甲醛对一氧化碳中毒血检验干扰的研究

目的探讨甲醛对一氧化碳中毒血的检测是否产生干扰,提高一氧化碳中毒鉴定的可靠性。方法采用常用的血中一氧化碳或碳氧血红蛋白饱和度的检测方法对未加甲醛和加甲醛的血样分别进行实验研究。结果甲醛对加热法、氢氧化钠法、氯化钯法、分光光度法等检测方法均可产生不同程度的干扰。结论经福尔马林灌注或固定的检材不宜用于一氧化碳中毒血检测,否则可能导致错误的鉴定结论。     

常规硅藻检验法的改良

日常办案中,硅藻检验常用的方法是硝酸酒精破机法,但如遇到脂肪的干扰,可能影响检验结果。为了减少人体组织脂肪对硅藻检验的影响和对现场对水样的快速处理,笔者对传统的硝酸破机法进行了改良,使操作更为简单,适用,现报道如下。     

毛细管电泳在毒品检验中的应用

毛细管电泳因其自身特性而适用于毒品检测。本文重点对毛细管电泳的五种模式在毒品检验中的应用进行了综述和比较 ,包括各自检测方法的应用范围、优点和局限。     

朱墨时序的应用及检验方法

朱墨时序的检验在文件检验领域中较为常见。本文主要是在许多文献的基础上以及本人从事文检工作中取得的一点经验,对现如今经常使用的解决朱墨时序问题的几方法的优点、适用范围以及其局限性进行深入的比较分析。     

几种朱墨交叉时序的检验方法及其比较分析

文件朱墨交叉时序的确定一直是困扰文检界的难题之一.本文简要介绍了目前常用的六种检验方法,并结合五个典型案例对各种检验方法进行比较分析,以探讨针对不同形成条件的文件物证进行检验时采用哪些检验方法更为有效的解决问题.希望能够在同类问题的研究上达到抛砖引玉的效果.     

常见油漆稀料的GC／MS的检验及分类研究

目的对常用油漆稀料的检验分析方法及分类进行研究,并建立SPME-GC／MS对纵火案件中油漆稀料快速、灵敏、准确的分析方法。方法采用SPME-GC／MS法对5种不同型号品牌的常见油漆稀料进行分析。结果确定了样品处理方法和仪器分析最佳条件。实验的5种油漆稀料样本根据组分特征和结构特征的不同可归纳为4类。结论该研究结果可为纵火案件中油漆稀料残留物提供一种新的检验方法和检验依据。     

文件朱墨时序的检验方法及其比较分析

文件朱墨时序的判定是文件检验领域的难题之一。本文以38篇文献为基础,综述了目前常用的解决朱墨时序问题的十一种方法。并对各种方法的适用范围、优点和局限进行比较分析,以期为文检工作者视检材的具体情况采用合适的检验方法,提供一些参考。     

应用数理统计t检验方法进行步法研究的探讨

目前,步法研究大多还停留在定性分析的经验阶段。本文旨在试用数理统计t检验方法进行定量分析,鉴别犯罪现场所遗留下的足迹步法,为认定或否定罪犯,提供一种新的研究方法和手段,该方法应是科学的行之有效的,同时,对足迹步法的深入研究亦提供了可靠的科学理论依据。     

清代的司法检验

清代司法检验在宋、元、明三代的基础上有了长足的进步发展,主要表现在一、司法检验的体系和制度进一步完善;二、检验方法虽超不出《洗冤录》以经验为主的范围,但对《洗冤录》确实有不少的订正补充,其中也积累了丰富的检验实例和经验。     

解释性适用：国际人权法在国内法院适用的新趋势

采行一元论和采行二元论的国家,在司法实践中出现了某种融合的趋势,解释性适用方法被广泛采用。这种方法以国内法为依托,通过援引国际人权法解释国内法的方式,实现国际人权法在国内的间接适用。可以作为解释资源的国际人权文件范围广泛,实际范围会受到各国国内法院所持的不同原理的影响。按照对国际法和国内法关系的不同理解,国内法院解释适用的具体方法可以被分为“立足于国内价值”的方法和“立足于国际价值”的方法两类。在国际人权法尚无法在我国法院直接适用的情况下,“解释性适用”方法为我们提供了一个突破现实瓶项的可选路径。具体而言,我们应当立足于“国内价值”,从价值增进型、价值确认型和语境解释这三种方法中选择适当的方法进行探索性实践和运用。     

Comparison of Different Analytical Methods for the Determination of Carbon Monoxide in Postmortem Blood

The determination of carbon monoxide (CO) and carboxyhemoglobin (COHb) is of utmost importance in forensic toxicology to determine the cause of death in cases of CO poisoning, fire, and explosions. To this end, reliable and updated analytical methods are required. In this paper, four different methods for the determination of carbon monoxide in postmortem blood samples were compared: (i) the spectrophotometric determination of COHb applying the method proposed by Rodkey and modified by Beutler–West, (ii) the spectrophotometric determination of CO using a micro-diffusion-based method, (iii) the determination of CO by gas chromatography coupled to a TCD detector, and (iv) the determination of COHb by blood gas analysis. Three postmortem blood samples were analyzed with all methods, and the results were comparable. The applied methodologies showed different features depending on the sensitivity, sample preparation, and volume. The HS-GC/TCD method in our hand was the most appropriate, on postmortem samples, and versatile to apply. Unfortunately, only a limited number of postmortem blood samples were available for this study due to the rarity of that kind of intoxication in our jurisdiction.     

Achiral and chiral quantification of methamphetamine and amphetamine in human urine by semi-micro column high-performance liquid chromatography and fluorescence detection

In this paper, miniaturized achiral and chiral high-performance liquid chromatographic procedures for the determination of methamphetamine and amphetamine in human urine are described. After a simple pretreatment of human urine (i.e., 10 microL of urine or diluted urine were acidified and dried-up under N2 at room temperature) and fluorescence derivatization with 4-(4,5-diphenyl-1H-imidazol-2-yl)-benzoyl chloride under mild conditions (pH 9.0, 10 min at room temperature), the derivatives were isocratically separated on a semi-micro ODS column with Tris-HCl buffer (0.1 M, pH 7.0): acetonitrile (45 + 55 v/v) at a flow rate of 0.2 mL/min or their enantiomers were separated on a semi-micro OD-RH column with sodium hexafluorophosphate (0.3 M aq.): acetonitrile (44 + 56 v/v) at a flow rate of 0.1 mL/min as the mobile phase. Wide-ranged calibration curves were obtained with detection limits for the achiral and chiral analyses in the atto and femtomol levels, respectively, per injected volume. Satisfactory within- and between-day reproducibility data were obtained with both the methods with the highest relative standard deviation being 9.6%. The methods were applied to the determination of methamphetamine and amphetamine in human urine samples and the concentrations determined by the two methods were well correlated (r = 0.994).     

Determination of cocaine in human hair by gas chromatography/mass spectrometry

A qualitative method for the determination of cocaine alone without its metabolites in human hair by gas chromatography/mass spectrometry (GC/MS) was developed. The assay used helium as carrier gas, a 30-m bonded phase fused silica OV-1 capillary column, and solid injection at 290 degrees C evaporator temperature. The cocaine concentrations in hair were determined also by radioimmunoassay (RIA). The values obtained are the sum of cocaine and its metabolites. Both GC/MS and RIA meet the requirements for the determination of drug abuse by two different methods in forensic science.     

The determination of cocaine and its major metabolite, benzoylecgonine, in postmortem fluids and tissues by computerized gas chromatography/mass spectrometry

An analytical procedure for the simultaneous determination of both cocaine and benzoylecgonine in postmortem fluid and tissue samples has been developed by using computerized gas chromatography/mass spectrometry and gas chromatography using a nitrogen/phosphorus (N/P) detector. Both methods are accurate and sensitive and allow the determination of tissue concentrations of cocaine and benzoylecgonine as low as 0.015 microgram/mL.     

尿中MDMA及其代谢物的GC和GC／MS分析

考察MDMA在人体内的代谢以及建立尿中MDMA和体内主要代谢物MDA的分析方法。尿样水解后经液-液提取处理,用GC／MS（EI、PCI）和GC／FID法分析。人摄入MDMA后尿中MDA和原体MDMA比约为0．10～0．14。GC／MS／SIM和GC／FID法的最低检出限为2ng／ml和50ng／ml,回收率大于85％,变异系数小于10％。该法简便快速、灵敏度高、结果可靠,可用于MDMA滥用者的尿样鉴定。MDA／MDMA浓度比可作为评判毒分结果的参考指标。     

Application of three spectrometric methods to total selenium determination in postmortem material in a case of acute selenium compound poisoning

Three spectrometric methods, that is, spectrofluorimetry (SF), atomic absorption spectrometry with electrothermal atomization (ET-AAS), and atomic fluorescence spectrometry with hydride generation (HG-AFS) were used for the determination of total selenium in biological samples taken from postmortem material in a case of acute selenium compound poisoning. The precision of the SF, ET-AAS, and HG-AFS methods (RSD, n=10) was found to be in the ranges of 10.0-15.0, 3.0-6.0 and 1.0-1.5%, respectively, and the detection limit was 10.0, 4.0, and 0.1 μg/L of Se, respectively. In the case of HG-AFS, the analytical procedure takes less time and is less laborious than the other methods considered. The obtained results show the usefulness of the HG-AFS method as a supplementary analytical tool to the SF and ET-AAS methods with respect to the determination of selenium as well as the possibility of using this method as a primary one in forensic toxicology practice.     

Investigations of clobazam (Frisium) by combined gas chromatography/mass spectrometry (author's transl)

Clobazam (Frisium) was hydrolyzed according to three methods commonly used in the determination of 1.4-benzo-diazepines; the reaction products were analyzed by gas chromatography/mass spectrometry and thin-layer chromatography. Five degradation products were obtained for which structure proposals are discussed. After oral intake two of these substances were also detected in human urine. It should be recognized that some of the above mentioned substances may be on-column degradation products of artifacts occurring during hydrolyzation and/or sample clean-up.     

尿液、血液中γ-羟丁酸的气质联用法分析

目的为尿液、血液中γ-羟丁酸(gamma-hydroxybutyricacid,GHB),γ-羟丁酸内酯(gamma-butyrolactone,GBL)和1,4-丁二醇(1,4-butanediol,1,4-BD)的鉴定提供方法和依据。方法100μl尿液或血液以GHBd6为内标,经乙酸乙酯提取、BSTFA衍生化后,用GC／MS法分析。结果测尿液中内源性GHB的线性范围是20-800ng／ml,R2=0.9995,最低检出限为10ng／ml(S／N≥3);测尿液、血液中外源性GHB的线性范围为5-60μg／ml,R2分别为0.9999和0.9928。相对回收率为99％-104％。以所建方法测定了健康志愿者尿液中内源性GHB含量,并考察了健康受试者外源性GHB的代谢情况。结论所建方法准确、便捷、省时、选择性好,适用于法医毒物学鉴定。     

The determination of drugs of abuse in whole blood by means of FPIA and EMIT-dau immunoassays--a comparative study

Six groups of common drugs of abuse (cannabinoids, benzoylecgonine, opiates, barbiturates, benzodiazepines and amphetamines) were determined in whole blood after acetone precipitation, using enzyme multiplied immunoassay (EMIT dau) and fluorescence polarisation immunoassay (FPIA--Abbott TDx and ADx) methods. Both methods, designed primarily for urine, allowed the determination of all above mentioned class of drugs but amphetamine. Only 1 ml of a pre- or postmortem blood sample was needed. The sensitivity of cannabinoids determination was higher by FPIA. The FPIA method gave more precise results, particularly in the case of autopsy blood. The method was applied for drug screening in autopsy and police blood samples. The results (both positive and negative) were in agreement with those obtained with chromatographic methods.     

The determination of psilocin and psilocybin in hallucinogenic mushrooms by HPLC utilizing a dual reagent acidic potassium permanganate and tris(2,2'-bipyridyl)ruthenium(II) chemiluminescence detection system

This paper describes a procedure for the determination of psilocin and psilocybin in mushroom extracts using high-performance liquid chromatography with postcolumn chemiluminescence detection. A number of extraction methods for psilocin and psilocybin in hallucinogenic mushrooms were investigated, with a simple methanolic extraction being found to be most effective. Psilocin and psilocybin were extracted from a variety of hallucinogenic mushrooms using methanol. The analytes were separated on a C12 column using a (95:5% v/v) methanol:10 mM ammonium formate, pH 3.5 mobile phase with a run time of 5 min. Detection was realized through a dual reagent chemiluminescence detection system of acidic potassium permanganate and tris(2,2'-bipyridyl)ruthenium(II). The chemiluminescence detection system gave improved detectability when compared with UV absorption at 269 nm, with detection limits of 1.2 x 10(-8) and 3.5 x 10(-9) mol/L being obtained for psilocin and psilocybin, respectively. The procedure was applied to the determination of psilocin and psilocybin in three Australian species of hallucinogenic mushroom.