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Recent advances in electrochemical detection of common azo dyes. 常见偶氮染料电化学检测的最新进展。
IF 2.8 4区 医学 Q2 TOXICOLOGY Pub Date : 2024-08-02 DOI: 10.1007/s11419-024-00696-y
Sumi Sundaresan, Vijendran Vijaikanth

Purpose: Food forensics is an emerging field and the initial part of this review showcases the toxic effects and the instrumental methods applied for the detection of the most commonly used azo dyes. Electrochemical detection has a lot of advantages and hence the significance of the most important techniques used in the electrochemical detection is discussed. The major part of this review highlights the surface modified electrodes, utilized for the detection of the most important azo dyes to achieve low detection limit (LOD).

Methods: A thorough literature study was conducted using scopus, science direct and other scientific databases using specific keywords such as toxic azo dyes, electrochemical detection, modified electrodes, LOD etc. The recent references in this field have been included.

Results: From the published literature, it is observed that with the growing interests in the field of electrochemical techniques, a lot of importance have been given in the area of modifying the working electrodes. The results unambiguously show that the modified electrodes outperform bare electrodes and offer a lower LOD value.

Conclusion: According to the literature reports it can be concluded that, compared to other detection methods, electrochemical techniques are much dependable and reproducible. The fabrication of the electrode material with the appropriate modifications is the main factor that influences the sensitivity. Electrochemical sensors can be designed to be more sensitive, more reliable, and less expensive. These sensors can be effectively used by toxicologists to detect trace amounts of harmful dyes in food samples.

目的:食品取证是一个新兴领域,本综述的第一部分展示了最常用偶氮染料的毒性作用和用于检测的仪器方法。电化学检测具有很多优势,因此本综述讨论了电化学检测中使用的最重要技术的意义。本综述的主要部分强调了表面修饰电极,用于检测最重要的偶氮染料,以实现低检测限(LOD):方法:利用 scopus、science direct 和其他科学数据库,使用有毒偶氮染料、电化学检测、改性电极、LOD 等特定关键词进行了全面的文献研究。结果:从已发表的文献中可以看出,随着人们对电化学技术领域的兴趣日益浓厚,人们对工作电极的改性给予了高度重视。结果明确显示,改性电极的性能优于裸电极,且 LOD 值更低:根据文献报告可以得出结论,与其他检测方法相比,电化学技术具有更高的可靠性和可重复性。对电极材料进行适当改性是影响灵敏度的主要因素。电化学传感器可以设计得更灵敏、更可靠、更便宜。毒理学家可以有效地利用这些传感器来检测食品样本中的痕量有害染料。
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引用次数: 0
Mephedrone concentrations in clinical intoxications and fatal cases: a systematic review. 临床中毒和死亡病例中的甲氧麻黄酮浓度:系统综述。
IF 2.8 4区 医学 Q2 TOXICOLOGY Pub Date : 2024-07-20 DOI: 10.1007/s11419-024-00693-1
Yu-Kai Chen, Chia-Pang Shih, Chien-Ho Wang, Chih-Chuan Lin

Background/purpose: Mephedrone, a ring-substituted synthetic cathinone derivative, gained popularity as a recreational drug in the late 2000s. Reports of fatalities related to mephedrone use have emerged with varying concentrations of blood mephedrone upon forensic investigations. This study aims to evaluate the existing literature on mephedrone concentrations in instances of clinical intoxication and fatal cases.

Methods: We comprehensively searched electronic databases, including Web of Science, PubMed, Embase, and the Cochrane Library, from inception to July 26, 2023. We selected case reports or case series of mephedrone intoxication presented with individual blood mephedrone concentration. Patient demographics, clinical characteristics, blood mephedrone concentrations, and outcomes were extracted for analysis.

Results: 77 cases from 14 case reports and 6 case series were identified for review. There were 34 deaths and 43 non-fatal intoxication cases. The median patient's age was 24 years (IQR: 10), and 91.4% were male. Forty-five of the 63 cases (71.4%) were reported with alcohol or other illicit drugs detected. The median blood mephedrone concentration was 0.37 mg/L (IQR: 1.09 mg/L). Death cases were older than non-fatal cases (median = 30 vs. 22 years, p = 0.029). The median blood mephedrone concentration was higher in death cases (1.30 mg/L vs. 0.12 mg/L, p < 0.0001).

Conclusions: Blood mephedrone concentration in dead patients is approximately 11 times higher than in non-fatal cases. This finding could serve as a stepping stone to the diagnosis of concentrations in clinical poisoning cases and deaths, especially in the treatment of poisoning patients. In more extensive prospective studies, further research is necessary to establish a standardized, real-time available methodology and validate the predictive value of mephedrone concentrations in the prognostic value of mephedrone concentrations.

背景/目的:甲氧麻黄酮是一种环状取代的合成卡西酮衍生物,在 2000 年代后期作为一种娱乐性毒品而大受欢迎。与使用甲氧麻黄酮有关的死亡报告不断涌现,法医调查发现血液中的甲氧麻黄酮浓度各不相同。本研究旨在评估现有文献中有关临床中毒和死亡病例中的甲氧麻黄酮浓度:我们全面检索了从开始到 2023 年 7 月 26 日的电子数据库,包括 Web of Science、PubMed、Embase 和 Cochrane Library。我们选择了以个体血液中甲氧麻黄酮浓度为依据的甲氧麻黄酮中毒病例报告或系列病例。我们提取了患者的人口统计学特征、临床特征、血液中的甲氧麻黄酮浓度和结果进行分析:从 14 份病例报告和 6 份系列病例中确定了 77 个病例供审查。其中有 34 例死亡病例和 43 例非致命中毒病例。患者年龄中位数为 24 岁(IQR:10),91.4% 为男性。63 例中有 45 例(71.4%)在报告时检测到酒精或其他违禁药物。血液中的甲氧麻黄酮浓度中位数为 0.37 毫克/升(IQR:1.09 毫克/升)。死亡病例的年龄大于非死亡病例(中位数 = 30 岁对 22 岁,p = 0.029)。死亡病例血液中的甲氧麻黄酮浓度中位数更高(1.30 毫克/升对 0.12 毫克/升,p):死亡患者血液中的甲氧麻黄酮浓度约为非死亡病例的 11 倍。这一发现可作为诊断临床中毒病例和死亡病例浓度的垫脚石,特别是在治疗中毒患者时。在更广泛的前瞻性研究中,有必要开展进一步的研究,以建立标准化的实时可用方法,并验证甲卡西酮浓度在甲卡西酮预后价值中的预测价值。
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引用次数: 0
Chemical composition of Ecstasy tablets seized in Poland between 2005 and 2020. 2005 年至 2020 年波兰缉获的迷魂药片的化学成分。
IF 2.8 4区 医学 Q2 TOXICOLOGY Pub Date : 2024-07-17 DOI: 10.1007/s11419-024-00691-3
Bogumiła Byrska, Roman Stanaszek

Purpose: The most commonly associated substance found in Ecstasy tablets is MDMA (3,4-methylenedioxymethamphetamine). In our study, we showed how the composition of psychoactive ingredients in Ecstasy tablets seized on the drug market in Poland has changed in the years 2005-2020.

Methods: The study material consisted of nearly 20,000 single Ecstasy tablets seized by representatives of law enforcement (the police, prosecutors) from 2005 to 2020 and analysed by the Institute of Forensic Research, Krakow, Poland. The analysis of the tablets was carried out by gas chromatography-mass spectrometry (GC-MS), high-performance liquid chromatography with diode array detection (HPLC-DAD) and ultra-high-performance liquid chromatography with photodiode array detection (UHPLC-PDA).

Results: Currently, new types of MDMA tablets are introduced onto the market, available in various colours and shapes. Our study showed that tablets sold on the street as Ecstasy have variable purity and sometimes contain little or no MDMA. The mean content of MDMA in one tablet seized in 2005-2011 decreased from 90 to 50 mg. In 2013, Ecstasy tablets with a very high MDMA content (average 195 mg per tablet) appeared on the market, but in the next 2 years, the MDMA content decreased again. From 2016, the average MDMA content began to rise again, ranging from 60 to 280 mg.

Conclusion: Tablets sold as Ecstasy also contained completely different psychoactive substances, including new psychoactive substances (NPS) (found in almost 20% of all examined tablets sold as Ecstasy) belonging to different chemical groups or their dangerous combinations (i.e. phenylethylamines, piperazines, tryptamines, cathinones, arylalkylamines, arylcyclohexylamines and piperidines). Such a large variety of psychoactive substances in Ecstasy tablets is associated with a high risk for users unaware of their composition.

目的:摇头丸中最常见的相关物质是亚甲二氧基甲基苯丙胺(3,4-亚甲二氧基甲基苯丙胺)。在研究中,我们展示了 2005-2020 年间波兰毒品市场上查获的摇头丸中精神活性成分的构成变化情况:研究材料包括执法代表(警察、检察官)在 2005 年至 2020 年期间缉获的近 20,000 片摇头丸,波兰克拉科夫法医研究所对这些药片进行了分析。对这些药片的分析采用了气相色谱-质谱法(GC-MS)、高效液相色谱-二极管阵列检测法(HPLC-DAD)和超高效液相色谱-光电二极管阵列检测法(UHPLC-PDA):目前,市场上出现了各种颜色和形状的新型亚甲二氧基甲基苯丙胺片剂。我们的研究表明,在街头作为摇头丸出售的药片纯度参差不齐,有时只含有少量或根本不含摇头丸。2005-2011 年缉获的摇头丸片剂中的亚甲二氧基甲基苯丙胺平均含量从 90 毫克降至 50 毫克。2013 年,市场上出现了亚甲二氧基甲基苯丙胺含量非常高的摇头丸片剂(平均每片 195 毫克),但在接下来的两年中,亚甲二氧基甲基苯丙胺含量再次下降。从 2016 年起,摇头丸的平均含量开始回升,从 60 毫克到 280 毫克不等:作为摇头丸销售的药片还含有完全不同的精神活性物质,包括新精神活性物质(NPS)(在所有作为摇头丸销售的受检药片中发现了近 20%),这些物质属于不同的化学组或其危险组合(即苯乙胺类、哌嗪类、色胺类、卡西酮类、芳基烷基胺类、芳基环己胺类和哌啶类)。迷魂药片中的精神活性物质种类如此之多,对不了解其成分的使用者来说风险很高。
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引用次数: 0
Development of an LC-MS/MS method for the determination of five psychoactive drugs in postmortem urine by optimization of enzymatic hydrolysis of glucuronide conjugates. 通过优化葡萄糖醛酸苷共轭物的酶水解,建立测定死后尿液中五种精神活性药物的 LC-MS/MS 方法。
IF 2.8 4区 医学 Q2 TOXICOLOGY Pub Date : 2024-07-01 Epub Date: 2024-04-01 DOI: 10.1007/s11419-024-00685-1
Tomohito Matsuo, Tadashi Ogawa, Masae Iwai, Katsutoshi Kubo, Fumio Kondo, Hiroshi Seno

Purpose: Toxicological analyses of biological samples play important roles in forensic and clinical investigations. Ingested drugs are excreted in urine as conjugates with endogenous substances such as glucuronic acid; hydrolyzing these conjugates improves the determination of target drugs by liquid chromatography-tandem mass spectrometry (LC-MS/MS). In this study, we sought to improve the enzymatic hydrolysis of glucuronide conjugates of five psychoactive drugs (11-nor-9-carboxy-Δ9-tetrahydrocannabinol, oxazepam, lorazepam, temazepam, and amitriptyline).

Methods: The efficiency of enzymatic hydrolysis of glucuronide conjugates in urine was optimized by varying temperature, enzyme volume, and reaction time. The hydrolysis was performed directly on extraction columns. This analysis method using LC-MS/MS was applied to forensic autopsy samples after thorough validation.

Results: We found that the recombinant β-glucuronidase B-One® quantitatively hydrolyzed these conjugates within 3 min at room temperature directly on extraction columns. This on-column method saved time and eliminated the loss of valuable samples during transfer to the extraction column. LC-MS/MS-based calibration curves processed with this method showed good linearity, with r2 values exceeding 0.998. The intra- and inter-day accuracies and precisions of the method were 93.0-109.7% and 0.8-8.8%, respectively. The recovery efficiencies were in the range of 56.1-104.5%. Matrix effects were between 78.9 and 126.9%.

Conclusions: We have established an LC-MS/MS method for five psychoactive drugs in urine after enzymatic hydrolysis of glucuronide conjugates directly on extraction columns. The method was successfully applied to forensic autopsy samples. The established method will have broad applications, including forensic and clinical toxicological investigations.

目的:生物样本的毒理学分析在法医和临床调查中发挥着重要作用。摄入的药物会以与葡萄糖醛酸等内源性物质共轭的形式排泄到尿液中;水解这些共轭物可提高液相色谱-串联质谱法(LC-MS/MS)对目标药物的测定。在本研究中,我们试图改进五种精神活性药物(11-去甲-9-羧基-Δ9-四氢大麻酚、奥沙西泮、劳拉西泮、替马西泮和阿米替林)葡萄糖醛酸轭合物的酶水解:通过改变温度、酶量和反应时间来优化尿液中葡萄糖醛酸共轭物的酶水解效率。水解直接在提取柱上进行。经过充分验证后,将这种使用 LC-MS/MS 的分析方法应用于法医尸检样本:结果:我们发现,重组β-葡糖醛酸酶 B-One® 可在室温下直接在提取柱上 3 分钟内定量水解这些共轭物。这种柱上方法节省了时间,并避免了宝贵样品在转移到提取柱过程中的损失。用这种方法处理的基于 LC-MS/MS 的校准曲线显示出良好的线性关系,r2 值超过 0.998。该方法的日内和日间准确度和精密度分别为 93.0-109.7% 和 0.8-8.8%。回收率为 56.1-104.5%。基质效应为 78.9% 至 126.9%:我们建立了一种直接在萃取柱上酶水解尿液中葡萄糖醛酸苷结合物的 LC-MS/MS 方法。该方法已成功应用于法医尸检样本。该方法应用广泛,包括法医和临床毒理学研究。
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引用次数: 0
Intracerebral hemorrhage in methanol toxicity patients during COVID-19 pandemic: case report and review of literature. COVID-19 大流行期间甲醇中毒患者的脑内出血:病例报告和文献综述。
IF 2.8 4区 医学 Q2 TOXICOLOGY Pub Date : 2024-07-01 Epub Date: 2024-02-09 DOI: 10.1007/s11419-023-00680-y
Hosein Safari, Reza Ajudani, Mohsen Savaie, Armin Jahangiri Babadi, Pooyan Alizadeh

Purpose: The aim of this study is to examine the clinical and imaging manifestations of methanol toxicity during the COVID-19 pandemic, as well as to review existing studies on this topic. The most common cause of methanol intoxication is methanol-adulterated liquor. The primary metabolite of methanol, formic acid, is responsible for pathological changes. Symptoms typically present within 6-24 h of consumption and can include visual disturbances, acute neurological symptoms, and gastrointestinal issues. During the initial year of the COVID-19 pandemic, methanol poisoning cases increased significantly.

Methods: In this study, We present six different patients with methanol intoxication and their clinical and imaging features.

Results: In the literature review, the most common clinical presentation was loss of consciousness and obtundation and the other was vision loss. CT scan findings showed bilateral putaminal necrosis and hemorrhage in 55% of methanol toxicity patients.

Conclusion: Methanol intoxication, causing bilateral putaminal involvement and a 50% mortality rate in intracerebral hemorrhage patients, warrants urgent toxicological analysis due to potential putaminal hemorrhage.

目的:本研究旨在探讨 COVID-19 大流行期间甲醇中毒的临床和影像学表现,并回顾现有的相关研究。甲醇中毒最常见的原因是掺有甲醇的白酒。甲醇的主要代谢产物甲酸会导致病理变化。症状通常在饮用后 6-24 小时内出现,包括视觉障碍、急性神经症状和胃肠道问题。在 COVID-19 大流行的最初一年,甲醇中毒病例显著增加:在本研究中,我们介绍了六名不同的甲醇中毒患者及其临床和影像学特征:在文献综述中,最常见的临床表现是意识丧失和昏迷,另一种是视力丧失。CT扫描结果显示,55%的甲醇中毒患者出现双侧副乳头坏死和出血:结论:甲醇中毒会导致双侧副中枢受累,脑出血患者的死亡率为 50%,因此需要对潜在的副中枢出血进行紧急毒理学分析。
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引用次数: 0
The biological effects and thermal degradation of NPB-22, a synthetic cannabinoid. 合成大麻素 NPB-22 的生物效应和热降解。
IF 2.8 4区 医学 Q2 TOXICOLOGY Pub Date : 2024-07-01 Epub Date: 2024-01-31 DOI: 10.1007/s11419-023-00679-5
Akihiro Takeda, Takahiro Doi, Akiko Asada, Katsuhiro Yuzawa, Akemichi Nagasawa, Kai Igarashi, Tomokazu Maeno, Atsuko Suzuki, Seiko Shimizu, Nozomi Uemura, Jun'ichi Nakajima, Toshinari Suzuki, Akiko Inomata, Takaomi Tagami

Purpose: NPB-22 (quinolin-8-yl 1-pentyl-1H-indazole-3-carboxylate), Adamantyl-THPINACA (N-(1-adamantantyl)-1-[(tetrahydro-2H-pyran-4-yl)methyl]-1H-indazole-3-carboxamide), and CUMYL-4CN-B7AICA (1-(4-cyanobutyl)-N-(2-phenylpropan-2-yl)-1H- pyrrolo[2,3-b]pyridine-3-carboxamide), synthetic cannabinoids were evaluated in terms of CB1 (cannabinoid receptor type 1) and CB2 (cannabinoid receptor type 2) activities, and their biological effects when inhaled similar to cigarettes were examined.

Methods: The half maximal effective concentration values of the aforementioned synthetic cannabinoids at the CB1 and CB2 were investigated using [35S]guanosine-5'-O-(3-thio)-triphosphate binding assays. In addition, their biological effects were evaluated using the inhalation exposure test with mice. The smoke generated was recovered by organic solvents in the midget impingers, and the thermal degradation compounds of the smoke components were identified and quantified using a liquid chromatography-photo diode array detector.

Results: NPB-22 and Adamantyl-THPINACA had equivalent CB1 activity in in vitro assays. Meanwhile, NPB-22 had a weaker biological effect on some items on the inhalation exposure test than Adamantyl-THPINACA. When analyzing organic solvents in the midget impingers, it was revealed that NPB-22 was degraded to 8-quinolinol and pentyl indazole 3-carboxylic acid by combustion. In addition, these degradation compounds did not have CB1 activity.

Conclusion: It was estimated that the biological effects of NPB-22 on the inhalation exposure test weakened because it underwent thermal degradation by combustion, and the resultant degradation compounds did not have any CB1 activity in vitro.

目的:对 NPB-22(1-戊基-1H-吲唑-3-羧酸喹啉-8-基酯)、Adamantyl-THPINACA(N-(1-金刚烷基)-1-[(四氢-2H-吡喃-4-基)甲基]-1H-吲唑-3-甲酰胺)和 CUMYL-4CN-B7AICA (1-(4-氰基丁基)-N-(2-苯基丙-2-基)-1H-吡咯并[2、3-b]吡啶-3-甲酰胺)合成大麻素的 CB1(大麻素受体 1 型)和 CB2(大麻素受体 2 型)活性进行了评估,并研究了它们吸入类似香烟的生物效应。方法:使用[35S]鸟苷-5'-O-(3-硫代)-三磷酸结合试验研究了上述合成大麻素在 CB1 和 CB2 上的半数最大有效浓度值。此外,还利用小鼠吸入暴露试验评估了它们的生物效应。在侏儒撞击器中用有机溶剂回收了产生的烟雾,并使用液相色谱-光电二极管阵列检测器对烟雾成分的热降解化合物进行了鉴定和定量:结果:NPB-22 和 Adamantyl-THPINACA 在体外实验中具有同等的 CB1 活性。同时,在吸入暴露试验中,NPB-22 对某些项目的生物效应弱于 Adamantyl-THPINACA。在分析侏儒撞击器中的有机溶剂时发现,NPB-22 通过燃烧降解为 8-喹啉醇和戊基吲唑-3-羧酸。此外,这些降解化合物没有 CB1 活性:结论:据估计,NPB-22 在吸入暴露试验中的生物效应有所减弱,这是因为它在燃烧过程中发生了热降解,而由此产生的降解化合物在体外没有任何 CB1 活性。
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引用次数: 0
Rapid screening of riot control agents using DART-TD-HRMS. 利用 DART-TD-HRMS 快速筛选防暴制剂。
IF 2.8 4区 医学 Q2 TOXICOLOGY Pub Date : 2024-07-01 Epub Date: 2024-02-22 DOI: 10.1007/s11419-024-00681-5
Lina Mörén, Anders Östin, Andreas Larsson, Julia Forsberg, Daniel Wiktelius, Pernilla Lindén

Purpose: Riot Control Agents (RCAs) are chemicals used in law enforcement for non-lethal riot control and use in conflicts between states that violates the Chemical Weapons Convention. OPCW's Scientific Advisory Board has identified sixteen potential RCAs including capsaicinoids, CS, and CR. RCAs may be misused for criminal purposes, so methods for detecting such misuse are needed. This study therefore evaluates the feasibility of a rapid, high throughput screening method of RCAs on surfaces (particularly clothing surfaces) by Direct Analysis in Real Time with a thermal desorption unit coupled to high-resolution mass spectrometry (DART-TD-HRMS).

Methods: A broadly applicable method for detecting potential RCAs was developed and tested on cotton fabric samples sprayed with self-defence sprays from an in-house reference stock. The feasibility of detecting RCAs by direct analysis of surface wipe samples placed in the DART source was also investigated.

Results: The method detected all sixteen RCAs and contaminated clothing were successfully screened for active agents in a reference collection of self-defence sprays. A pilot study also showed that RCAs can be detected by holding a sample directly in front of the DART source.

Conclusion: DART-TD-HRMS enables rapid and simple screening of RCAs on fabric samples enabling a high sample throughput.

目的:骚乱控制剂(RCAs)是执法部门用于非致命性骚乱控制的化学品,也可用于违反《化学武器公约》的国家间冲突。禁止化学武器组织的科学顾问委员会已经确定了十六种潜在的 RCA,包括辣椒素、CS 和 CR。RCA 可能会被滥用于犯罪目的,因此需要找到检测此类滥用的方法。因此,本研究评估了通过热脱附装置与高分辨率质谱联用直接实时分析法(DART-TD-HRMS)对表面(尤其是衣物表面)上的 RCA 进行快速、高通量筛选的可行性:方法:开发了一种广泛适用的检测潜在 RCA 的方法,并在喷洒了自卫喷雾剂的棉织物样品上进行了测试。此外,还研究了通过直接分析置于 DART 源中的表面擦拭样本来检测 RCA 的可行性:结果:该方法检测出了所有 16 种 RCA,并成功地在自卫喷雾剂参考样品集中对受污染的衣物进行了活性剂筛查。一项试验研究还表明,将样品直接放在 DART 源前也能检测出 RCA:结论:DART-TD-HRMS 可以对织物样品上的 RCA 进行快速、简单的筛查,从而提高样品处理量。
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引用次数: 0
Development of a simple screening method for analyzing cereulide toxin in fried rice using liquid chromatography-tandem mass spectrometry. 利用液相色谱-串联质谱法开发分析炒米中麦角内酯毒素的简易筛选方法。
IF 2.8 4区 医学 Q2 TOXICOLOGY Pub Date : 2024-07-01 Epub Date: 2024-03-22 DOI: 10.1007/s11419-024-00683-3
Hiroshi Koike, Maki Kanda, Chie Monma, Souichi Yoshikawa, Hiroshi Hayashi, Yoko Matsushima, Yumi Ohba, Momoka Hayashi, Natsumi Furuta, Wakaba Okada, Chieko Nagano, Keiko Yokoyama, Tomoko Yokoyama, Takeo Sasamoto

Purpose: The presence of cereulide, an emetic toxin produced by Bacillus cereus, in fried rice samples is critical evidence of food poisoning even in situations where B. cereus could not be detected. This study aims to develop a screening method for analyzing cereulide in fried rice using the QuEChERS procedure and liquid chromatography-tandem mass spectrometry (LC-MS/MS).

Methods: Cereulide was identified and quantified in fried rice samples using the QuEChERS extraction method and LC-MS/MS. The accuracies of the methods were determined by analyzing fortified blank samples at two concentrations (10 and 50 µg/kg) conducted on three samples daily for five days.

Results: The QuEChERS procedure removed matrix compounds from fried rice. Characteristic MS/MS spectra enabled the identification of cereulide. As the matrix effects in seven fried rice samples were within ± 6%, an external solvent calibration curve could be used for quantification. This method exhibited good accuracy ranging from 88 to 89%. The relative standard deviations for both repeatability and intra-laboratory reproducibility were < 4%. These standard deviations satisfied the criteria of the Japanese validation guidelines for residues (MHLW 2010, Director Notice, Syoku-An No. 1224-1). The limit of quantification was 2 μg/kg. The applicability of this method was confirmed using the analysis of cereulide in fried rice samples incubated with emetic Bacillus cereus.

Conclusions: The QuEChERS extraction procedure described herein showed substantial promise as a reliable screening tool for cereulide in fried rice sample.

目的:即使在无法检测到蜡样芽孢杆菌的情况下,炒饭样本中存在蜡样芽孢杆菌内酯(一种由蜡样芽孢杆菌产生的催吐毒素)也是食物中毒的重要证据。本研究旨在利用 QuEChERS 程序和液相色谱-串联质谱法(LC-MS/MS),开发一种分析炒饭中蜡样内酯的筛选方法:方法:采用 QuEChERS 萃取法和液相色谱-串联质谱法对炒米样品中的谷维素进行鉴定和定量。结果:QuEChERS 方法去除了样品中的基质(10 微克/千克和 50 微克/千克),而 LC-MS/MS 方法去除了样品中的基质(10 微克/千克和 50 微克/千克),而 LC-MS/MS 方法去除了样品中的基质(50 微克/千克):结果:QuEChERS 程序可去除炒米中的基质化合物。通过特征性的 MS/MS 图谱可以鉴定出麦角苷。由于 7 个炒米样品中的基质效应在 ± 6% 以内,因此可以使用外部溶剂校准曲线进行定量。该方法的准确度为88%至89%。重复性和实验室内重现性的相对标准偏差均为结论:本文所述的 QuEChERS 提取程序作为一种可靠的筛查炒米样品中谷胱甘肽的工具,显示出了巨大的潜力。
{"title":"Development of a simple screening method for analyzing cereulide toxin in fried rice using liquid chromatography-tandem mass spectrometry.","authors":"Hiroshi Koike, Maki Kanda, Chie Monma, Souichi Yoshikawa, Hiroshi Hayashi, Yoko Matsushima, Yumi Ohba, Momoka Hayashi, Natsumi Furuta, Wakaba Okada, Chieko Nagano, Keiko Yokoyama, Tomoko Yokoyama, Takeo Sasamoto","doi":"10.1007/s11419-024-00683-3","DOIUrl":"10.1007/s11419-024-00683-3","url":null,"abstract":"<p><strong>Purpose: </strong>The presence of cereulide, an emetic toxin produced by Bacillus cereus, in fried rice samples is critical evidence of food poisoning even in situations where B. cereus could not be detected. This study aims to develop a screening method for analyzing cereulide in fried rice using the QuEChERS procedure and liquid chromatography-tandem mass spectrometry (LC-MS/MS).</p><p><strong>Methods: </strong>Cereulide was identified and quantified in fried rice samples using the QuEChERS extraction method and LC-MS/MS. The accuracies of the methods were determined by analyzing fortified blank samples at two concentrations (10 and 50 µg/kg) conducted on three samples daily for five days.</p><p><strong>Results: </strong>The QuEChERS procedure removed matrix compounds from fried rice. Characteristic MS/MS spectra enabled the identification of cereulide. As the matrix effects in seven fried rice samples were within ± 6%, an external solvent calibration curve could be used for quantification. This method exhibited good accuracy ranging from 88 to 89%. The relative standard deviations for both repeatability and intra-laboratory reproducibility were < 4%. These standard deviations satisfied the criteria of the Japanese validation guidelines for residues (MHLW 2010, Director Notice, Syoku-An No. 1224-1). The limit of quantification was 2 μg/kg. The applicability of this method was confirmed using the analysis of cereulide in fried rice samples incubated with emetic Bacillus cereus.</p><p><strong>Conclusions: </strong>The QuEChERS extraction procedure described herein showed substantial promise as a reliable screening tool for cereulide in fried rice sample.</p>","PeriodicalId":12329,"journal":{"name":"Forensic Toxicology","volume":" ","pages":"163-171"},"PeriodicalIF":2.8,"publicationDate":"2024-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11269499/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140193555","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Short- and long-term stability of synthetic cathinones and dihydro-metabolites in human urine samples. 合成卡西酮和二氢代谢物在人体尿样中的短期和长期稳定性。
IF 2.8 4区 医学 Q2 TOXICOLOGY Pub Date : 2024-07-01 Epub Date: 2024-03-30 DOI: 10.1007/s11419-024-00684-2
Abdulaziz A Aldubayyan, Erika Castrignanò, Simon Elliott, Vincenzo Abbate

Purpose: Synthetic cathinones constitute the second largest group of new psychoactive substances, which are often used for recreational purposes and reported in toxicological analysis. Various factors may influence the stability of synthetic cathinones between sampling and analysis, and therefore, stability studies are required to determine the best storage conditions as well as extend the period of detection.

Methods: This study involved sixteen synthetic cathinones and ten dihydro-metabolites spiked in human urine to evaluate the stability under common storage conditions to imitate real forensic toxicology samples. The samples were stored at either room temperature (22-23 °C) for up to 3 days, refrigerated (4 °C) for up to 14 days or frozen (-40 °C) for up to 12 months, and analyzed in triplicate using a validated liquid chromatography-tandem mass spectrometry method.

Results: Analytes' concentrations decreased over time, although slower when stored frozen. All analytes remained stable (> 80%) for 1 month when stored frozen before losses in content were more apparent for some compounds, depending on their chemical structure. Under all storage conditions, the highest instability was observed for analytes containing halogens (i.e., chlorine or fluorine). Thus, halogenated analytes were further investigated by using liquid chromatography coupled to quadruple time-of-flight mass spectrometry to attempt identifying degradation products.

Conclusions: Irrespective of parent analytes, dihydro-metabolites had improved stability at each tested temperature, which highlights their importance as appropriate urine biomarkers when retesting is required after a long period of storage.

目的:合成卡西酮是第二大类新型精神活性物质,经常被用于娱乐目的,并在毒理学分析中被报告。从采样到分析期间,各种因素都可能影响合成卡西酮的稳定性,因此需要进行稳定性研究,以确定最佳储存条件并延长检测期:本研究在人体尿液中添加了十六种合成卡西酮和十种二氢代谢物,以评估它们在普通储存条件下的稳定性,从而模仿真实的法医毒理学样本。样品在室温(22-23 °C)下最多储存 3 天,在冷藏(4 °C)下最多储存 14 天,或在冷冻(-40 °C)下最多储存 12 个月,并采用经过验证的液相色谱-串联质谱法对一式三份样品进行分析:结果:分析物的浓度随着时间的推移而下降,但冷冻保存时下降较慢。所有分析物在冷冻保存 1 个月后仍保持稳定(> 80%),某些化合物的含量损失更为明显,这取决于其化学结构。在所有储存条件下,含有卤素(即氯或氟)的分析物的不稳定性最高。因此,我们使用液相色谱法和四重飞行时间质谱法对卤代分析物进行了进一步研究,试图找出降解产物:无论母体分析物如何,二氢代谢物在每个测试温度下的稳定性都有所提高,这突出了它们在长期储存后需要重新测试时作为合适的尿液生物标记物的重要性。
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引用次数: 0
Kerosene condenses in the trachea following inhalation. 煤油吸入后会在气管中凝结。
IF 2.8 4区 医学 Q2 TOXICOLOGY Pub Date : 2024-07-01 Epub Date: 2024-03-04 DOI: 10.1007/s11419-024-00682-4
Sella Takei, Hiroshi Kinoshita, Sachiko Kawahara, Mitsuru Kumihashi, Mostofa Jamal, Tadayoshi Yamashita, Etsuko Tanaka, Hiroko Abe, Kunihiko Tsutsui, Shoji Kimura

Purpose: We have investigated the absorption dynamics of petroleum fuel components from the analytical results of autopsy samples.

Methods: Post-mortem samples of the severely burned case, including femoral blood, intratracheal contents (mucus) and intratracheal gas-phase samples were collected, and analysed by gas chromatography-mass spectrometer with head-space solid-phase microextraction.

Results: The composition of flammable substances in the tracheal gas phase differed slightly from that in mucus.

Conclusion: High-boiling point components are retained in the trachea, whereas relatively lower-boiling point components are detected predominantly in the tracheal gas phase and blood.

目的:我们从尸体解剖样本的分析结果中研究了石油燃料成分的吸收动态:方法:采集严重烧伤病例的尸检样本,包括股部血液、气管内内容物(粘液)和气管内气相样本,并通过气相色谱-质谱仪和顶空固相微萃取进行分析:结果:气管气相中的可燃物质成分与粘液中的可燃物质成分略有不同:结论:高沸点成分保留在气管中,而相对较低的沸点成分主要在气管气相和血液中检测到。
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引用次数: 0
期刊
Forensic Toxicology
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