γ-羟基丁酸在急性中毒大鼠体液和组织中的检测及分布

目的建立生物检材中γ-羟基丁酸(GHB)的检测方法,研究GHB急性中毒大鼠体内GHB的分布,为GHB中毒的鉴定提供方法和评价依据。方法用GC/MS法检测生物检材中的GHB;以1000mg/kg剂量给大鼠灌胃使其染毒,分别于1h和3h处死,测定体液和组织中GHB的含量。结果测组织中内源性GHB的线性范围是1～20μg/g,R2=0.9974;测组织中外源性GHB的线性范围为100～1500μg/g,R2=0.9958。相对回收率为98%～103%。体内内源性GHB的含量均≤10μg/mL或10μg/g。尿液中GHB含量为最高,其他依次为:胃、血液、肠、肾、肺、脾、心、肝和脑。结论所建方法准确、便捷,适用于GHB中毒的鉴定;尿液是体内检测GHB的最佳检材。     

吸附管／气相色谱／质谱法分析纵火案的纵火剂残留物

用吸附管(AT)/气相色谱(GC)/质谱(MS)法检测纵火残留物中轻质矿物油是通过吸附管动态吸附检材中可挥发的有机物,然后通过热脱附将挥发物送至GC及GC/MS中检测。它既适用于轻组份的碳氢化合物,如汽油,也适用于较高分子的碳氢化合物,如柴油和煤油。用沸石预处理样品克服了样品中水分对鉴定的干扰。用本方法能够得到比过去所使用的溶剂提取法或顶空法(HS)更高的吸附效率和灵敏度,解决了以往由于残留物中热解产物干扰所造成的GC图形混乱复杂,难以准确分析鉴定的问题。用本方法分析纵火或火灾案件中常见的残留物-轻质矿物油,具有快速、灵敏、准确和简便等特点,可广泛应用于公安、司法和保险等各个领域。     

GC/FID法分析生物检材中的三唑酮

本文通过实验研究,初步确立了以GC/FID法分析生物检材中三唑酮的方法,提取净化操作简单,回收率高,通过一起三唑酮中毒案件的检验,证明本方法适用于实际办案。     

毒性元素砷、汞、铅试样处理方法及等离子体光谱测试技术研究

本文详细地介绍了低温加压消化法处理生物样品中毒性元素砷、汞、铅的处理方法.研究表明样品处理回收率为92%～95%,检测灵敏度达 ppb级,相对标准偏差系数<2%.建立了一个适用于从痕量到高含量砷、汞、铅检材的毒化标准分析方法.结果表明该法灵敏度高、准确、简便、快速,对砷、汞、铅的检验水平提高到了国内最高水平.     

LC／MS／MS法测定生物组织中百草枯

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。     

尸体材料中对硫磷(1605)代谢产物氨基对硫磷的检测

本文报道了对硫磷(1605)中毒后其代谢产物氨基对硫磷的测定方法。检材中的氨基对硫磷经有机溶剂提取,用气相色谱(NPD)测定,在肝或血中的回收率皆在70％以上。本法适用于腐败组织中以检测氨基对硫磷来确定1605中毒。     

离子对SPE—HPLC法检测生物检材中的百草枯

目的建立生物检材中百草枯的简便、快速、灵敏、可靠的高效液相色谱分析方法。方法生物检材酶解后,用以十二烷基三甲基溴化铵和十二烷基硫酸钠预处理过的C18固相柱萃取,HPLC/DAD进行分析。结果回收率81%～94%,检出限为1ng·mL-1,线性范围50ng·mL-1～1mg·mL-1,结论此方法适用于中毒生物检材中百草枯的检测。     

生物检材中乌头碱的GC/MS分析

目的 建立GC/MS-SIM检测生物检材中乌头碱的定性方法。方法 以MSTFA作为衍生化试剂,吡啶为溶剂,于60℃反应30min,综合质谱图及保留时间定性分析。结果 经该方法测得乌头碱最小检出量为20ng(S/N≥100)。结论 GC/MS-SIM法适用于药材及生物检材中乌头碱的定性分析。     

HPLC法分析海洛因中毒死亡后生物检材中的吗啡

初步建立了以HPLC方法检测海洛因中毒生物检材中的吗啡方法,给出两种比较理想、可供定性、定量分析的色谱条件;生物检材处理,提取净化方法简便快速,并通过对10例海洛因中毒死亡者血液的检测,效果理想,实践证明方法可靠,适用于实际案件的鉴定。     

高效液相色谱法测定生物体液中百草枯

目的建立HPLC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,水溶性正相液相色谱分析,结合保留时间和紫外光谱对样品中百草枯进行定性。结果经该方法测得百草枯的最小检出限为10ng/m l血(S/N≥3),线性范围为0.1~10μg/ml。结论该方法快速、灵敏、准确,能有效祛除复杂生物基质中杂质干扰,使待测组分获得满意的峰形,适用于生物检材中百草枯的分析。     

Determination of carbon monoxide in blood by gas chromatography using a thermal conductivity detector

A method is described for the gas chromatographic quantitation of carbon monoxide by means of thermal conductivity detection. Carbon monoxide is released from blood samples as small as 0.02 mL using a unique extraction chamber. The method was compared to a standard gas chromatographic and spectrophotometric method of carbon monoxide quantitation. It was comparable to the former with all samples evaluated and apparently more reliable than the latter with decomposed samples.     

Gas chromatographic method of quantitative determination of carbon monoxide in cadaver blood

A gas chromatographic method has been developed for measurement of carbon monoxide in cadaveric blood on a chromatographer with thermal conductivity detector and air oxygen as the internal standard. The error of the method is no more than 4% with the mean quadratic deviation +/- 0.18-0.33 min. The method was studied on 10 model and 30 expert blood samples. Putrefactive products did not influence the accuracy of analysis.     

顶空气质联用法测定腐败血、肝检材中CO

目的研究CO中毒腐败血、肝组织检材中CO的HS/GC/MS检测。方法用HS/GC/MS法分析碳氧血红蛋白(COHb)血的线性范围。配制10%、30%、50%、70%浓度COHb血样,分别在室温、冷藏、冷冻条件下保存,分别在当日、第4、14、45d进行测定,比较实验结果。腐败肝组织由雄性健康家兔通CO气体致死,当天解剖,家兔肝常温隔绝空气保存并放35d至腐败,期间进行不定期顶空测定分析。结果制备的COHb血在0-100%之间有良好的线性关系Y=2.4X+2.2(r=0.9995)。以此方法测定家兔CO中毒致死的COHb新鲜血的浓度和4℃下放置45dCOHb腐败血,结果表明温度对血样中COHb%的测定影响最大。采用HS/GC/MS法检测,每次只需0.25ml血样或1g肝脏,分析一次时间只需3min,均可检测出新鲜检材和常温放置45d的腐败肝组织检材CO的含量。结论HS/GC/MS法能检出CO中毒的腐败生物检材中CO。     

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.     

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。     

Suicidal Carbon Monoxide Poisoning by Combining Formic Acid and Sulfuric Acid Within a Confined Space

Suicide by inhalation of carbon monoxide produced by mixing formic acid and sulfuric acid within a confined space is a rare method of suicide. This method is similar to the so‐called “detergent suicide” method where an acid‐based detergent is mixed with a sulfur source to produce hydrogen sulfide. Both methods produce a toxic gas that poses significant hazards for death investigators, first responders and bystanders. Carbon monoxide is an odorless gas, while hydrogen sulfide has a characteristic rotten eggs odor, so the risks associated with carbon monoxide are potentially greater due to lack of an important warning signal. While detergent suicides have become increasingly common in the USA, suicide with formic acid and sulfuric acid is rare with only three prior cases being reported. Greater awareness of this method among death investigators is warranted because of the special risks of accidental intoxication by toxic gas and the possibility that this method of suicide will become more common in the future.     

Death scene evaluation in a case of fatal accidental carbon monoxide toxicity

Exposure of humans to high concentrations of carbon monoxide can result in death, due to the formation of carboxyhaemoglobin (COHb), which impairs the oxygen carrying capacity of the haemoglobin. Carbon monoxide is responsible of a great number of accidental domestic poisonings and deaths throughout the world, particularly in homes that have faulty or poorly vented combustion appliances. A case is reported, in which a 21-year-old woman was found dead, due to carbon monoxide poisoning from a gas water heater, despite the puzzling evidence that the heater has been used for more than 10 years without any problem. An evaluation of the exposure to CO was performed, by measuiring the rate of production of CO from the heater, and using the Coburn-Forster-Kane equation to describe the kinetics of the poisoning process. The death was attributed to an accidental poisoning from carbon monoxide due to a sum of unfortunate circumstances.     

Suicidal and accidental carbon monoxide poisonings due to charcoal fires in closed spaces

The number of fatal carbon monoxide poisonings has significantly decreased since the introduction of natural gas. Apart from their occurrence during house fires, accidental and suicidal carbon monoxide poisonings are only rarely seen nowadays. We report on 7 cases of unintentional and intentional fatal carbon monoxide poisoning (CO-Hb concentrations between 56.4% and 74%) due to improper handling of charcoal fires in closed spaces. Autopsy findings and results of the toxicological analysis are presented and discussed.     

Suicide by inhalation of carbon monoxide in a residential fire

Fire deaths are usually accidental, but atypical cases of homicide or suicide have been described. In suicide by fire, the only method reported by several authors consists of self-immolation. We present here the unusual case of an adult female who committed suicide by waiting in the living room after setting fire to her bedroom. The autopsy revealed smoke inhalation and the toxicological analysis revealed carboxyhemoglobin levels of 67%. Very few cases of suicide by fire not of the self-immolation type have been reported, and all have been anecdotal. A review of the literature is presented and a new term, "suicide by inhalation of carbon monoxide in a fire," is proposed for such cases.     

Diagnosis of carbon monoxide poisoning following embalming and exhumation

Clots of blood, which were found in the cardiac ventricles at an autopsy of an embalmed corpse, were to analyse for carbon monoxide. It was not possible to determine reliably the CO-Hb-content of the blood clots with the known methods. Therefore a new procedure was developed. Carbon monoxide was released by a solution of nitric acid and determined gas chromatographically by a headspace method. In the same vessel the iron-content of the sample was measured after decomposition with atomic absorption spectrometry. This procedure is especially suitable for samples like putrid or heat-clotted blood.