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Determination of fentanyl contamination on United States paper currency by LC-QQQ-MS. 利用 LC-QQQ-MS 测定美国纸币上的芬太尼污染。
IF 2.5 3区 医学 Q1 Medicine Pub Date : 2024-03-28 DOI: 10.1093/jat/bkae010
Matthew P Hewes, Donna M Papsun, Barry K Logan, Alex J Krotulski

Previous research has evaluated the extent to which cocaine and other drugs were detectable on currency in the USA. The literature was in agreement that the majority of bills exhibited some degree of contamination. With the increase of fentanyl in the illicit drug supply, this study was designed to evaluate the extent that fentanyl, cocaine, methamphetamine and other substances were present on circulating currency in 2022. A quantitative assay using liquid chromatography-triple quadrupole mass spectrometry was developed and validated to detect six analytes: fentanyl, 4-anilino-N-phenethylpiperidine, acetylfentanyl, benzylfentanyl, cocaine and methamphetamine. One-dollar bills were collected from 13 cities across the country. Sample preparation consisted of soaking the bills in methanol followed by liquid-liquid extraction. Chromatographic separation was achieved using a C18 analytical column and gradient elution with ammonium formate in water (5 mM, pH 3) and 0.1% formic acid in acetonitrile. The quantitative working range for this assay was 0.1 μg to 1.0 μg per bill (equivalent to 1 ng/mL to 100 ng/mL of extract). Fentanyl was detected on the majority (63%) of samples, with 61% of samples having ≥0.1 μg of fentanyl and 4% of samples having ≥1.0 μg. Cocaine and methamphetamine were detected on 100% and 98% of bills, respectively, typically in amounts >1.0 μg. The remaining fentanyl-related substances were detected in 15% of samples in amounts no >0.69 μg per bill and exclusively in the presence of fentanyl. Unsurprisingly, areas of the country with higher incidence of fentanyl use yielded higher frequency of contaminated bills and higher concentrations. Human exposure to drugs on currency is unlikely to have any significant impacts toxicologically or pharmacologically; however, our research findings suggest that paper currency could serve as a useful substrate for surveillance of drug trends regionally, nationally and/or internationally.

以往的研究对美国货币中可卡因和其他药物的可检测程度进行了评估。文献一致认为,大多数纸币都受到了一定程度的污染。随着非法毒品供应中芬太尼的增加,本研究旨在评估 2022 年流通货币中芬太尼、可卡因、甲基苯丙胺和其他物质的含量。研究开发并验证了一种使用液相色谱三重四极杆质谱法的定量检测方法,可检测出六种分析物:芬太尼、4-苯胺基-N-苯乙基哌啶、乙酰芬太尼、苄基芬太尼、可卡因和甲基苯丙胺。从全国 13 个城市收集了一元纸币。样品制备包括将钞票浸泡在甲醇中,然后进行液液萃取。使用 C18 分析柱和甲酸铵水溶液(5 mM,pH 3)及 0.1% 甲酸乙腈溶液进行梯度洗脱,实现色谱分离。该检测方法的定量工作范围为每法案 0.1 μg 至 1.0 μg(相当于 1 纳克/毫升至 100 纳克/毫升的提取物)。大多数样本(63%)中都检测到了芬太尼,其中 61% 的样本中芬太尼含量≥0.1 μg,4% 的样本中芬太尼含量≥1.0 μg。可卡因和甲基苯丙胺的检出率分别为 100%和 98%,通常含量大于 1.0 微克。其余与芬太尼有关的物质在 15%的样本中被检测到,每张钞票中的含量不超过 0.69 微克,并且只存在芬太尼。不足为奇的是,在该国芬太尼使用率较高的地区,受污染钞票的出现频率更高,浓度也更高。人类接触纸币上的毒品不太可能在毒理学或药理学上产生任何重大影响;不过,我们的研究结果表明,纸币可以作为监测地区、国家和/或国际毒品趋势的有用基质。
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引用次数: 0
High-sensitivity neonatal urine drug testing has similar positivity rates to meconium for detecting in utero exposure to methamphetamine and cocaine. 高灵敏度新生儿尿液药物检测在检测子宫内暴露于甲基苯丙胺和可卡因方面与胎粪具有相似的阳性率。
IF 2.5 3区 医学 Q1 Medicine Pub Date : 2024-03-01 DOI: 10.1093/jat/bkad085
Hannah M Brown, Stephen M Roper, Dennis J Dietzen, Bridgit O Crews

Current guidelines recommend universal screening for substance use disorders in obstetric patients, and neonatal drug testing is also frequently performed. Meconium is often the preferred specimen type to detect neonatal drug exposure due to a longer window of detection compared to urine, but most laboratories send out meconium testing to specialized reference laboratories, which can delay results for several days or more. Here, we evaluate a rapid and definitive liquid chromatography-tandem mass spectrometry method for neonatal urine drug testing and compare results obtained using this method to paired meconium drug testing in 1,424 neonates for amphetamines, cocaine, cannabinoids, opiates, oxycodone and phencyclidine. Urine testing showed equivalent sensitivity to current meconium methods for detecting in utero exposure to amphetamines and cocaine.

目前的指南建议普遍筛查产科患者的物质使用障碍,并经常进行新生儿药物检测。胎便通常是检测新生儿药物暴露的首选标本类型,因为与尿液相比,胎便的检测窗口更长,但大多数实验室将胎便检测送到专门的参考实验室,这可能会延迟几天或更长时间才能得出结果。在这里,我们评估了一种快速和确定的液相色谱串联质谱(LC-MS/MS)方法用于新生儿尿液药物检测,并将该方法与1424例新生儿的配对胎粪药物检测结果进行了比较,其中包括安非他明、可卡因、大麻素、阿片类药物、羟考酮和苯环利定(PCP)。尿检结果显示,目前胎粪法检测子宫内安非他明和可卡因暴露的灵敏度与之相当。
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引用次数: 0
A fast and reliable LC-MS-MS method for the quantification of saxitoxin in blood plasma samples. 一种快速可靠的 LC-MS/MS 方法,用于定量检测血浆样品中的沙司毒素。
IF 2.5 3区 医学 Q1 Medicine Pub Date : 2024-03-01 DOI: 10.1093/jat/bkad092
Klára Odehnalová, Petra Přibilová, Blahoslav Maršálek, Pavel Babica

Saxitoxins (STXs) are potent neurotoxins produced by marine dinoflagellates or freshwater cyanobacteria known to cause acute and eventually fatal human intoxications, which are classified as paralytic shellfish poisonings (PSPs). Rapid analysis of STXs in blood plasma can be used for a timely diagnosis and confirmation of PSPs. We developed a fast and simple method of STX extraction based on plasma sample acidification and precipitation by acetonitrile, followed by quantification using liquid chromatography-tandem mass spectrometry (LC-MS-MS). Our approach provides the results ≤30 min, with a limit of detection of 2.8 ng/mL and a lower limit of quantification of 5.0 ng/mL. Within-run and between-run precision experiments showed good reproducibility with ≤15% values. Standard curves for calibration were linear with correlation coefficients ≥0.98 across the assay calibration range (5-200 ng/mL). In an interlaboratory analytical exercise, the method was found to be 100% accurate in determining the presence or absence of STX in human plasma specimens, with recovery values of 86-99%. This simple method for STX determination in animal or human plasma can quickly and reliably diagnose STX exposures and confirm suspected PSP cases to facilitate patient treatment or expedite necessary public health or security actions.

沙西毒素(STXs)是由海洋甲藻或淡水蓝藻产生的强效神经毒素,已知可导致急性和最终致命的人类中毒,被归类为麻痹性贝类中毒(PSPs)。血浆中 STXs 的快速分析可用于及时诊断和确认麻痹性贝类中毒。我们开发了一种快速、简单的 STX 提取方法,该方法基于血浆样品酸化和乙腈沉淀,然后使用液相色谱-串联质谱(LC-MS/MS)进行定量。我们的方法可在 30 分钟内得到结果,检测限 (LOD) 为 2.8 纳克/毫升,定量下限 (LLOQ) 为 5.0 纳克/毫升。运行内和运行间精密度实验显示重现性良好,值≤15%。在测定校准范围(5-200 ng/mL)内,校准标准曲线线性相关系数≥0.98。在一项实验室间分析工作中发现,该方法在确定人体血浆标本中是否含有 STX 时准确度达 100%,回收率为 86-99%。这种在动物或人体血浆中测定 STX 的简单方法可以快速可靠地诊断接触 STX 的情况,并确认疑似 PSPs 病例,从而促进患者治疗或加快必要的公共卫生或安全行动。
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引用次数: 0
Solriamfetol and m-chlorophenylpiperazine cause false positive amphetamine results on urine drug screening. 索利氨酚和间氯苯哌嗪导致尿药物筛选安非他明假阳性。
IF 2.5 3区 医学 Q1 Medicine Pub Date : 2024-03-01 DOI: 10.1093/jat/bkad088
Ashley R Rackow, Claire E Knezevic

Urine drug screening by immunoassay is a common method to quickly identify drug exposures in the emergency setting and to detect unexpected drug exposures in a variety of patient care and occupational health settings. Although they provide rapid results, immunoassays are susceptible to cross-reactivity with other medications and metabolites. Herein we evaluate the performance of the Thermo Scientific DRI Amphetamines immunoassay for reactivity with trazodone, aripiprazole, atomoxetine, solriamfetol and relevant metabolites. Each of these compounds were spiked into drug-free urine across a range of concentrations and assessed for positivity on amphetamine screen. We demonstrate that the Thermo Scientific DRI assay is susceptible to interferences from m-chlorophenylpiperazine (mCPP), the main metabolite of trazodone, and solriamfetol. Characterization of assay-specific interferences in toxicology screening is instrumental for accurate interpretation of toxicology results, evaluation of patients in emergent settings and supporting patient care.

通过免疫分析法进行尿液药物筛选是一种常见的方法,可以在紧急情况下快速识别药物暴露,并在各种患者护理和职业卫生环境中检测意外的药物暴露。尽管免疫测定法能提供快速的结果,但容易与其他药物和代谢物发生交叉反应。在此,我们评估了Thermo Scientific DRI安非他明免疫测定与曲唑酮、阿立哌唑、阿托西汀、索利氨酚和相关代谢物的反应性。这些化合物中的每一种都以一定的浓度加入到无药尿液中,并在安非他命筛查中评估为阳性。我们证明了Thermo Scientific的DRI检测容易受到mCPP(曲唑酮的主要代谢物)和索利氨酚的干扰。毒理学筛查中检测特异性干扰的表征有助于准确解释毒理学结果,评估紧急情况下的患者,并支持患者护理。
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引用次数: 0
Screening and confirmation of psilocin, mitragynine, phencyclidine, ketamine and ketamine metabolites by liquid chromatography-tandem mass spectrometry. 利用液相色谱-串联质谱法筛选和确认 Psilocin、Mitragynine、Phencyclidine、Ketamine 和 Ketamine 代谢物。
IF 2.5 3区 医学 Q1 Medicine Pub Date : 2024-03-01 DOI: 10.1093/jat/bkae002
Madeleine E Wood, Glenna J Brown, Erin L Karschner, Joshua Z Seither, Jordan T Brown, Jessica L Knittel, Jeffrey P Walterscheid

A safe and productive workplace requires a sober workforce, free from substances that impair judgment and concentration. Although drug monitoring programs already exist, the scope and loopholes of standard workplace testing panels are well known, allowing other substances to remain a source of risk. Therefore, a high-throughput urine screening method for psilocin, mitragynine, phencyclidine, ketamine, norketamine and dehydronorketamine was developed and validated in conjunction with a urine and blood confirmation method. There are analytical challenges to overcome with psilocin and mitragynine, particularly when it comes to drug stability and unambiguous identification in authentic specimens. Screening and confirmation methods were validated according to the American National Standards Institute/Academy Standards Board (ANSI/ASB) Standard 036, Standard Practices for Method Validation in Forensic Toxicology. An automated liquid handling system equipped with dispersive pipette extraction tips was utilized for preparing screening samples, whereas an offline solid-phase extraction method was used for confirmation sample preparation. Both methods utilized liquid chromatography-tandem mass spectrometry to achieve limits of detection between 1-5 ng/mL for the screening method and 1 ng/mL for the confirmation method. Automation allows for faster throughput and enhanced quality assurance, which improves turnaround time. Compared to previous in-house methods, specimen volumes were substantially decreased for both blood and urine, which is an advantage when volume is limited. This screening technique is well suited for evaluating large numbers of specimens from those employed in safety-sensitive workforce positions. This method can be utilized by workplace drug testing, human performance and postmortem laboratories seeking robust qualitative screening and confirmation methods for analytes that have traditionally been challenging to routinely analyze.

一个安全和富有成效的工作场所需要一支清醒的员工队伍,不使用会影响判断力和注意力的物质。虽然药物监测计划已经存在,但标准工作场所检测面板的范围和漏洞众所周知,这使得其他物质仍然是风险来源。因此,我们开发了一种高通量尿液筛查方法,用于筛查西洛辛、米曲宁、苯环利定、氯胺酮、氯克他明和脱水氯克他明,并结合尿液和血液确认方法进行了验证。西洛辛和米曲宁在分析方面有许多难题需要克服,特别是在药物稳定性和真实样本的明确鉴定方面。筛选和确认方法根据 ANSI/ASB 标准 036《法医毒理学方法验证标准操作规范》进行了验证。筛查样本的制备使用了配备分散移液管提取吸头的自动液体处理系统,而确认样本的制备则使用了离线 SPE 方法。两种方法均采用液相色谱串联质谱法,筛选方法的检测限在 1-5 纳克/毫升之间,确认方法的检测限在 1 纳克/毫升之间。自动化可加快通量并提高质量保证,从而缩短周转时间。与以前的内部方法相比,血液和尿液的样本量都大大减少,这在样本量有限的情况下是一个优势。这种筛查技术非常适合对大量来自安全敏感岗位的样本进行评估。工作场所药物检测、人体表现和死后实验室可以利用这种方法,对传统上难以进行常规分析的分析物进行可靠的定性筛选和确认。
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引用次数: 0
Distribution of quetiapine between serum and whole blood in therapeutic drug monitoring specimens 治疗药物监测样本中奎硫平在血清和全血中的分布情况
IF 2.5 3区 医学 Q1 Medicine Pub Date : 2024-02-23 DOI: 10.1093/jat/bkae006
Håvard Breivik, Mette Elise Tunset, Morten Brix Schou, Joachim Frost
Quetiapine use is on the rise, leading to a corresponding increase in acute intoxications, some of which have fatal outcomes. When assessing whole blood quetiapine concentrations during forensic autopsies, interpretations are primarily based on toxicity data from studies of serum concentrations. To our knowledge, there are only two previous studies that have attempted to establish the ratio between whole blood and serum quetiapine concentrations, with limited populations and high variability of results. Paired specimens of whole blood and serum from 16 quetiapine users recruited from the Psychiatric Clinic, St. Olav University Hospital were analyzed using LC-MSMS. Quetiapine concentrations in both matrices were determined and compared. The mean blood:serum ratio of quetiapine was 0.74 (SD = 0.05, 95% CI 0.71-0.76, p &lt; 0.001), range 0.66-0.85. Simple linear regression showed strong linear correlation between quetiapine concentrations in the two matrices (B=0.774, p&gt;0.001, r=0.999). Our results imply that quetiapine occurs at lower concentrations within erythrocytes than in plasma. This is most likely due to a high degree of plasma protein binding. Other factors which may influence the distribution of quetiapine between these compartments are solubility, metabolism and passive or active efflux mechanisms. We did not observe any covariation between blood:serum ratios and serum concentrations. Quetiapine was consistently present at lower concentrations in whole blood than in serum. If so inclined to, a conversion factor of approximately 0.7 may be considered for extrapolation of concentrations from serum to whole blood, at least in cases with therapeutic quetiapine concentration levels.
喹硫平的使用呈上升趋势,导致急性中毒事件相应增加,其中一些会造成致命后果。在法医尸检中评估全血奎硫平浓度时,主要是根据血清浓度研究中的毒性数据进行解释。据我们所知,此前只有两项研究试图确定全血和血清中奎硫平浓度的比例,但研究对象有限,结果差异很大。我们使用 LC-MSMS 分析了从圣奥拉夫大学医院精神病诊所招募的 16 名奎硫平使用者的全血和血清配对标本。测定并比较了两种基质中的喹硫平浓度。喹硫平的平均血药浓度比为 0.74(SD = 0.05,95% CI 0.71-0.76,p &lt; 0.001),范围为 0.66-0.85。简单线性回归结果显示,两种基质中的喹硫平浓度之间具有很强的线性相关性(B=0.774,p&gt;0.001,r=0.999)。我们的研究结果表明,喹硫平在红细胞中的浓度低于血浆。这很可能是由于血浆蛋白结合度较高所致。可能影响喹硫平在这些区室之间分布的其他因素包括溶解度、新陈代谢以及被动或主动外流机制。我们没有观察到血液:血清比率与血清浓度之间存在任何共变。全血中的喹硫平浓度始终低于血清中的浓度。如果愿意,至少在治疗性喹硫平浓度水平的病例中,可以考虑使用约 0.7 的换算系数将血清中的浓度外推至全血中。
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引用次数: 0
Correction to: Urine and hair drug test results associated with daily consumption of codeine-predominant poppy seed food products. 更正:尿液和毛发药物检测结果与每天食用以可待因为主的罂粟籽食品有关。
IF 2.5 3区 医学 Q1 Medicine Pub Date : 2024-01-31 DOI: 10.1093/jat/bkad090
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引用次数: 0
High-performance liquid chromatography-tandem mass spectrometry method for measuring cotinine and trans-3'-hydroxycotinine in bronchoalveolar lavage fluid of patients with e-cigarette, or vaping, product use-associated lung injury. HPLC-MS/MS法测定电子烟或产品使用相关肺损伤(EVALI)患者支气管肺泡灌洗液中的可替宁和反式-3’-羟基可替宁。
IF 2.5 3区 医学 Q1 Medicine Pub Date : 2024-01-31 DOI: 10.1093/jat/bkad077
Tiffany Seyler, Benjamin C Blount, Lanqing Wang

In 2019, nearly 3000 U.S. residents developed severe lung injury associated with recent use of e-cigarette or vaping products. The Centers for Disease Control and Prevention responded to the outbreak, which was formally defined as e-cigarette, or vaping, product use-associated lung injury (EVALI). Centers for Disease Control and Prevention Laboratory rapidly developed assays to analyze potentially harmful and addictive substances in bronchoalveolar lavage (BAL) fluid collected from EVALI case patients. This report describes the development and validation of a high-throughput isotope-dilution high performance liquid chromatography-tandem mass spectrometry method for measuring two nicotine biomarkers, cotinine (COT) and trans-3'-hydroxycotinine (HCT), in bronchoalveolar lavage fluid samples. COT and HCT are the major metabolites of nicotine, the addictive alkaloid presents in tobacco products. This method had good specificity and sensitivity. The limit of detection is 0.033 and 0.0165 ng/mL for COT and HCT, respectively, using only 200 µL of sample volume. The within-run and between-run precision were 2-10%. The overall accuracy, calculated from recovery in three different sample matrices spiked at three concentrations, was 94.8% and 93.6% for COT and HCT, respectively. This novel HPLC-MS-MS method was utilized to characterize recent tobacco exposure in EVALI case patients. This method is useful for characterizing tobacco exposure that may be related to acute and chronic lung injury.

2019年,近3000名美国居民因最近使用电子烟或电子烟产品而出现严重肺损伤。美国疾病控制与预防中心(CDC)对疫情做出了回应,疫情被正式定义为电子烟或电子烟产品使用相关肺损伤(EVALI)。CDC实验室迅速开发了分析EVALI病例患者支气管肺泡灌洗液中潜在有害和成瘾物质的方法。本报告描述了一种高通量同位素稀释HPLC-MS/MS方法的开发和验证,该方法用于测量BAL流体样品中的两种尼古丁生物标志物,可替宁(COT)和反式-3’-羟基可替宁。COT和HCT是尼古丁的主要代谢产物,尼古丁是烟草制品中存在的一种令人上瘾的生物碱。该方法具有良好的特异性和敏感性。仅使用200µL样品体积,COT和HCT的检测限分别为0.033和0.0165 ng/mL。批内和批间精度为2-10%。COT和HCT的总准确度分别为94.8%和93.6%,通过在三种浓度下加标的三种不同样品基质中的回收率计算得出。这种新的HPLC-MS/MS方法用于表征EVALI病例患者最近的烟草暴露。这种方法可用于表征可能与急性和慢性肺损伤有关的烟草暴露。关键词:电子烟,电子烟,EVALI,尼古丁,羟基可替宁,可替宁。
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引用次数: 0
Bibliometric evaluation of Journal of Analytical Toxicology as a scholarly publication according to the Web-of-Science citation database. 根据科学网引文数据库对《分析毒理学杂志》作为学术出版物的文献计量学评估。
IF 2.5 3区 医学 Q1 Medicine Pub Date : 2024-01-31 DOI: 10.1093/jat/bkad080
Alan Wayne Jones

Soon approaching its 50th anniversary, Journal of Analytical Toxicology (JAT) is an international scholarly publication specializing in analytical and forensic aspects of toxicology. Science Citation Index (SCI) and Journal Citation Reports (JCR), both of which are part of the Web-of-Science (WOS) database, were used to make a bibliometric evaluation of JAT articles. Between 1977 (volume 1) and 2023 (volume 47), a total of  n = 4,785 items were published in JAT; the top-ten most highly cited articles and the most prolific authors were identified. Changes in the journal impact factor (JIF) were studied between 1997 and 2022, and this metric varied from a low of 1.24 (2006) to a high of 3.36 (2020).The most recent JIF (2022) dropped to 2.5 and the corresponding 5 year JIF was 2.6. JAT's most highly cited article (590 cites) was a working group (SWGTOX) report dealing with standard practices for the validation of analytical methods in forensic toxicology laboratories. JAT published 62 articles each of which were cited over 100 times and the H-index for JAT was 89. The most prolific author of JAT articles was credited with 119 items, the first in 1980 (volume 4) and the latest in 2023 (volume 47). JAT articles were cited 4,537 times in 2022 by all journals in the JCR database, although 520 of these were self-citations (11.5%). Bibliometric methods are increasingly used to evaluate the published work of individual scientists, university departments, entire universities and whole countries. Highly cited articles are considered more influential and authoritative compared with papers that are seldom or never cited.

《分析毒理学杂志》(JAT)即将迎来50周年纪念,是一本专门研究毒理学分析和法医学方面的国际学术出版物。科学引文索引(SCI)和期刊引文报告(JCR)都是科学网(WOS)数据库的一部分,用于对JAT文章进行文献计量评估。1977年(第1卷)至2023年(第47卷)期间,JAT共发表了4785篇文章;确定了十大被引用率最高的文章和最多产的作者。研究了1997年至2022年间期刊影响因子(JIF)的变化,该指标从1.24(2006年)的低点到3.36(2020年)的高点不等。最近的JIF(2022年)降至2.5,相应的5年JIF为2.6。JAT最受好评的文章(590次引用)是一份工作组(SWTOX)报告,该报告涉及法医毒理学实验室使用的验证分析方法的推荐方法。JAT发表了62篇文章,每篇文章被引用超过100次,JAT的H指数为89。JAT文章最多产的作者有119篇文章,第一篇是在1980年(第4卷),最近一篇是在2023年(第47卷)。2022年,JCR数据库中的所有期刊引用了4537次JAT文章,尽管其中520次是自我引用(11.5%)。文献计量方法越来越多地用于评估科学家个人、大学部门、整个大学和整个国家的发表工作。与很少或从未被引用的论文相比,被高度引用的文章被认为更具影响力和权威性。
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引用次数: 0
Simple and rapid detection of three amatoxins and three phallotoxins in human body fluids by UPLC-MS-MS and its application in 15 poisoning cases. UPLC-MS/MS法简便快速地检测人体体液中的三种鹅膏毒素和三种鬼洛毒素及其在15例中毒病例中的应用。
IF 2.5 3区 医学 Q1 Medicine Pub Date : 2024-01-31 DOI: 10.1093/jat/bkad081
Shuo Yang, Di Wen, Fenshuang Zheng, Shanbai Pu, Zhuonan Chen, Mobing Chen, Bin Di, Wei Liu, Yan Shi

Amatoxins and phallotoxins are toxic cyclopeptides found in the genus Amanita and are among the predominant causes of foodborne sickness and poisoning-related fatalities in China. This study introduces and validates a simple, rapid and cost-effective ultra-performance liquid chromatography-mass spectrometry method for the simultaneous determination and quantification of α-amanitin, β-amanitin, γ-amanitin, phallisacin, phallacidin and phalloidin in human blood and urine. Quick therapeutic decision-making is supported by a 9 min chromatographic separation performed on a Waters Acquity UPLC HSS T3 column (100 mm × 2.1 mm, 1.8 µm) using a gradient of high-performance liquid chromatography (HPLC)-grade water and methanol:0.005% formic acid. The analyte limit of quantification was 1-3 ng/mL in blood and 0.5-2 ng/mL in urine. Calibrations curves, prepared by spiking drug-free blood and urine, demonstrated acceptable linearity with mean correlation coefficients (r) greater than 0.99 for all phallotoxins and amatoxins. Acceptable intraday and interday precision (relative standard deviation <15%) and accuracy (bias, -4.8% to 13.0% for blood and-9.0% to 14.7% for urine) were achieved. The validated method was successfully applied to analyze 9 blood samples and 2 urine samples testing positive for amatoxins and/or phallotoxins. Amatoxins and/or phallotoxins were identified in each whole blood sample at a range of 1.12-5.63 ng/mL and in two urine samples from 1.01-9.27 ng/mL. The method has the benefits of simple sample preparation (protein precipitation) and wide analyte coverage, making it suitable for emergency quantitative surveillance toxicological analysis in clinics and forensic poisoning practice.

Amatoxins和phallotoxins是鹅膏属中发现的有毒环肽,是中国食源性疾病和中毒相关死亡的主要原因之一。本研究介绍并验证了一种简单、快速、经济高效的超高效液相色谱-质谱法(UPLC-MS/MS)同时测定和定量人体血液和尿液中的α-鹅膏素、β-鹅膏苷、γ-鹅膏肽、鬼笔素(PSC)、鬼笔苷(PCD)和鬼笔肽(POD)的方法。在Waters Acquity UPLC HSS T3柱(100 mm×2.1 mm,1.8µm)上使用HPLC级水和甲醇(0.005%甲酸)梯度进行9分钟色谱分离,支持快速治疗决策。分析物LOQ在血液中为1-3 ng/mL,在尿液中为0.5-2 ng/mL。通过在无药物的血液和尿液中加标制备的校准曲线显示出可接受的线性,所有鬼洛毒素和阿苯氧胺的平均相关系数(r)均大于0.99。可接受的日内和日间精密度(RSD
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引用次数: 0
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Journal of analytical toxicology
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