Blood carbofuran concentrations in suicidal ingestion cases

We describe four fatal cases due to ingestion of carbofuran, a carbamate insecticide. Carbofuran was detected in the gastric contents using thin layer chromatography (TLC) and gas chromatography/mass spectrophotometry (GC/MS), and quantified in the blood using a gas chromatograph equipped with nitrogen-phosphorus detector (NPD). Fatal concentrations of carbofuran in blood ranged from 0.32 to 11.6 microg/ml.     

静松灵的检验

本实验建立了用固相萃取(SPE)、薄层色谱和气—质联用法(GC-MS)分析血、尿、肝中静松灵的方法,在1g尿、血、肝中添加0.01mg药物、回收率分别为96.1%、90%、67%.该方法简单快速准确,经动物实验及案件鉴定验证,效果较好.     

离子交换柱法萃取血样中4种巴比妥类药物

目的建立血样中4种常见巴比妥类药物的固相萃取方法。方法采用Oasis MAX固相萃取柱对样品进行预处理,以2%氨水淋洗2,%甲酸-甲醇洗脱,GC/NPD定量检验,GC/MS定性检验。结果血样中4种常见巴比妥类药物平均萃取回收率达80%以上,以信噪比10/1计,最小定量限为1～2μg/mL,以信噪比3/1计,检出限为0.5～1μg/mL,在1～50μg/mL范围内,线性相关系数均在0.99以上。结论本文固相萃取方法检出限低,回收率高,选择性强,可应用于血样中4种常见巴比妥类药物的检测。     

A fatality involving U4Euh, a cyclic derivative of phenylpropanolamine

A fatality following ingestion of diazepam and 4,5-dihydro-4-methyl-5-phenyl-2-oxazolamine, a cyclic derivative of phenylpropanolamine known as U4EuH or 4-methyl aminorex, is described. Solid dosage samples of U4EuH were analyzed using gas chromatography, ultraviolet and infrared spectroscopy, nuclear magnetic resonance, and mass spectrometry. Physiological fluids were analyzed quantitatively by gas chromatography and qualitatively by gas chromatography-mass spectrometry. Concentrations of 4,5-dihydro-4-methyl-5-phenyl-2-oxazolamine were: in blood 21.3 mg/L; in urine 12.3 mg/L. Diazepam concentration in blood was 0.8 mg/L.     

Sudden death caused by 1,1-difluoroethane inhalation

A 20-year-old man was found dead on the floor next to a computer, with a nearly full can of "CRC Duster" dust remover located next to the deceased on the floor, and an empty can of the same product on the computer desk. Toxicologic evaluation using either gas chromatography/mass spectrometry (GC/MS) or gas chromatography/flame ionization detector (GC/FID) method identified the active ingredient 1,1-difluoroethane (Freon 152a) in all tissues analyzed. Tissue distribution studies revealed highest concentration in central blood, lung, and liver. It is believed that the 1,1-difluoroethane inhalation was the cause of death.     

Intratracheal gas analysis for volatile substances by gas chromatography/mass spectrometry--application to forensic autopsies

Intratracheal gas analysis was carried out by gas chromatography/mass spectrometry (GC/MS) in 20 burned body cases (13 males and 7 females). Volatile aromatic and aliphatic hydrocarbons were detected by GC/MS using a GS-Q column with the intratracheal gas as well as the blood in 19 cases. The characteristic patterns of mass chromatograms for gasoline, kerosene (gas oil), and liquid petroleum gas could be differentiated from each other using the intratracheal gas. The burned body in one case showed no presence of volatile substances in the intratracheal gas, nor intratracheal soot, although high concentrations (1 microg/g and more) of volatile substances were detected on the clothes. The victim also had normal CO-Hb concentrations (0.1 to 0.2%) in the heart blood. The results of intratracheal gas analysis were consistent with signs of the vital reaction. In conclusion, intratracheal gas analysis provides a supportive method for diagnosing the cause of death in burned bodies, and yields for at least 48 hours valuable information on volatile hydrocarbons (being detected in deliberate or accidental fire cases) to which the body had been exposed just before death.     

直接进样气相色谱法测定全血中乙醇的含量

目的建立一种直接进样气相色谱法检测全血中的乙醇。方法全血经硫酸铝钾沉淀蛋白,加入内标异丙醇后,用直接进样气相色谱法进行检测,FID为检测器,用保留时间定性,内标标准曲线法定量。结果该方法线性范围为0.2-1.4mg/m L,相关系数R=0.999 3,总分析时间不超过5min,最低检测限为0.01mg/m L,相对标准偏差（RSD）〈5%,平均回收率为92.3%;所建立的方法与顶空气相色谱（HS-GC）法比较相对偏差（RD）〈10%。结论该方法可用于全血中乙醇的检测。     

Detection of low levels of flunitrazepam and its metabolites in blood and bloodstains.

Detection of low levels of flunitrazepam and its metabolites was developed using solid-phase extraction to isolate the drugs from whole liquid blood and dried bloodstains, with subsequent derivatization with pentafluoropropionic anhydride (PFPA) followed by N-(tert-butyldimethyl-silyl)-N-methyl-trifluoroacetamide (MTBSTFA) with 1% TBDMSCI. Analysis was confirmed by gas chromatography/mass spectroscopy using select ion monitoring (sim) in electron impact mode. The limit of detection of this procedure using 1 ml of blood was determined to be 0.1 microgram/dl.     

气相色谱-串联质谱法分析尿和血中除草剂百草枯

目的建立尿和血中百草枯的离子交换固相萃取-气相色谱-串联质谱分析方法。方法尿样加内标乙基百草枯,用732阳离子交换树脂提取;血样加内标乙基百草枯,用三氯乙酸凝聚蛋白质后取上清液用732阳离子交换树脂提取。提取物用硼氢化钠在水溶液中碱性条件下还原,还原物用有机溶剂提取进行气相色谱-串联质谱法分析。结果尿和血中百草枯的提取率分别为76％和74％,检测限分别为2ng／mL和10ng／mL,尿添加百草枯100ng／mL和血添加百草枯500ng／mL水平的回收率分别为99．6±5．6％和99．3±7．6％（Mean±CV）。结论本文建立的分析方法灵敏度高,能够满足中毒致死案件检验及临床毒物检验的需要。     

A fatality involving clomipramine

A fatality following ingestion of the tricyclic antidepressant clomipramine (Anafranil), alprazolam (Xanax), and ethyl alcohol is described. Clomipramine and N-desmethylclomipramine were quantitated by high performance liquid chromatography and alprazolam by gas liquid chromatography. Concentrations of clomipramine and N-desmethylclomipramine were: in blood--0.84 and 1.4 mg/L; in urine--0.56 and 0.62 mg/L. Alprazolam concentration in blood was 0.069 mg/L. Ethyl alcohol was measured by headspace gas chromatography and found to be 375, 385, and 435 mg/dL in blood, urine, and vitreous humor, respectively. These findings are compared to previous reports of clomipramine related fatalities and alprazolam toxicity combined with ethyl alcohol.     

The analysis of an intracerebral hematoma for drugs of abuse

Toxicological investigations were performed on an intracerebral hematoma, antemortem blood, and postmortem blood of an individual who was found unresponsive in his home. The hematoma was found to have ethanol at a concentration of 0.05% (w/v), and benzoylecgonine (a cocaine metabolite) was also confirmed at a concentration of 0.43 mg/L by specific analysis using gas chromatography/mass spectrometry (GC/MS). These results enabled the pathologist to record the cause of death as intracerebral hemorrhage due to acute cocaine intoxication.     

A reported case involving impaired driving following self-administration of xylazine

A case of suspected drug-impaired driving involving self-administration of xylazine (Xyla-Ject), a veterinary tranquilizing agent, and paroxetine is presented. Qualitative and quantitative analysis of xylazine and paroxetine were performed by gas chromatography with a flame-ionization detector (GC-FID) and gas chromatography/mass spectrometry (GC/MS). Whole blood xylazine and paroxetine concentrations were 0.57 and 0.02 microg/ml, respectively.     

固相萃取-气相色谱法提取全血中的外源性褪黑素

目的建立血样中褪黑素的固相萃取方法。方法采用OasisHLB固相萃取柱提取,GC/NPD定量检验,GC/MS定性检验。结果血样中褪黑素平均萃取回收率达80%以上,最低检出限0.02μg/mL,线性良好,相关系数R2=0.9978。结论该方法操作简便快速,提取回收率高,重现性好,提取物干净,可用于实际案件当中。     

A simple, rapid and simultaneous analysis of complex volatile hydrocarbon mixtures in blood using gas chromatography/mass spectrometry with a wide-bore capillary column

A screening method for detecting volatile hydrocarbons in blood has been developed using gas chromatography/mass spectrometry with a wide-bore capillary column and a headspace method. Toluene-d8 and indan were used as the internal standards for quantitative analysis. Hydrocarbons with retention indices from 600 to 1200 were simultaneously and quantitatively detected in relatively low concentrations (0.01 microgram/ml) in reconstructed ion chromatography. This method could prove useful in forensic cases in which urgent examination of complex hydrocarbon mixtures, e.g. petroleum components, is required.     

Detection of morphine and codeine in blood samples with gas chromatography/mass spectrometry (NCI and PCI) for differentiating codeine use from use of heroin and morphine

Morphine and codeine were isolated from blood with C18 Bond Elut columns and derivatised with pentafluoropropionic anhydride (PFPA). The PFPA-derivatives were examined by means of gas chromatography/mass spectrometry using electron impact and chemical ionisation (positive and negative mode). The negative chemical ionisation, as most sensitive, was applied for the quantitation of both examined substances in forensic blood samples.     

Fatality due to methyl acetylene-propadiene (MAPP) inhalation

A 33-year-old man died after intentionally inhaling a gaseous mix of methyl acetylene (propyne) and propadiene (allene) commonly known as MAPP, which is used for soldering and welding. He was found with a plastic bag securely placed over his head and a cylinder of MAPP alongside his head. The cylinder had been vented into the bag using a flexible hose. A comprehensive toxicological analysis revealed only a trace of diphenhydramine in the liver and 0.02 mg/L of morphine in the urine. Analysis of blood by headspace gas chromatography (HS-GC) detected two unknown peaks. These were determined to be the components of MAPP gas. MAPP was quantitated in femoral blood (59.6 mg/L) and brain (43.6 mg/kg) using a HS-GC method. The cause of death was attributed to acute MAPP intoxication, and the manner was determined to be suicide. A discussion on the analytical and interpretive considerations commonly encountered when analyzing volatile compounds is also presented.     

Automated determination of carboxyhemoglobin contents in autopsy materials using head-space gas chromatography/mass spectrometry

To establish a method for the routine analysis of carboxyhemoglobin (COHb) in autopsy materials including those which have undergone postmortem changes, e.g. thermo-coagulation, putrifaction and contamination, an automated head-space gas chromatography/mass spectrometry (GC/MS) analysis was utilized. The procedure consisted of preparation of the sample in a vial and a carbon monoxide (CO) saturated sample, for estimation of hemoglobin content, in another vial, the addition of n-octanol, potassium ferricyanide and an internal standard (t-butanol), GC separation and determination of CO using a GC/MS system equipped with an automated head-space gas sampler. The method was practical not only with the blood and bone marrow aspirates to confirm the findings on the CO-oximeter system, but also with the thermo-coagulated and putrified blood.     

Analysis of 2-hydroxyimipramine in an imipramine-related fatality

A fatality following ingestion of the tricyclic antidepressant imipramine (Novopramine), acetaminophen, and ethyl alcohol is described. Imipramine, desipramine, acetaminophen, and 2-hydroxyimipramine were quantitated by high performance liquid chromatography, and ethyl alcohol by gas liquid chromatography. Concentrations of imipramine, desipramine, 2-hydroxyimipramine, and acetaminophen were: in blood--9.0, 1.1, 3.9, and 11 mg/L; in urine--92, 14, and 42 mg/L (acetaminophen not quantitated in urine). Ethyl alcohol concentration in blood was less than 10 mg/dL and 105 mg/dL in the urine by headspace gas chromatography. These findings are compared to previous reports of imipramine-related fatalities. To our knowledge, this is the first fatality reported involving imipramine where analysis included quantitation of 2-hydroxyimipramine in blood and urine.     

Fatal intoxication involving 2-methyl AP-237

Novel synthetic opioids contribute considerably to the opioid epidemic, especially with the frequent emergence of structurally similar compounds. This case report describes a fatal intoxication involving 2-methyl AP-237. A 54-year-old Caucasian male was found deceased from an apparent drug overdose. A plastic container labeled “2MAP” and a cut straw were found in the decedent's backpack at the scene. A white substance found in the container tested positive for fentanyl by field testing. According to his medical history, the decedent was treated for a drug overdose 3 years prior to his death. With no diagnostic findings at autopsy, the case was submitted for toxicological analysis. An unknown substance was detected in peripheral blood and urine using gas chromatography with nitrogen phosphorous detection (GC-NPD). Further testing was conducted using gas chromatography–mass spectrometry (GC–MS) and liquid chromatography-quadrupole-time-of-flight mass spectrometry (LC-QTOF-MS) which confirmed the presence of 2-methyl AP-237 and potential metabolites in blood and urine. Quantitation by GC-NPD revealed concentrations of 2-methyl AP-237 in blood and urine at 480 ng/mL and 4200 ng/mL, respectively. The toxicological analysis also identified and quantitated alprazolam in the blood at 55 ng/mL. Additionally, the metabolism of 2-methyl AP-237 was investigated and three hydroxylated metabolites were identified in peripheral blood and urine. Limited literature is available for the detection and quantitation of 2-methyl AP-237 in postmortem specimens. Given the toxicological findings with unremarkable autopsy findings, this case is an example of a fatal intoxication involving 2-methyl AP-237.     

A fatality involving secobarbital, nitrazepam, and codeine

A fatal case involving the suicidal ingestion of secobarbital, nitrazepam, and codeine is presented. The drugs were quantified using gas chromatography for codeine and high-performance liquid chromatography for the two other drugs. The blood concentrations of secobarbital, nitrazepam, and codeine were found to be 11.48, 1.72, and 0.036 microgram/ml, respectively. Results are discussed in the light of the existing literature.