UPLC-MS/MS法同时检测全血中16种除草剂

目的建立全血中16种除草剂的超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测方法,为除草剂中毒案事件及其他刑事案件血液中该16种除草剂的检验鉴定提供依据。方法取200μL的血液,加入800μL乙腈-水(体积比80/20),进行蛋白沉淀后,采用Acquity BEH C18(2.1mm×100mm,1.7μm)色谱柱,以水(5mmol/L的甲酸铵,0.1%的甲酸)-乙腈为流动相进行梯度洗脱,采用电喷雾离子源(ESI)、多反应监测(MRM)正离子模式对16种化合物进行检测。结果在1~200ng/mL范围内线性关系良好,R2均大于0.996;基质效应(ME%)为85.2%~104.4%,相对标准偏差(RSD%)为0.72%~4.84%;仪器检出限(IDLs)为0.2~2 ng/mL(信噪比S/N≥3),方法检出限(MDLs)为0.5~3ng/mL(信噪比S/N≥3),最低定量限(LOQs)为1~7ng/mL(信噪比S/N≥10)。结论本实验建立的全血中16种除草剂同时检验方法,前处理简便快捷、回收率高、精密度好、方法检出限低,可作为该16种除草剂中(投)毒案件的检验方法。     

Evaluation of methyl tert-butyl ether (MTBE) as an interference on commercial breath-alcohol analyzers.

Anecdotal reports suggest that high environmental or occupational exposures to the fuel oxygenate methyl tert-butyl ether (MTBE) may result in breath concentrations that are sufficiently elevated to cause a false positive on commercial breath-alcohol analyzers. We evaluated this possibility in vitro by establishing a response curve for simulated breath containing MTBE in ethanol. Two types of breath-alcohol analyzers were evaluated. One analyzer's principle of operation involves in situ wet chemistry (oxidation of ethanol in a potassium dichromate solution) and absorption of visible light. The second instrument uses a combination of infrared absorption and an electrochemical sensor. Both types of instruments are currently used, although the former method represents older technology while the latter method represents newer technology.The percent blood alcohol response curve was evaluated over a breath concentration range thought to be relevant to high-level environmental or occupational exposure (0-361 microg/l). Results indicate that MTBE positively biases the response of the older technology Breathalyzer when evaluated as a single constituent or in combination with ethanol. We conclude that a false positive is possible on this instrument if the MTBE exposure is very high, recent with respect to testing, and occurs in combination with ethanol consumption. The interference can be identified on the older technology instrument by a time dependent post-reading increase in the instrument response that does not occur for ethanol alone. In contrast, the newer technology instrument using infrared and electrochemical detectors did not respond to MTBE at lower levels (0-36 microg/l), and at higher levels (>72 microg/l) the instrument indicated an "interference" or "error". For this instrument, a false positive does not occur even at high MTBE levels in the presence of ethanol.     

家兔死后体表锐器伤出血现象的研究

目的对家兔死后体表锐器损伤出血现象进行研究,以期能够贴近实际办案需要,找到一个更为实用的鉴别生前锐器伤和死后锐器伤的方法。方法家兔脱毛,制作锐器损伤模型,采用大体观察结合HE染色镜下组织病理学观察。结果死后锐器损伤出血量均较少,随着时间延长出血量减少,出血速度慢。死后30min的锐器损伤在形成过程与生前损伤有所区别,但在死后12h肉眼观察结果与生前损伤难以区别。死后1h以上的锐器损伤与生前损伤不同之处在于创缘不会被血染。结论位于尸体低下位置的死后30min内的锐器创与生前锐器创的区别是出血量相对较少。死后60min-90min的锐器伤出血量少,创缘皮肤不被血染,肌肉的出血较局限,与生前损伤相鉴别较容易。     

AutoMate Express™ forensic DNA extraction system for the extraction of genomic DNA from biological samples

Abstract: The AutoMate Express? Forensic DNA Extraction System was developed for automatic isolation of DNA from a variety of forensic biological samples. The performance of the system was investigated using a wide range of biological samples. Depending on the sample type, either PrepFiler? lysis buffer or PrepFiler BTA? lysis buffer was used to lyse the samples. After lysis and removal of the substrate using LySep? column, the lysate in the sample tubes were loaded onto AutoMate Express? instrument and DNA was extracted using one of the two instrument extraction protocols. Our study showed that DNA was recovered from as little as 0.025 μL of blood. DNA extracted from casework‐type samples was free of detectable PCR inhibitors and the short tandem repeat profiles were complete, conclusive, and devoid of any PCR artifacts. The system also showed consistent performance from day‐to‐day operation.     

The gas chromatographic determination of carbophos in cadaveric material

The authors developed a method of malathion insecticide determination in the cadaveric material (blood and wall of the stomach) including extraction of 5 ml of blood (5 g of fragmented tissue of stomach wall) by hexan; preparative chromatographic purification of extract on silicagel layer L 5/40 mkm in hexan-diethyl ether system 10:2; Gas-liquid chromatographic investigation on column with 5% SE-30 and 5% XE-60 (Chromatograph "Colour-106" with thermionic detector). This method makes it possible to detect 72-76% of malathion added.     

根据双刃刺器刺创口推断刺器宽度

解决根据皮肤创口推断刺器宽度的问题。实验在自愿捐献的12具男性尸体的胸部,用不同宽度和厚度的双刃匕首致创221个。应用法医学、解剖学及数理统计的理论和技术对创口形成机理、影响因素及其与刺器宽度的相关关系进行分析,得出了以下结论：刺器厚度与创口长度无明显相关,刺器宽度与创口长相关,创口回缩程度与创口方向及刺器宽度相关。并建立了两个最优回归方程,提出了一个根据皮肤双刃利器创口推断刺器宽度的方法。     

Distribution of A and B antigens in organs of blood group AB individuals: observations disclosed by a double immunoenzymatic labeling method

The localization of A and B antigens in the organs of blood group AB individuals has been studied using a double immunoenzymatic labeling method. Both A and B antigens were found in the various epithelial cells of these organs, but the epithelial cells could be classified into the following four types depending on the reaction pattern with anti-A and anti-B sera: type 1: cells that stained positive with both anti-A and anti-B sera; type 2: cells that stained positive with anti-A serum only; type 3: cells that stained positive with anti-B serum only; type 4: cells that were negative with both sera. The distribution of each of these epithelial cell types varied considerably, even in the same tissue and individual. Our results seem to suggest that a dissociation in the conversion to the A and B antigens occurs in the tissue of individuals belonging to blood group AB and that the degree of this dissociation varies from tissue to tissue and from cell to cell.     

GC/NPD、GC/FID分析生物样品中的氟乙酰胺

报道了用ＧＣ／ＮＰＤ、ＧＣ／ＦＩＤ分析生物试样中的氟乙酰胺的方法。在１ｇ肝组织中加入５．０μｇ氟乙酰胺,回收率为８５．１％,ＲＳＤ为５．３９（ｎ＝７）;１ｍｌ血中加５μｇ,回收率为８５．１％,ＲＳＤ为７．１１％;在１ｇ胃组织中加入１０μｇ,回收率为８１．６％,ＲＳＤ为１０．１％（ｎ＝７）。研究的方法经动物实验和中毒案件的应用,效果较好     

液相色谱-串联质谱法测定血液和尿液中秋水仙碱

目的建立检测血液和尿液中秋水仙碱的液相色谱-串联质谱法。方法0.5mL血液或尿液以丁丙诺啡为内标,经pH9.2硼酸盐缓冲溶液碱化后,用乙酸乙酯进行提取,在ZORBAX SB-C18液相柱(150mm×2.1mm×5μm)上以V(甲醇)∶V(20mmol/L乙酸铵和0.1%甲酸缓冲溶液)=80∶20为流动相,流速为0.2mL/min,采用电喷雾正离子模式离子化、多反应监测模式检测秋水仙碱,内标法定量。结果血液、尿液中秋水仙碱与内标丁丙诺啡色谱分离良好,秋水仙碱在0.1~50 ng/mL内均具有良好的线性,相关系数>0.9990,最低检出限为0.05ng/mL,方法回收率为94%~116%,日内与日间精密度(RSD)均小于8.5%。结论所建LC-MS-MS方法灵敏度高、操作简便、快速、准确,适用于血液及尿液等生物检材中痕量秋水仙碱成分的检测。     

Special design characteristics of the Japanese "Tan-to" (knife) as criteria for dangerousness

The great angle gauge of the blade top and the asymmetrical sharpening of the edge, the thickness of the blade (nearly 0.3 cm) and especially the short sharpened blade top give excellent stability of the cutting edge of this instrument and of its blade top. Flat bones can be perforated very easily without damaging the blade top. In recent times a newly developed Japanese tan-to is available in the FRG. The blade of this dagger can be fixed at right angles to the knife-handle, ready for use just as an "American San Francisco Push-Dagger" or an Indian "katar", obviously very dangerous weapons. The possession of this new generation of Japanese tan-to should be legally prohibited.     

Skeletal muscle as an alternative specimen for alcohol and drug analysis

In a random group of medical examiner cases, muscle tissue, as well as blood and vitreous humor, was analyzed for ethyl alcohol, and the results were compared. When the blood concentration was greater than 0.10 g/dL, the muscle to blood ratio was 1.00 or less (average 0.94), and when the blood concentration was less than 0.10 g/dL, this ratio was greater than 1.00 (average 1.48). The author proposes that this ratio is dependent upon the time course of absorption and distribution, as has been observed for vitreous humor, but with a more rapid equilibration. Muscle tissue was also analyzed in another group of cases found to be positive for one or more drugs in blood. The concentrations of the drugs in muscle varied from none detected to 6.5 times those in blood and seemed to be dependent on the time course between ingestion and death, as well as on the nature of the drug. For most common basic drugs, the ratios were often near unity. Muscle is proposed as a useful alternative specimen to postmortem blood.     

小鼠各脏器及血中甲基苯丙胺的分布

目的通过给小鼠腹腔注射甲基苯丙胺(MAMP),建立小鼠急性染毒模型。方法运用GC/NPD技术,系统地进行了染毒小鼠模型各脏器及血中甲基苯丙胺(MAMP)的定性定量测定。采用1-萘胺作为内标,样品处理时采取加盐酸成盐后,又碱化,用有机溶剂萃取浓缩挥发。结果回收率高于80%。血、各脏器中最低检出限为2～5ng/ml。结论脑、肾、脾组织可以用于法庭科学分析。     

体位性窒息对脑血管损伤的实验观察

目的 观察体位性窒息对脑血管损伤的影响。方法 家兔20只,致其中10只体位性窒息,另10只断颈处死进行对照。用兔抗人白蛋白抗体和兔抗人(von Willebrand Factor,vWF)抗体进行LSAB免疫组化法显色。结果抗人白蛋白抗体及抗人vWW、检测均显示出阳性;对照组显示不明显。秩和检验显示,两组间具有显著性差异。结论　在体位性窒息时,呼吸障碍所引起的缺氧,可损害脑血管的正常结构。     

精神病犯服刑能力评定量表研究

目的制订符合中国法律体系的精神病犯服刑能力评定量表。方法根据鉴定实践,结合中国法律,研究者首先创建了称为“精神病犯服刑能力评定量表”的评定工具,然后再回顾性运用该工具,通过诊断性实验,对该工具的信度、效度及实用性进行了检验。结果该量表同质性信度为0.8779,量表评定与专家评定一致性为0.909,除了阴性似然比为0.0683,其他诊断性指标均大于0.80。结论精神病犯服刑能力评定量表具有较好的实用性。     

液相色谱/质谱法检测血液中的艾司佐匹克隆

目的建立手性分离-液相色谱/质谱法,用于分离检测血液中艾司佐匹克隆。方法血液经HLB小柱固相萃取后,采用手性分离柱,用电喷雾正离子模式离子化、多反应监测模式检测艾司佐匹克隆,外标法定量。结果采用本文方法可有效分离佐匹克隆的左旋、右旋异构体,血中艾司佐匹克隆在1～100ng/mL范围内线性关系良好,相关系数为0.996 4,最低检出限为0.8ng/mL,回收率为76%～88%,日内与日间精密度均小于8%。结论本文所建方法简便、快速、分离度好,适用于血液中艾司佐匹克隆的检测。     

中国刑法教义学:经验、反思与建构

当代中国刑法教义学经历了去政治化工具的教义学、作为解释学工具的教义学及作为学科精致化工具的教义学的发展节点。面临实定法的粗疏与缺陷,理论继受过程中的移植落差,中国刑法教义学的发展呈现出诸多特殊的面向。一方面是中国刑法实定法规定的非理性,另一方面是刑法教义学本身的高度理性,二者之间形成了持久的紧张关系,在这种紧张关系之中开展教义学研究需要厘清实定法不可质疑性前提与教义学科学性的关系、立法论与解释论的关系,培育连接立法-司法-法学研究者的教义学共同体,同时警惕对德日刑法教义学的过度路径依赖,积极进行本土化教义学理论的创新与构建。     

Postmortem determination of the biological distribution of sufentanil and midazolam after an acute intoxication

A case is presented of a death caused by self-injection of sufentanil and midazolam. Biological fluids and tissues were analyzed for midazolam by high performance liquid chromatography (HPLC) and gas chromatography/mass spectrometry (GC/MS) and for sufentanil by GC/MS. Midazolam was extracted from basified fluids or tissues homogenated with n-butyl chloride and analyzed by HPLC by using a phosphate buffer: acetonitrile (60:40) mobile phase on a mu-Bondapak C18 column at 240 nm. Sufentanil was extracted from basified fluids and tissue homogenates with hexane:ethanol (19:1). GC/MS methodology for both compounds consisted of chromatographic separation on a 15-m by 0.25-mm inside diameter (ID) DB-5 (1.0-micron-thick film) bonded phase fused silica capillary column with helium carrier (29 cm/s) splitless injection at 260 degrees C; column 200 degrees C (0.8 min) 10 degrees C/min to 270 degrees C; and electron ionization and multiple ion detection for midazolam (m/z 310), methaqualone (IS, m/z 235), sufentanil (m/z 289), and fentanyl (IS, m/z 245). Sufentanil concentrations were: blood 1.1 ng/mL, urine 1.3 ng/mL, vitreous humor 1.2 ng/mL, liver 1.75 ng/g, and kidney 5.5 ng/g. Midazolam concentrations were: blood 50 ng/mL, urine 300 ng/mL, liver 930 ng/g, and kidney 290 ng/g. Cause of death was attributed to an acute sufentanil/midazolam intoxication and manner of death a suicide.     

Determination of Both Fetus’ and Mother's Blood Type from an Autopsy Case Immersed in Formalin for Over 50 Years

A female fetus which had been immersed in formalin for more than 50 years was found in Japan. Because no liquid blood could be obtained, we tried to use immunohistochemistry (IHC) methods to tissue samples obtained at autopsy to identify both the fetal and mother's blood type. We detected B antigens on endothelial cells in paraffin sections of the fetal organs. Furthermore, we observed both anti‐A‐ and anti‐B‐positive red blood cells in the intervillous space, which is indicative of the mother's blood type. To our knowledge, this is the first case report on determining the blood type of both the fetus and the mother from tissue immersed in formalin for such a long time. The results suggest that IHC is valuable for the determination of ABO blood type in circumstances of long postmortem duration and unfavorable storage conditions.     

PryJector: a device for in situ visualization of chemical and physical property distributions on surfaces using projection and hyperspectral imaging

Traditional forensic methods that highlight the spatial distribution of properties such as blood and fingerprints have two main disadvantages: they often apply chemicals that may influence further analyses, and they cannot easily be modified to search for new compounds/properties. A new instrument (called PryJector) avoids these problems by dynamically projecting back onto the surface under study spatially distributed information of compounds/properties (chemical images) obtained from multivariate analysis of hyperspectral images. Selectivity to target compounds/properties is ensured by multivariate modeling which makes the instrument much more flexible compared to traditional methods. The functionality of the PryJector is demonstrated in an application related to the detection of counterfeit pharmaceuticals where compounds otherwise indistinguishable to the human eye are made clearly visible by projection of false-colored chemical images. The PryJector is shown to be a noninvasive and very flexible instrument for highlighting spatial distributions of various compounds/properties.     

The extent of postmortem drug redistribution in a rat model.

The aim of this study was to investigate the postmortem redistribution of several drugs in a rat model and to examine if any of the pharmacological properties was related to the extent of this phenomenon. One of the following drugs: phenobarbital (phenobarbitone), acetaminophen (paracetamol), carbamazepine, codeine, verapamil, amphetamine, mianserin, trimeprazine (alimemazine) or chloroquine was administered together with nortriptyline orally to rats 90 min prior to sacrifice. Heart blood was sampled immediately before sacrifice and after 2 h postmortem, as it has previously been shown that this is sufficient time for postmortem concentration changes to occur in heart blood. Blood was also sampled from the clamped abdominal inferior vena cava (representing peripheral blood) and tissue samples were taken from lungs, myocardium, liver, kidney, thigh muscle, forebrain, and vitreous humor together with a specimen from the minced carcass. Drugs were analyzed by high performance liquid or gas chromatography. For phenobarbital, acetaminophen and carbamazepine the postmortem to antemortem blood drug concentration ratios were close to 1.0 and tissue concentrations were low. The postmortem to antemortem heart blood drug concentration ratio for chloroquine (6.9 +/- 1.5) was higher than for nortriptyline (3.5 +/- 0.3), and the remaining drugs (codeine, verapamil, amphetamine, mianserin, and trimeprazine) showed ratios of the same magnitude as nortriptyline. The postmortem to antemortem blood drug concentration ratios for both heart blood and blood from the vena cava and also the lung to antemortem blood drug concentration ratio were closely related to the apparent volume of distribution for the drugs studied (p < 0.001). Accordingly, an apparent volume of distribution of more than 3-4 L/kg is a good predictor that a drug is liable to undergo postmortem redistribution with significant increments in blood levels. The postmortem drug concentration in blood from vena cava was closely related to the antemortem blood level, confirming that among the postmortem samples, the peripheral blood sample was the most representative for the antemortem blood concentration.