Fatal intoxication with 1,4-butanediol: Case report and comprehensive review of the literature

A fatal case of 1,4-butanediol (1,4-BD) oral ingestion is reported here, in which a 51-year-old man was found dead in his bed. According to the police report, the deceased was a known drug user. A glass bottle labeled (and later confirmed to be) “Butandiol 1,4” (1,4-BD) was found in the kitchen. Furthermore, the deceased's friend stated that he consumed 1,4-BD on a regular basis. The autopsy and histological examination of postmortem parenchymatous organ specimens did not revealed a clear cause of death. Chemical-toxicological investigations revealed gammahydroxybutyrat (GHB) in body fluids and tissues in the following quantities: femoral blood 390 mg/L, heart blood 420 mg/L, cerebrospinal fluid 420 mg/L, vitreous humor 640 mg/L, urine 1600 mg/L, and head hair 26.7 ng/mg. In addition, 1,4-BD was qualitatively detected in the head hair, urine, stomach contents, and the bottle. No other substances, including alcohol, were detected at pharmacologically relevant concentrations. 1,4-BD is known as precursor substance that is converted in vivo into GHB. In the synoptic assessment of toxicological findings, the police investigations and having excluded other causes of death, a lethal GHB-intoxication following ingestion of 1,4-BD, can be assumed in this case. Fatal intoxications with 1,4-BD have seldom been reported due to a very rapid conversion to GHB and, among other things, non-specific symptoms after ingestion. This case report aims to give an overview to the published of fatal 1,4-BD-intoxications and to discuss the problems associated with detection of 1,4-BD in (postmortem) specimens.     

Evaluation of portable gas chromatography–mass spectrometry (GC–MS) for the analysis of fentanyl,fentanyl analogs,and other synthetic opioids

Potent synthetic opioids including fentanyl and its analogs are frequently encountered in the field and require detection and identification by first responders to maintain the safety of drug abusers, first responders, health-care providers, and the public at large. Due to the low concentration at which these substances may be encountered and the complicating matrices within which they may be dispersed, the use of portable gas chromatography–mass spectrometry (GC–MS) for their identification in the field offers great potential value. This research established that portable GC–MS is a useful method for the detection and identification of a large number of synthetic opioids, especially fentanyl and its analogs. In this study, 250 synthetic opioids and related substances including 210 fentanyl analogs were analyzed using portable GC–MS. It was concluded that 225 of the 250 (90.0%) opioids analyzed were successfully detected onboard at the time of analysis and identified as either the substance (55.2%) or an analog (34.8%). These outcomes have equivalent benefit for the field analysis of illicit drugs due to both initiating the same subsequent actions by first responders.     

GC/MS检验不同案件中摇头丸

目的 分析不同案件缴获的“摇头丸”主要成分和添加物,为确定“摇头丸”的合成路线、非法来源提供依据.方法 以GC/MS检测法为主要检测方法.结果 检验的14个“摇头丸”主要成分为甲基苯丙胺和咖啡因,其中含有少量的其他杂质如麻黄碱和氯胺酮等.结论 检测的14个“摇头丸”样本其中12个含甲基苯丙胺,实为冰毒成分,1个为咖啡因均不属于摇头丸.     

HS-SPME-GC/MS法检测尿液及毛发中苯丙胺类毒品

目的采用顶空固相微萃取（HS-SPME）、GC/MS分析方法,对生物样品中苯丙胺（AM）、甲基苯丙胺（MAM）、3,4-亚甲二氧基苯丙胺（MDA）和3,4-亚甲二氧基甲基苯丙胺（MDMA）4种苯丙胺类毒品进行定性定量分析。方法在碱性和饱和盐处理状态下,采用100μm聚二甲基硅氧烷（PDMS）萃取纤维,于顶空瓶中进行生物样品AM、MAM、MDA、MDMA 4种毒品萃取,以2-甲基苯乙胺为内标,经气-质联用选择离子检测（GC/MS/SIM）模式进行定性定量分析。对HS-SPME条件优化,对方法的精密度、准确度和检出限进行测定。结果 AM、MAM、MDA、MDMA 4种毒品尿液中的最低检出限为5ng/mL,毛发中的最低检出限为0.5ng/mg。尿液中线性关系范围为0.05μg/mL~5μg/mL,r〉0.991,回收率为82%~108%,RSD为2.6%~6.1%（n=5）;毛发中线性关系范围为5ng/mg~500ng/mg,r〉0.992,回收率为80%~113%,RSD（%）为1.4%~6.8%（n=5）。结论 HS-SPME-GC/MS各项定量参数符合分析要求。该方法简单、灵活、经济、快速、无溶剂,适用于生物检材中该类毒品的分析。     

血液中64种常见有机氯菊酯类农药的快速筛查

目的建立人体血浆中64种有机氯菊酯类农药多残留的气相色谱（GC）快速筛查分析方法。方法空白人体静脉抗凝血用乙腈沉淀蛋白,乙酸乙酯∶环己烷（v/v,3∶1）进行液液萃取净化,使用HP-5色谱柱,采用气相色谱进行定性、定量分析。对方法进行优化并进行方法学评价。结果 64种农药在0.001~0.1μg/mL范围内线性关系均良好,相关系数在0.990 1~0.999 9之间。检出限在0.001~0.15μg/mL范围内,方法定量限在0.001~0.5μg/mL之间,回收率总体于80%~110%之间,相对标准偏差小于15%,方法检出限总体于0.01μg/mL以下,日内精密度在1.5%~11.5%之间,日间精密度在2.9%~13.9%之间。结论本文建立的人体血浆的农药多残留快速筛查测定法,符合农药残留分析方法的要求,可在相关研究和实践中选用。     

新型香草香料“K3”的GC／MS解析

目的对新型香草香料“K3”的主要化合物成分进行解析,为相关研究和应用提供参考。方法采用GC／MS方法,对新型香草香料“K3”样本进行检测,根据“K2”的主成分推断“K3”样本中检出的2种主要化合物成分的性质,并对其碎片离子图进行解析。结果初步推断香料“K3”中的化合物1为苯环上的2个氢被2个（-OCH3）基训取代的苯乙酰吲哚类化合物,分子式为C23H27NO3,分子量为365;化合物2为AM-2201（F代JWH-18）,分子式为C24HzzFNO,分子量为359。结论新型香草香料“K3”中含有合成大麻素类成分,该类药物应引起相关部门的重视。     

自动顶空GC/MS测定血液中乙醇含量不确定度评定

目的评定自动顶空—气相色谱—质谱法(GC/MS)测定血液中乙醇含量的不确定度。方法从分析测量过程着手,依据不确定度评定的指导性文件,分析了不确定度来源,量化不确定度分量,计算检测结果的合成标准不确定度和扩展不确定度。结果血液样本两次测定结果平均值为0.738mg/mL的扩展不确定度为0.084mg/mL。结论血液中乙醇含量的不确定度主要来源于样品检测、乙醇标准溶液和标准曲线。     

Extraction and isolation of cannabinoids from marijuana seizures and characterization by 1H NMR allied to chemometric tools

Marijuana, a drug derived from the Cannabis sativa L. plant, is the world's most consumed illicit drug. In this paper, a total of 156 marijuana samples seized in the state of Espírito Santo (ES), Brazil were studied and analysed by proton nuclear magnetic resonance (¹H NMR) spectroscopy to identify the major cannabinoids present. A crude extract of all samples was purified using high performance liquid chromatography so that these compounds could serve as reference substances. Nine fractions were obtained and analysed by ¹H NMR and gas chromatography–mass spectrometry (GC–MS), with five presented cannabinoids. ?⁹-THC (Δ⁹-trans-tetrahydrocannabinol), ?⁹-THCA (?⁹-tetrahydrocannabinolic acid), ?⁸-THC (?⁸-tetrahydrocannabinol), 11-hydroxycannabinol, CBV (cannabivarin), and CBN (cannabinol) were found, and their chemical structures were confirmed by GC–MS. The latter compound was obtained with high purity (≈100%), while the others were obtained as less complex mixtures with purity higher than 75% (except for Δ⁸-THC). Principal component analysis (PCA) was used on the ¹H NMR spectra of the 156 samples, and it was found that the samples were grouped according to the months, differentiating into two groups (from July 2014 to January 2015 and from February 2015 to July 2015), where non-grouping was observed from four macro-regions of the ES state (North, Central, Metropolitan, and South). The chemical profile of the seized samples was correlated to the ¹H NMR spectrum of an isolated CBN sub-fraction, in which the group formed by samples seized in the year 2015 presented lower CBN content in the chemical composition. From the PCA score plot, two groups of samples were confirmed using the partial least squares discriminant analysis and orthogonal projections to latent structures classification methods.     

A method for the rapid detection of the zopiclone degradation product 2-amino-5-chloropyridine

Zopiclone (Zimovane) is a cyclopyrrolone compound which exhibits hypnotic and sedative effects while also exhibiting anticonvulsant and muscle relaxant activities. The detection and quantification of zopiclone is difficult. It has a high molecular weight compared to most other commonly used drugs, therapeutic levels are not high, and it is unstable in nucleophilic solvents. A degradation product of zopiclone, 2-amino-5-chloropyridine (ACP) together with a method for its detection using high-performance liquid chromatography with diode array detection has been described previously. An account is presented of a simple method for the detection of ACP using gas chromatography with mass selective detection (GC/MS) which will facilitate detection of zopiclone use as part of a routine screen.     

Testing human hair for cannabis

To validate information on cannabis use, we investigated human hair and pubic hair for cannabinoids (THC and THC-COOH) by gas chromatography/mass spectrometry. Samples (100 mg approximately) were decontaminated with methylene chloride, then pulverized and dissolved in 1 ml 1 N NaOH for 10 min at 95 °C in the presence of 200 ng of deuterated standards. After cooling, samples were extracted by n-hexane/ethyl acetate after acidification with acetic acid. After derivatization of the dry extract by PFPA/PFP-OH, the drugs were separated on a 30-m capillary column and detected using selected-ion monitoring (m/z 377 and 459 for THC and THC-COOH, respectively). Forty-three hair samples were obtained from fatal heroin overdose cases. Among them, 35% tested positive for cannabinoids. Hair concentrations ranged from 0.26 to 2.17 ng/mg (mean, 0.74 ng/mg) and 0.07 to 0.33 ng/mg (mean, 0.16 ng/mg) of THC and THC-COOH, respectively. As is generally the case for other drugs detected in hair, metabolite concentration was always lower when compared to the parent drug concentration. In pubic hair, THC concentrations ranged from 0.34 to 3.91 ng/mg (mean, 1.35 ng/mg) and THC-COOH concentrations from 0.07 to 0.83 ng/mg (mean, 0.28 ng/mg). In most cases, the highest cannabinoid concentration was found in pubic hair, suggesting that this sample may be the more suitable for cannabis testing.