提供参考依据。  相似文献   

2.
GC/MS是分析微量多组分有机毒物比较理想的工具,GC对微量有机混合物具有高度分离能力,MS鉴定有机物灵敏、准确。加上计算机监测和数据处理,使GC/MS可为法庭科学提供快速、灵敏、准确的鉴定结论。但在实际工作中发现,该法在吩噻嗪类和安定类混合药物的分析中仍有困难。由于吩噻嗪类和安定类药物结构相似,用轰击源(EI)方法有时个别药物分离不够理想,而用化学源(CI)方法可以获得药物各自的特征峰,混合药物中各组分达到完全分离。我们对国内常见的8种药物进行了分析条件的佳化选择和动物实验,取得了理想的效果。实验一、试…  相似文献   

3.
气-质联用法(EI.PCI.NCI)在系统毒物分析中的应用   总被引:1,自引:0,他引:1  
本文应用电子轰击质谱(EI),正、负化学电离质谱(PCI.NCI)技术,建立了315种常见毒,药物的气一质联用系统分析方法。并建立了 EIMS、PCIMS、NCIMS 质谱图谱库。司法鉴定实践表明使用气相保留指数,特征碎片和 EI、PCI、NCI 图谱库检索等多指标的系统分析方法,是未知物鉴定的强有力的工具。  相似文献   

4.
目的 建立X射线衍射法(XRD)检验有机炸药的方法.方法 使用X射线衍射仪对有机炸药苦味酸(PA),太安(PTEN),黑索金(RDX),梯恩梯(TNT)进行测试分析.结果 准确测定出有机炸药的物质组成及结构.结论 该方法能够直接给出有机炸药的分子式及结构组成,定性准确,操作简便,可用于有机炸药的定性检测.  相似文献   

5.
目的不同方法检测三唑仑及代谢物α-羟基三唑仑,为其及时、准确的检测提供科学证据和最优方法。方法用GC/NPD、GC/MS、MS/MS、GC/ECD对兔体内三唑仑及代谢物α-羟基三唑仑进行检测。结果GC/ECD法最易检测出三唑仑及其代谢物。结论兔胃及内容物、尿液中容易检测到三唑仑及其代谢物;运用酶水解后,检测率最高;GC/ECD检测三唑仑及其代谢物的灵敏度最高。  相似文献   

6.
刘颖  罗芳 《刑事技术》2005,(5):29-30
目的本文研究GC/MS测定氟草烟的检测方法。方法采用GC/EI/MS、GC/CI/MS结合分析,确定氟草烟的色谱峰,并得到氟草烟的质谱图。结果通过质谱解析确认氟草烟的质谱图。结论本方法结果准确可靠。  相似文献   

7.
本文采用质谱仪的正、负化学源及MS/MS方式检测炸药残留物,方法简单、快速、灵敏度高,样品用量少,而且可用于混和物的直接分析。  相似文献   

8.
LC/MS/MS法测定生物组织中百草枯   总被引:2,自引:1,他引:1  
目的建立LC/MS/MS检测生物体液中百草枯方法。方法弱阳离子交换固相萃取小柱提取剂,应用LC/MS/MS法对生物样品中百草枯进行定性定量分析。结果经该方法测得百草枯的最小检出限为10ng/ml血(S/N≥3),线性范围为0.02~20μg/ml。结论该方法快速、灵敏、准确,适用于生物检材中百草枯的分析。  相似文献   

9.
氟乙酸五氟苄基酯的气相色谱分析   总被引:2,自引:0,他引:2  
目的 对氟乙酸根阴离子的衍生物-氟乙酸五氟苄基酯(PFB-MFA)进行了气相色谱分析,以满足氟乙酰胺类鼠药化验工作的需要。方法 使用GC/ECD、GC/MS Scan、GC/MS SIM对该化合物的标准溶液进行了分析,得到了各种分析方法的校正曲线及检测限。结果 三种方法测定PFB-MFA的线性范围分别为GC/ECD 0.01~0.1ng/μl、GC/MS SCAN 1~100ng/μl、GC/MS SIM 5×10~(-3)~1ng/μl。三种方法对氟乙酸根阴离子的检测限分别为:GC/ECD1.31×10~(-4)ng/μl、GC/MS SCAN 0.13ng/μl、GC/MS SIM 1.76×10~(-4)ng/μl。结论 氟乙酸根阴离子的衍生物氟乙酸五氟苄基酯在GC/ECD及GC/MS上具有一定的线性范围,有非常高的灵敏度,可用于法庭科学的定性定量分析。  相似文献   

10.
本文建立了超高效液相色谱–四级杆串联飞行时间质谱测定涉爆案件中17种有机炸药(TNT、RDX、HMX、PETN、CE、2-Am-DNT、4-Am-DNT、PYX、2-HADNT、4-HADNT、1,2-DNG、1,3-DNG、3,5-DNA、R-SALT、4-NDPA、NTO、4,4’-DNDPA)的快速定性、定量方法。本研究将有机炸药爆炸残留物或原药经有机溶剂直接溶解,用PLD+净化柱或有机微孔过滤膜净化提取,提取液采用超高效液相色谱–四级杆串联飞行时间质谱进行定性、定量检测。分析采用Shim-pack Velox Biphenyl(2.1 mm×100 mm×2.7μm)色谱柱,质谱扫描方式为负离子的全扫描/数据依赖二级质谱扫描(Full MS/DDA-MS2)模式。结果表明17种有机炸药的检出限在0.1~10 ng/mL之间,所有目标物在其相应的浓度范围内线性关系良好,日内相对标准偏差(RSD)为1.6%~5.3%(n=6),日间相对标准偏差(RSD)为1.7%~8.5%(n=24)。应用本方法可同时准确、快速、高效地对涉爆案件中的17...  相似文献   

11.
Method detection limits are determined and compared for analysis of liquid injections of organic explosives and related compounds by gas chromatography-mass spectroscopy utilizing electron impact (EI), negative ion chemical ionization (NICI), and positive ion chemical ionization (PICI) detection methods. Detection limits were rigorously determined for a series of dinitrotoluenes, trinitrotoluene, two nitroester explosives, and one nitramine explosive. The detection limits are lower by NICI than by EI or PICI for all explosives examined, with the exception of RDX. The lowest detection limit for RDX was achieved in the PICI ionization mode. Judicious choice of the appropriate ionization mode can enhance selectivity and significantly lower detection limits. Major ions are reported for each analyte in EI, PICI, and NICI detection modes.  相似文献   

12.
In this study, a standard method by gas chromatography coupled with mass spectrometry (GC/MS) for the analysis of classical organic explosives was developed. This method was validated in the EI mode, based on the XPT 90-210 standard method. Detection limits (LOD) and quantitation limits (LOQ) were both determined using electronic impact (EI) and negative ion chemical ionization (NICI) modes. These were compared and results showed that in the NICI mode, detection limits were lower than in the EI mode, thus NICI mode appeared to be the best way to analyze nitrate esters. Results of ion trap MS detection were then compared with those obtained in a previous study with single quadrupolar technology. Major ions that were obtained using ion trap MS detection in these two modes were reported.  相似文献   

13.
In this paper, swabbings from various public areas in 28 different cities throughout the United States were collected. A wide variety of objects were tested, ranging from park benches and telephones to sign posts and mailboxes. Inorganic anions and cations common in low explosives were detected simultaneously using capillary zone electrophoresis. Organic high explosives including nitroaromatics, nitramines, and nitrate esters were detected using gas chromatography with a pulsed-discharge electron capture detector. Confirmation of selected results was performed by ion chromatography and negative ion chemical ionization GC/MS. In general the results provide two major conclusions: (i) with the exception of nitrate, most low explosive oxidizers are rare in the environment; (ii) no organic explosives or significant interferences to these explosives were detected.  相似文献   

14.
This paper describes a simple processing and analysis scheme for explosives trace swab samples which deals both with organic and inorganic materials. Swabs, wetted with ethanol or ethanol/water mixture, were extracted with ethanol/water mixture. The extract was passed directly through a simple column containing an acrylonitrile/styrene copolymer adsorbent. The adsorbent retained common organic explosives, which were recovered with an efficiency of 30-50% as a relatively clean ethyl acetate solution. The concentrated ethyl acetate eluate was analysed using gas chromatography with chemiluminescence or mass spectrometric detection. The unretained inorganic ions and sugars, which were recovered with generally high efficiency as an ethanol/water solution, could be directly analysed using ion chromatography and/or capillary electrophoresis. Minor difficulties encountered in the analysis of sugars, fluoride and phosphate were examined.  相似文献   

15.
本文考察了顶空固相微萃取在有机爆炸物现场非介入性检测中的适用性。由固相萃取(SPME)纤维头吸附的有机爆炸物用真空气相色谱一质谱联用仪进行检测。该方法所需的洗脱温度低,色谱分离时间短。SPME适用于提取蒸汽压不低于2.4,6-三硝基甲苯(TNT)的挥发性和半挥发性有机爆炸物,如较易挥发且不稳定的化合物三过氧化三丙酮(TATP)的非介入性检测就可以应用该方法。本研究使用静态顶空,尽可能地减少顶空体积,实现了较高的灵敏度。在现场,SPME方法的灵敏度受环境温度的影响较大:由于样品的蒸汽压未达到平衡,在固定顶空体积和萃取时间的条件下,SPME纤维头萃取的样品总量随温度的提高而增加。在有合适容器的情况下SPME纤维头上萃取的样品在取样3天后仍然能顺利检测。  相似文献   

16.
The effectiveness of a number of the explosives contamination prevention controls that are adopted within the Forensic Explosives Laboratory (FEL) principal trace laboratory has been scrutinised. Within the trace laboratory, rigorous procedures for processing forensic swab samples for traces of organic explosives are routinely adopted by forensic scientists. In order to demonstrate the effectiveness of these procedures, and the principle of separating the sample from the laboratory and the forensic scientist, explosives-free swab samples and appropriate controls have been processed, in accordance with trace laboratory procedures, in several explosives contaminated environments. In all cases, no explosives were detected in the post-processing samples, demonstrating that the contamination prevention procedures are effective, robust and fit-for-purpose.  相似文献   

17.
Solid-phase microextraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS) is a simple, reliable technique for the recovery and analysis of many organic explosives. However, this technique is impractical for the analysis of ammonium nitrate-type explosives due to the extreme polarity, low molecular weight, and high volatility of the amine moiety. This article describes an initial investigation of a derivatization process utilizing alkylchloroformates that converts ammonium nitrate and methylammonium nitrate into a form suitable for recovery by SPME and analysis by GC-MS.  相似文献   

18.
《Science & justice》2021,61(6):697-703
The identification and confirmation of trace explosive residues along with potential precursors and degradation products require a comprehensive laboratory analysis procedure. This study presents the determination of organic explosives consisting of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX), 2,4,6-trinitrotoluene (TNT), 2,4,6,N-tetranitro-N-methylaniline (Tetryl), 1,3,5-trinitrobenzene (1,3,5-TNB) and pentaerythritol tetranitrate (PETN) by a high-resolution liquid chromatography quadrupole time-of-flight mass spectrometry (LC−QTOF/MS). The qualitative information including retention time, collision energy, precursor ions, and characteristic fragmentation pattern of each explosive were collected using an atmospheric pressure chemical ionization (APCI) in negative ion mode. The separation efficiency among five compounds was greatly achieved in this study. Four real explosive samples consisting of TNT, RDX, PETN and Tetryl and 12 Ionscan® quality control swabs from the Royal Thai Army were also tested to validate and verify the viability of the GC–MS method used to validate results from an Ionscan® system. The results showed that LC−QTOF/MS is a powerful technique for the identification and confirmation of thermally unstable organic explosives on Ionscan® swabs compared to a conventional GC−MS technique.  相似文献   

19.
The goal of this paper is to describe applications of two recently developed HPLC methods for the analysis and confirmation of the presence of hydrogen peroxide residues in field studies. The procedure utilizes two different HPLC systems, one with post-column derivatization followed by fluorescence detection (HPLC/FD), and the other with electrochemical detection (HPLC/ED). The two systems were utilized to detect hydrogen peroxide in a variety of typical forensic samples including pre- and post-blast samples, as well as a series of environmental control samples. Peroxide-based organic explosives were also examined due to their propensity to produce peroxide residues following detonation. Because samples collected from post-blast scenes are frequently shipped or stored prior to analysis, the effects of storage time, temperature and type of substrate material on the recovery of hydrogen peroxide residues were also investigated. The combined results of the study demonstrate the capability of two HPLC approaches with selective detection in the analysis and investigation of suspected incidents involving peroxide based explosives.  相似文献   

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