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法庭毒物检验鉴定主要依据气相色谱仪和气-质联用仪,气相色谱仪对毒物定性是以药物的Rt值来判定,但由于GC法鉴别能力较差,许多药物之间Rt值相近,很难判别,为此我们利用VSOS将单柱单检测器改造成双毛细管柱双检测器定性分析。样品进样后经VSOS同时进入两根不同极性的毛细管柱,至两个不同的检测器,根据样品在不同极性色谱柱中的保留时间和不同检测器对同一毒物的选择性响应的差异,对毒物进行定性分析,该方法可使GC鉴别能力获得很大提高。1仪器与方法1.1仪器、试剂Varian3800气相色谱仪,配氢火焰离子检测器(FID)和氮磷检测器(TSD);DM… 相似文献
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GC/MS/AMDIS在法医毒物分析中的应用 总被引:1,自引:0,他引:1
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。 相似文献
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<正> “双专业”,即大学生入学一年后根据自己的能力选择自己喜读的两个专业,把两个专业的课程修满学分达到要求后得到两个专业的毕业证书。北京大学法律学系从1994年开始实行“双专业”教育。通过一年多的实践,其利弊不同程度地显示出来,就此,谈谈我对双专业实施问题的见解和看法。 实行双专业,它是对传统高等教育模式的一种补充和完善,需要在实践中不断进行检验。法律系实行双专业在北大教学改革中实属首创,其有利之处可归纳为以下三点: 相似文献
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刺激性毒物西阿尔(CR)的检验 总被引:1,自引:0,他引:1
目的简要介绍刺激性毒物西阿尔的物理、化学性质及检验方法;方法使用直接提取法对常见检材进行提取,使用TLC、GC/MS方法对其进行定性分析,以西阿尔在不同展开系统下的Rf值和特征质谱图作为定性依据;结果可快速准确的对西阿尔进行定性分析;结论该方法简便,易行,准确,可靠,可用于案件检验。 相似文献
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固相萃取是近年发展起来的一种样品前处理技术,主要用于样品的分离和富集,能够将生物检材中的目标待测物有效的与杂质组分分离,具有较高的回收率,其样品预处理过程简单,操作便捷。在法庭科学领域,可根据生物检材,如生物体液、组织、毛发等基质的性质,选择相应的固相萃取方法;同时亦可根据目标待测物,如目标待测物的酸碱性,选用不同的固相萃取方法。色谱法是一种分离和分析方法,它利用不同物质在不同相态的选择性分配,使混合物中的不同组分根据其性质不同而分离。质谱法在分析中可提供丰富的结构信息。固相萃取-色谱质谱联用技术集固相萃取与色谱质谱检测技术优点于一体,可实现对复杂基质中的特定毒物与非特定毒物进行高效萃取、净化与检测,具有检材消耗少、检测速度快、灵敏度高等特点,已被广泛应用于环境监测、药物分析、法庭科学领域等,成为当前毒物筛查的重要手段,具有选择性好、灵敏度高、基质效应低等特点,且易实现在线分析,特别适用于法庭毒物分析中单一毒物或多种毒物的筛查。本文综述了固相萃取-色谱质谱联用技术在法庭科学毒物毒品分析中的应用进展,以供同行参考。 相似文献
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红外光谱在毒药物检验中的应用 总被引:1,自引:0,他引:1
目的 建立毒药物检验的红外光谱测定方法。 方法 用液液萃取法提取检材中的安眠药、精神药品、农药、杀鼠剂和无机毒物 ,然后应用红外光谱法进行定性分析。 结果 常见毒药物均有其特征红外吸收峰 ,通过其特征吸收峰可以区分不同毒药物。 结论红外光谱法快速、准确 ,适用于干扰较轻检材中毒药物的定性分析。 相似文献
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An evaluation of fused silica capillary columns for the screening of basic drugs in postmortem blood: qualitative and quantitative analysis 总被引:1,自引:0,他引:1
Fused silica capillary columns (Durabond) have been evaluated for the screening of more than 100 basic drugs in postmortem blood samples. The combination of these columns, nitrogen-phosphorus detectors, and SKF-525A (internal standard) allows for the simultaneous screening and quantitation of several basic drugs such as amphetamines, amitriptyline, and codeine. Approximately 2000 blood samples have been analyzed by this procedure. The use of capillary columns results in excellent baseline stability and this, together with an autosampler and data system, enables unattended overnight operation. "Double peaking" associated with splitless injection can be a problem as can sensitivity for some of the polar drugs; however, with the extraction procedure described and the equipment used, the screening of blood for basic drugs is improved when compared with packed column technology. 相似文献
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《Science & justice》2022,62(2):193-202
Cyanide is a powerful and rapidly acting poison. In Japan, cyanide poisoning is rare, and regular cyanide testing can be costly and time consuming. In contrast, alcohol analysis is routinely performed in most forensic laboratories. In this study, we attempted to develop a method for the simultaneous quantification of cyanide and alcohols in blood using headspace gas chromatography (HS–GC). As nitrogen-phosphorus detection (NPD) is more sensitive to hydrogen cyanide than mass spectrometry (MS), a Deans switch was used to switch the detectors during a single run. The separation provided by three analytical columns, PoraBOND Q, CP-Sil 5 CB, and HP-INNOWax, was investigated, and PoraBOND Q was selected. The use of HS–GC–MS/NPD with a Deans switch enabled the simple and simultaneous quantification of cyanide, ethanol, and 1-propanol. Eighteen other volatile compounds were detected in the SIM/scan mode of the MS. 相似文献
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A novel method for the forensic analysis of commercial petroleum products is presented. In this approach, the petroleum sample is extracted with nitromethane and then separated by capillary liquid chromatography with laser-induced fluorescence detection. The addition of selective fluorescence quenching agents allows the sample to be profiled by the distribution of alternant and nonalternant polycyclic aromatic hydrocarbons (PAHs). In preliminary studies, the quenching behavior of nitromethane and diisopropylamine was established by using a standard mixture of sixteen PAHs ranging in size from two to six aromatic rings. Subsequent examination of new and used motor oil demonstrated that characteristic differences arise in the PAH content, which may allow for the unique identification of oil from a particular engine or vehicle. In addition, three brands of petrolatum jelly were successfully distinguished. Although a number of alternant alkylated and heterocyclic PAHs were found in all petrolatum samples, there were significant differences in the relative concentrations of alternant as well as nonalternant PAHs. This allowed for clear differentiation of the samples through qualitative inspection of their chromatograms as well as quantitative statistical correlation techniques. 相似文献
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Fast Gas Chromatography (GC) allows for analysis times that are a fraction of those seen in traditional capillary GC. Key modifications in fast GC include using narrow, highly efficient columns that can resolve mixtures using a shorter column length. Hence, a typical fast GC column has an inner diameter of 100–180 μm. However, to maintain phase ratios that are consistent with typical GC columns, the film thickness of fast GC stationary phases are also low (e.g., 0.1–0.18 μm). Unfortunately, decreased film thickness leads to columns with very low sample capacity and asymmetric peaks for analytes that are not sufficiently dilute. This paper describes micro-bore (50 μm i.d.) capillary columns with thick films (1.25 μm), and low phase ratios (10). These columns have greater sample capacity yet also achieve minimum plate heights as low as 110 μm. Hence, separation efficiency is much higher than would be obtained using standard GC columns. The capillary columns were prepared in-house using a simple static-coating procedure and their plate counts were determined under isothermal conditions. The columns were then evaluated using temperature programming for fast GC–MS analysis of ignitable liquids and their residues on fire debris exemplars. Temperature ramps of up to 75 °C min?1 could be used and separations of ignitable liquids such as gasoline, E85 fuel, and lighter fluid (a medium petroleum distillate) were complete within 3 min. Lastly, simulated fire debris consisting of ignitable liquids burned on carpeting were extracted using passive headspace absorption-elution and the residues successfully classified. 相似文献
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In forensic examination of illicit heroin samples high-resolution capillary gas chromatography is compared with gas chromatography with packed columns. Separation efficiency, reproducibility of qualitative and quantitative determinations and stability of the columns are examined.A practical method with silylation of the samples is presented which allows safe identification and quantification of many various compounds contained in illicit heroin samples. The gas chromatographic data of 35 substances (opium alkaloids and synthetic derivatives, adulterants and diluents) are listed. The method also allows the quantification of morphine, opium, and cocaine samples. 相似文献
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Inductively coupled plasma mass spectrometry (ICP-MS) was used to analyze glass evidence from a case in which a person broke a window in each of 15 vehicles in a parking lot in order to gain entry into the vehicles. The results of the analysis by traditional methods, which measure the properties of color, thickness, density, and refractive index, are also reported. A total of 15 known samples representing the windows on the cars and 42 questioned glass fragments recovered from the suspect and the police vehicle where the suspect was sitting were submitted for analysis. Density comparisons separated one of the known samples into three samples, increasing the number of known samples from 15 to 17. The concentrations of 16 elements were measured for all but three of the samples using an external calibration ICP-MS method with internal standardization. Color assessment (non-instrumental) separated the 17 known samples into two groups, and refractive index measurements resulted in six groups when the Emmons double variation method was used and ten groups when the Glass Refractive Index Measurement 2 (GRIM2) system was used. Elemental analysis, by itself, differentiated all of the known samples from each other and associated four of the known sample fragments with several of the questioned sample fragments. The informing power of RI, density, and elemental analysis comparisons is evaluated and a summary of the case results is reported. 相似文献
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A simple and rapid method for isolation of seven antiepileptics (2 hydantoin, 2 oxazolidin, and 3 suximide derivatives) from urine and plasma is presented. Urine and plasma (1 ml) samples containing seven antiepileptics were mixed with distilled water (4 ml), and the sample solution was poured into a pretreated Sep-Pak C18 cartridge; this was washed with water and chloroform/methanol was passed through it to elute the antiepileptics. The eluate was mixed with isoamyl acetate and evaporated under a stream of N2. The drugs were detected by gas chromatography with fused silica capillary columns, splitless injection and flame ionization detection. Separation of the seven antiepileptics from each other and from impurities was satisfactory with the use of an SPB-1 capillary column. The detection limit for the seven antiepileptics with the present method was 0.1-1.0 microgram/ml urine or plasma. The recovery of the drugs from urine and plasma was more than 70% and 50%, respectively. 相似文献