微波消解ICP-MS法测定人发中的汞

目的建立人发中汞的电感耦合等离子体质谱分析方法。方法采用微波消解法处理样品,以铟（115In）作内标,用电感耦合等离子体质谱分析人发中的汞含量。结果方法检出限为0.0032μg/g,准确度通过测定人发标准物质GBW07601、GBW09101b进行验证,检测结果与标准参考值相符。结论该方法快捷、高效,灵敏度、准确度高,适用于人发中汞含量的检测。     

血液中Cr、Cd、As、Tl和Pb的电感耦合等离子体质谱分析

目的 建立血液中Cr、Cd、As、Tl和Pb的电感耦合等离子体质谱(ICP-MS)分析方法. 方法血液采用微波消解仪进行处理,以115In元素作内标,使用ICP-MS方法对血液中Cr、Cd、As、Tl和Pb进行分析.结果 方法检出限为0.00001～0.00249μg/L,准确度为90.1%～110.7%,精密度为4.0%～7.9%. 结论建立的方法准确、快速、线性范围宽、灵敏度高,适用于Cr、Cd、As、Tl和Pb中毒案件的检测.     

玻璃中痕量金属元素检测方法研究

目的建立玻璃中金属元素的快速检测方法。方法采用高温消解法对样品进行预处理,用电感耦合等离子体发射光谱仪同时对多种金属元素进行检测,同时对方法的精密度和准确度进行了测定。结果采用氢氟酸对样品进行预处理,各元素同时测定的发射光谱图相互无干扰。在所设定的条件下,各种元素的回收率均〉75％,相对标准偏差均〈10％。结论玻璃中金属元素可以通过高温消解进行预处理,应用电感耦合等离子体发射光谱仪同时进行检测。     

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.     

应用等离子发射光谱分析技术测定人体组织中的汞含量

汞中毒案件的传统分析是将洁净的铜片或铜丝放入酸性检材试料中煮沸,如表面被一层银灰色沉积物所覆盖,则可以证实检材中含有汞。也可做汞的升华实验来确定汞的存在。用原子吸收光谱仪、原子发射光谱仪、扫描电子显微镜、离子色谱法等分析技术来确定汞的存在与定量,检材需要一定的前处理,有些只能进行半定量分析。本文在改进湿法消化人体生物组织样品(肝、肾)方法的同时,应用等离子体发射光谱分析技术测定人体组织中的汞含量,此法具有可靠、准确、简便、快速、抗干扰性强等特点,同时还可对多种有毒金属元素进行定性、定量。     

从一起汞中毒事故谈乡镇企业劳动卫生监督与服务

某镇办金矿于1993年1月开工,该矿采用"土法练金",即用金属汞吸附矿砂中的金,然后放在炉火上烧炼,使汞蒸发而得金、在开工不到一个月的时间里,该矿就有十余人出现急性中毒症状,其中严重的一人,中毒约两个月后因肝、肾、脑多脏器损害而死亡,为此,我们对事故现场进行了劳动卫生学调查,调查中我们了解     

激光剥蚀电感耦合等离子体质谱技术检测车辆油漆金属元素

目的建立车辆油漆的激光剥蚀电感耦合等离子体质谱（laser ablation inductively coupled plasma mass spectrometry,LA—ICP—MS）分析方法。方法对38种车辆油漆样品采用激光剥蚀,电感耦合等离子体质谱进行测定,通过各油漆样品本含有金属元素种类和金属元素响应相对比值的差异对油漆样品进行区分。结果38种样品中有30种可直接依据所含金属元素种类的差异进行对其进行区分,其余8种依据元素间响应值比值的差异进行区分,方法重现性良好,精密度（RSD）小于10％。结论所建立的LA—ICP—MS方法简便快速、精密度良好、对样品微损,适用于法庭科学对车辆油漆的检测。     

ICP/MS定量检测人体组织铊含量1例

铊（Thallium,Tl）为银白色金属,原子量204.38,易溶于水,其化合物对人体有毒。硫酸铊最小致死量为15.8mg/kg。铊定量检验方法较多,如原子吸收光谱法,溶出伏安法。本文采用电感耦合等离子体发射光谱/质谱仪法（ICP/MS）,使用样品量少,结果准确。     

血、尿中金属毒物的电感耦合等离子发射光谱检测方法

目的建立血和尿中的有毒金属元素快速检测方法。方法通过模拟样品,采用微波消解炉对样品进行预处理,用电感耦合等离子发射光谱仪同时对多种可疑有毒金属元素进行检测。结果血、尿样品经消解或酸稀释处理,镉、钴、铬、铜、镍等元素可检测方法平均回收率范围为75.5%～127.5%,变异系数小于16.4%结论在中毒剂量,对肝脏和肾脏组织中的可疑有毒金属元素,可以采用电感耦合等离子发射光谱仪同时进行检测。     

化妆品汞超标致人身损害法医临床鉴定分析

随着经济的发展及人们法律意识的增强，因不合格化妆品导致汞中毒的人身损害民事和刑事案例呈逐年增多的趋势，此类损伤的人体损伤程度及其因果关系的分析已成为司法鉴定中新的重点及难点。通过对7例经由化妆品汞含量超标导致人体损伤的案件进行回顾性分析，结合被鉴定人接触含汞化妆品后的发病时间、临床表现以及生化检验结果，对以化妆品涂抹面部方式所导致的汞中毒进行逐一研究。结果发现，受害人均为（37±5）岁的中年女性，中毒后发病时间不等，均出现以肾毒性为主的临床表现，且尿液及血液中的有形成分均为异常，其中兼有神经系统症状者占71.4%，经明确诊断并行规律的驱汞治疗后预后良好。通过总结化妆品汞超标导致汞中毒后人体受损的主要器官、临床特征及此类案件法医临床鉴定分析的着重点，以期为此类案件的法医临床鉴定分析提供一定的经验及思路。     

GC-MS determination of gamma-hydroxybutyric acid (GHB) in blood

A fast and efficient procedure has been developed for the analysis of total mercury in human tissues and blood using a hydride vapor generator system coupled to an atomic absorption spectrometer (HVG-AA). Tissue and blood samples were digested in a pressurized microwave decomposition system and the digest diluted prior to formation of free mercury vapor and analysis by atomic absorption. Recovery studies performed on 10 spiked/unspiked pairs of human liver and on 10 spiked/unspiked pairs of human blood samples yielded average recoveries of 99.7% (CV=0.4%) and 101.2% (CV=0.5%), respectively. The method detection limit for liver and blood was 50 microg Hg/kg and 12.5 microg Hg/l, respectively. The "normal" concentrations of mercury in human liver and blood are 33-490 microg Hg/kg and 0.6-59 microg Hg/l, respectively [1]. This method is able to determine mercury poisoning levels and may also be applied to detect mercury near the lower levels of these "normal" ranges, using the standard addition method approach.     

A fatal case of mercuric cyanide poisoning

A 57-year-old pharmacist was found dead 11 days after his disappearance. At the autopsy, samples of blood, urine, gastric content were obtained. Presence of ethanol, cyanide and mercury were detected in some samples. Cyanide and mercury were identified and quantified using high-performance liquid chromatography with diode array detector (HPLC) in fluorescence mode and ICP with mass selective detector (ICP-MS) respectively. Whole blood concentrations of ethanol was 1.72 g/L. Cyanide and mercury concentrations in whole blood were respectively 0.16 and 3.8 mg/L. Concentrations of cyanide (27 mg/L) and mercury (150 mg/L) in gastric contents prove a massive oral ingestion of mercuric cyanide or mercuric oxycyanide occurred. In this case report, the death was attributed to the combined toxicity of cyanide and mercury.     

Accidental potassium dichromate poisoning. Toxicokinetics of chromium by ICP-MS-CRC in biological fluids and in hair

Intoxications by chromium (Cr) compounds are very life threatening and often lethal. After oral ingestion of 2 or 3g of hexavalent Cr (Cr(VI)), gastrointestinal injury, but also hepatic and renal failure, often occurs which each leads to a fatal outcome in most patients. Cellular toxicity is associated with mitochondrial and lysosomal injury by biologically Cr(VI) reactive intermediates and reactive oxygen species. After Cr(VI) has been absorbed, there is not much that can be done except to control the main complications as the treatment is only symptomatic. The biotransformation of Cr(VI) to Cr(III) reduces the toxicity because the trivalent form does not cross cellular membranes as rapidly. In fact, more than 80% of Cr(VI) is cleared in urine as Cr(III). We report the case of a 58-year-old male patient who was admitted to hospital after accidental oral ingestion of a 30 g/L potassium dichromate (the estimated amount of ingested Cr is about 3g). ICP-MS equipped with a collision/reaction cell (CRC) and validated methods were used to monitor plasma (P), red blood cells (RBCs), urine (U) and hair chromium. For urine the results were expressed per gram of creatinine. After 7 days in the intensive care unit, the patient was discharged without renal or liver failure. P, RBC and U were monitored during 49 days. During this period Cr decreased respectively from 2088 μg/L to 5 μg/L, 631 μg/L to 129 μg/L and 3512 μg/g to 10 μg/g. The half-life was much shorter in P than in RBC as the poison was more quickly cleared from the P than from the RBC, suggesting a cellular trapping of the metal. Hair was collected 2 months after the intoxication. We report a very rare case of survival after accidental Cr poisoning which has an extremely poor prognosis and usually leads to rapid death. For the first time, this toxicokinetic study highlights a sequestration of chromium in the RBC and probably in all the cells.     

A Rare Case of Poisoning with a Volatile Substance: Quantitative Determination of n‐Butane in Postmortem Tissue

Poisoning with volatile substances remains exceptional. Authors report the case of a married couple who were found in a car with a butane gas bottle: the woman was dead and her husband alleged it was an unsuccessful suicide pact. A specific research of volatile substances on postmortem samples with headspace gas chromatography–mass spectrometry following a quantitative determination was performed. The n‐butane concentrations detected were composed of 610 μg/L (cardiac blood), 50 μg/kg (brain), 134 μg/kg (lungs), 285 μg/kg (liver), and 4090 μg/kg (heart) and were compatible with the rare lethal concentrations evoked in the literature. The cause of death was determined to be asphyxiation through n‐butane criminal poisoning. Authors recommendation therefore is to take samples immediately and place them in properly sealed containers and hence analyzing the samples as soon as possible after collecting them or storing them under ?30°C (?22°F) if analyses cannot be performed immediately.     

Smoking trials with mercury contaminated cigarettes. Studies of attempted poisoning]

In the context with an attempted poisoning it was investigated, to which extent an intoxication can be caused by smoking cigarettes, which contain elementary mercury. With a smoking apparatus the effect of the amount (9 mg to 1.4 g) and of the distribution of the Hg within the cigarette on its concentration in the mainstream and sidestream smoke as well as in the ash and the filter was analytically determined. It follows from these experiments, that at a good distribution almost independently of the amount involved only up to 2 mg Hg per cigarette are inhalated with the mainstream smoke, whereas up to 97% are found in the sidestream smoke. In the ash and the filter only small amounts are detected. By comparison with cases described in literature it is shown, that a poisoning by such cigarettes is possible only after frequent smoking or by passive smoking via the sidestream smoke in small and badly aerated rooms.     

高效液相色谱法测定人血液、尿液中的2,4-D丁酯

目的建立检测血液、尿液中2,4-D丁酯的高效液相色谱分析方法。方法采用正己烷为样品萃取溶剂,色谱柱为Zorbax SB-Aq柱,流动相为V（甲醇）∶V（水）=60∶40。结果 2,4-D丁酯在血液和尿液中的线性范围分别为0.10～10.00μg/mL（r≥0.999 8）和0.08～8.00μg/mL（r≥0.999 5）,检测限分别为0.002 0μg/mL和0.001 8μg/mL,准确度为94.5%～104.5%,日内、日间精密度≤4.5%。结论本研究建立的血液、尿液中2,4-D丁酯的提取和HPLC检测方法,可应用于2,4-D丁酯中毒的快速检验和中毒死亡的法医学鉴定。     

电热板消解电感耦合等离子体质谱法测定人发中33种无机元素的含量

目的建立头发中33种无机元素的电热板消解电感耦合等离子体质谱（inductivelycoupledplas—ma—IllasssDectrometry,ICP—MS）测定方法。方法以锂（6Li）、锗（^72Ge）、钇（^89Y）、铟（^115In）、铽（^159yb）作内标,硝酸和过氧化氢作为消解酸体系．采用电热板消解对头发进行前处理,ICP—MS法分析人发中33种无机元素的含量。结果电热板消解ICP—MS法的检出限为0．0001μg／g（Th）-10．9μg／g（Ca）,定量限为O．0005μg／g（Th）～25μg／g（Ca）,加标回收率为86％～113％,日内及日间精密度≤9.2％,与微波消解法检测结果相比,差异无统计学意义。结论电热板消解ICP—MS法高效、准确度高,适用于对头发中33种无机元素的分析。     

Fatal Intoxication with Toluene Due to Inhalation of Glue

Two cases of fatal intoxications with toluene due to glue sniffing are described. In case 1, the autopsy did not indicate cause of death, while in case 2, the cause of death was determined to possibly be due to mechanical asphyxia by drowning. As the decedents had a history of glue sniffing, toxicological analyses were performed. Using gas chromatography with flame ionization detector and gas chromatography/mass spectrometry (GC/MS) with headspace method, toluene was detected in biological samples. Toluene ranged from 3.81 to 20.97 μg/g, with the highest concentrations observed in liver and brain (13.82–20.97 μg/g) in both cases. Based upon this data, the cause of death in both cases was determined to be toluene poisoning. Toxicological investigations are extremely important and should be considered mandatory in all deaths thought to be due to volatile substance abuse, as well as all deaths that are thought to be due to poisoning in young people.     

Application of dispersive liquid-liquid microextraction and CE with UV detection for the chiral separation and determination of the multiple illicit drugs on forensic samples

A new method was developed for pre-concentration, chiral separation and determination of multiple illicit drugs on forensic samples using dispersive liquid-liquid microextraction (DLLME) and capillary electrophoresis (CE) with Ultra Violet (UV) detection. The method was based on the formation of tiny droplets of an organic extractant in the prepared sample solution using water-immiscible organic solvent (chloroform) dissolved in water-miscible organic dispersive solvent (isopropyl alcohol). The organic phase, which extracted heroin, DL-methamphetamine, DL-3, 4-methylenedioxymethamphetamine and dl-ketamine from the prepared sample solution, was separated by centrifuging. The sedimented phase was transferred into a small volume CE auto-sampler vial with 10 μL of 1% HCl methanol solution and evaporated to dryness. The residue was reconstituted in lidocaine hydrochloride aqueous solution (internal standard) and introduced by electrokinetic injection into CE. Parameters affecting extraction efficiency were investigated and optimized. Under optimum conditions, linearity of the method was 0.15-6500 μg/L for all target analytes. The LODs (S/N=3) were 0.05-0.20 μg/L. Excellent repeatability (RSD ≤ 4.4%, n=5) was achieved. The feasibility of this method was demonstrated by analyzing spiked forensic samples. To our knowledge, it is the first time to combine DLLME with CE for chiral separation and determining illicit drugs on forensic samples.