Automatic analytical approach for the determination of 12 illicit drugs and nicotine metabolites in wastewater using on-line SPE-UHPLC-MS/MS

In this study,we developed a novel on-line solid phase extraction(SPE)-ultra-high-performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS)-based analytical method for simultaneously quantifying 12 illicit drugs and metabolites(methamphetamine,amphetamine,morphine,codeine,6-monoacetylmorphine,benzoylecgonine,3,4-methylenedioxymethamphetamine,3,4-methylenedioxyamphetamine,cocaine,ketamine,norketamine,and methcathinone)and cotinine(COT)in wastewater samples.The analysis was performed by loading 2 m L of the sample onto an Oasis hydrophilic-lipophilic balance cartridge and using a cleanup step(5%methanol)to eliminate interference with a total run time of 13 min.The isotope-labeled internal standard method was used to quantify the target substances and correct for unavoidable losses and matrix effects during the on-line SPE process.Typical analytical characteristics used for method validation were sensitivity,linearity,precision,repeatability,recovery,and matrix effects.The limit of detection(LOD)and limit of quantification(LOQ)of each target were set at 0.20 ng/L and 0.50 ng/L,respectively.The linearity was between 0.5 ng/L and250 ng/L,except for that of COT.The intra-and inter-day precisions were<10.45%and 25.64%,respectively,and the relative recovery ranged from 83.74%to 162.26%.The method was used to analyze various wastewater samples from 33 cities in China,and the results were compared with the experimental results of identical samples analyzed using off-line SPE.The difference rate was between 19.91%and-20.44%,and the error range could be considered acceptable.These findings showed that on-line SPE is a suitable alternative to off-line SPE for the analysis of illicit drugs in samples.

Quantitative Structure-retention Relationship Study on the GC-MS Retention Time of Illicit Drugs

A quantitative structure-retention relationship（QSRR） study has been carried out on the gas chromatograph-mass spectrometry（GC-MS） system retention time（RT） of two sets of illicit drugs by using molecular structural descriptors.Heuristic method（HM） was utilized to construct the linear models.Appropriate models with low standard errors and high correlation coefficients were obtained（R2=0.9873,F=390.18 for data set 1 and R2=0.9881,F=749.13 for data set 2）.The results of leave-one-out cross validation showed good predictive ability of these proposed models（R c2v= 0.9812 and R c2v= 0.9824,respectively）.Each molecular descriptor in the two models was disputed to unfold the relationship between the molecular structures and RT.

Analysis and Dynamics of Illicit Drug Use Described by Fractional Derivative with Mittag-Leffler Kernel

Illicit drug use is a significant problem that causes great material and moral losses and threatens the future of the society.For this reason,illicit drug use and related crimes are the most significant criminal cases examined by scientists.This paper aims at modeling the illegal drug use using the Atangana-Baleanu fractional derivative with Mittag-Leffler kernel.Also,in this work,the existence and uniqueness of solutions of the fractional-order Illicit drug use model are discussed via Picard-Lindelöf theorem which provides successive approximations using a convergent sequence.Then the stability analysis for both disease-free and endemic equilibrium states is conducted.A numerical scheme based on the known Adams-Bashforth method is designed in fractional form to approximate the novel Atangana-Baleanu fractional operator of order 0<a≤1.Finally,numerical simulation results based on different values of fractional order,which also serve as control parameter,are presented to justify the theoretical findings.

Quality Control of Selected Antimalarials Sold in the Illicit Market: An Investigation Conducted in Porto-Novo City (Republic of Benin)

Malaria is a parasitic disease caused by the bite of female Anopheles mosquito and particularly affects the tropical areas of the world. According to national statistics it is the leading cause of consultations and hospitalizations. Nowadays, despite the surveillance systems for efficient malaria control and access to generic drugs, Benin is witnessing an increased development of illicit drug markets with a large part of the population going towards such markets. However, this is not without adverse impact on the health of individuals, as well as, the economic status of the country. Therefore, the situation needs to be seriously considered by policy makers at various levels, health professionals but also the entire international community in order to thwart this scourge.Regarding the aforementioned situation, the current study was undertaken aiming to perform a quality control of selected antimalarial drugs of the illegal market in Porto-Novo city. Therefore, 40 antimalarial batches were randomly collected in the illicit drug market and submitted to analytical tests such as: macroscopic examination (a visual and critical examination);mass uniformity test;disintegration test;identification test and active ingredients’ content measurement. At the end of the study, the percentages of non-compliance is 97.5%, 5%, 15% and 27.5%, respectively for the content uniformity tests, disintegration, identification and assay. Over-all, 42.5% of noncompliance was recorded. The findings of this study prove that street vended drugs offer no guarantee of good quality and pose a threat to the health of populations. Also, the rate of non-compliance denotes a flaw in the security of the drug distribution system.

Presence of Illicit Drugs in the Sarno River (Campania Region, Italy)

The presence of illicit drugs and their metabolites in surface waters has to be considered a new type of hazard, still unknown, for both the human health and the aquatic ecosystem, due to the potent pharmacological activities of all the illicit drugs. Our research was aimed at evaluating the presence of illicit drugs in the Sarno River (Campania region, Italy), crossing a densely populated area, the basin of the Sarno River, one of the largest and most important economic areas in Campania region, famous for the presence of zones with high landscape-environmental value. The drugs selected for this study were the most used in Campania region. The presence of illicit drugs in surface water was analyzed by a selective multi-residue assay based on liquid chromatographytandem mass spectrometry. The analysis showed the presence of all the illicit drugs investigated: cocaine and its main metabolites (benzoylecgonine, nor-benzoylecgonine), morphine, THC-COOH and codeine;cocaine was the most abundant illicit drug. The presence of illicit drugs and their metabolites in the Sarno River suggests new potential risk for the basin’s inhabitants, using water in the food chain, via field irrigation and animal feed, and for the health of the aquatic fauna.

Differentiation of illicit drugs with THz time-domain spectroscopy

The terahertz time-domain spectroscopy(THz-TDS) was used for sensing and identifying illicit drugs.The absorption spectra of seven illicit drug samples(morphine and its hydrochloride,cocaine hydrochloride,codeine phosphate,papaverine hydrochloride,pethidine hydrochloride,and thebaine) were studied by THz-TDS at 0.3-2.0 THz at room temperature.The geometric structure and vibration frequencies of morphine were calculated by density functional theory.The four absorption features were dominated by intra-/inter-molecular collective or lattice vibration modes.Each illicit drug has a distinct signature in its THz spectra.The results indicate that the THz-TDS can be used to identify and discriminate illicit drugs by their characteristic fingerprints.

缺席审判与违法所得没收程序的差异化构建与调适--以节省司法资源与追回国家资产为视角

缺席审判程序与违法所得没收程序在主要功能、适用对象上存在明显竞合。同时,二者在竞合的表象后面,在适用案件范围和适用条件上呈现出弱层次性,而在程序性质和证明标准上存在本质差别。缺席审判程序是刑事对人之诉,对案件的证明标准与普通案件无异;违法所得没收程序是对物之诉,带有强烈的民事程序属性,对案件的证明标准相对较低。二者存在的上述差异,尤其在证明标准方面的差异,为司法实践的程序选择适用提供了客观衡量基准。在具体程序选择问题上,检察机关可构建基于政策和法律的二元考量模式。此外,两种程序的竞合关系及存在的证明标准差异也使得二者具有互相转换的理论可行性。立足于当前司法实践和立法现状,可在补全各程序的必备条件后进行程序转换,这不仅可节省司法资源和追回国家资产,也有利于“一体构建追逃防逃追赃机制”。基于诉审关系,两种程序转换的主体应为检察机关。

基于国际反腐视角的中国追逃追赃的原则与策略研究

党的二十大报告进一步强调“深化反腐败国际合作,一体构建追逃防逃追赃机制”,这是推动追逃追赃工作高质量发展的现实要求。针对当前追逃追赃过程中的新问题和新动向,既要保持对形势的清醒认识,也要坚持将战略的原则性与策略的灵活性相结合。在反腐败追逃追赃的过程中要以增强忧患意识和保持战略定力相统一、坚持战略判断和战术决断相统一、坚持斗争过程和斗争实效相统一为基本遵循。通过对江苏省领跑反腐败追逃追赃的成功经验进行分析总结,提炼了有关反腐败追逃追赃的斗争策略,为未来追逃追赃工作实现高质量发展提供启发。

雨水管网混接入渗诊断技术研究进展

雨水管网是缓解城市内涝、改善水环境质量的重要市政基础设施,受管材老化腐蚀和施工过程不当等影响,我国城市雨水管网建成后普遍存在地下水入渗和污水混接问题,制约着雨水管网功能高效发挥。排水管网入流入渗诊断技术可为雨水管网混接入渗问题的识别和定位提供支持。综述了排水管网入流入渗诊断技术(物探检测技术、流量分析技术、特征因子分析技术、水动力反演模型技术)的基本原理、研究进展、应用特征等,对比分析了不同技术应用于雨水管网混接入渗诊断的适用性、实施要点、诊断水平和发展阶段等,并提出未来雨水管网混接入渗诊断技术的发展方向。结果表明:1)特征因子分析技术可在不干扰雨水管网正常运行条件下识别和量化混接入渗问题、提供治理优先级,因此经济和环境效益显著;2)光纤分布式测温(FDTS)技术和水动力模型反演技术在无干扰定位雨水管网混接入渗方面优势显著,前者易于实施且定位精准度高,后者具有成本低且可评级混接入渗等级特点,可根据场景特征因地制宜选用;3)未来雨水管网混接入渗诊断技术将朝着低成本、无干扰、可量化、可定位的方向发展。通过评估不同技术在当前和未来的综合应用效果,明确了单一诊断技术难以具备未来预期特征,而特征因子分析技术耦合FDTS技术或水动力模型反演技术的分级诊断体系具有实现未来技术发展目标的优势潜力。研究可为雨水管网混接入渗诊断技术的科学应用和优化创新提供参考。

薄膜固相微萃取/气相色谱-质谱法同时分析电子烟中香精和违禁药物

利用浸涂法制备了沉积聚苯乙烯-二乙烯基苯(PS-DVB)颗粒的PDMS薄膜,通过优化萃取条件,建立基于自制固相微萃取薄膜的电子烟中低沸点香精和高沸点违禁药物的顶空气相色谱-质谱分析方法,确定最佳萃取温度和萃取时间分别为180℃和30 min。对比了热脱附与液液萃取两种薄膜脱附方式,结果显示二者在分析电子烟香精和违禁药物方面相互补充,但考虑方法的适用性,建立了基于液液萃取脱附方式的电子烟特征成分检验技术。通过与传统的样品处理方式直接稀释进样和商品化固相微萃取纤维对比,凸显基于自制PS-DVB/PDMS薄膜顶空分析电子烟特征成分的灵敏度与普适性,所建方法具有去除丙二醇和丙三醇基质干扰、满足高温萃取需求、吸附容量大、成本低的优势。将所建方法应用于实际案件中电子烟样品的检测,检测结果与案情相符,证实方法的准确性与实用性。该研究为电子烟液顶空气体中的香精和违禁药物提供了一种高效、准确的微全分析方案,对生命健康、法庭科学和和公共环境领域具有重要意义。

电导率作为排水管道水质特征指标的潜力分析

水质在线监测是推进排水管道实时分析与动态管理的重要基础。由于监测便捷、成本较低,电导率已被广泛应用于水环境日常监测与水处理效果分析等领域。文章综述了电导率在指示各类水质污染中的应用情况,发现排水系统中的电导率特征主要受排入的雨水及污水中离子含量变化的影响;综合分析排水管道水质特性与安装条件以及电导率测量原理后发现,以电磁法为测量原理的电导率在线监测设备具有更好的适用性,其测量的稳定性和设备的耐受性也要远高于其他化学指标;基于雨污混合试验,发现电导率可以灵敏地反馈不同的雨污混合比。综上,电导率作为排水管道的水质特征初筛指标具有显著优势,但仍需在属地特征方面做好前期研究工作。

A quantitative analysis of socioeconomics of illicit drug use for improving targeted interventions in Hong Kong

Illicit drug use is a critical and challenging issue globally,but there is a lack of thorough understanding of the underlying mechanisms of drug use,which is essential for policy interventions,in many threatened places.This study aims to explore the socioeconomic determinants of drug use to support policy design in Hong Kong and other regions with similar issues.Multiple linear regression models and fixed-effects models are employed to examine the socioeconomic determinants of drug use based on the most comprehensive data on drug use and population in Hong Kong from 1991 to 2016.The estimates show that demographic and socioeconomic characteristics are important predictors of illicit drug use.The highest rate of drug use is observed for people aged between 20 and 30,as well as for those with primary education.Compared with males,the female drug use rate is 15(or 46)per 10,000 people lower for the newly(or previously)addicted cases.A 10%increase in monthly income is associated with a 14%drop in drug use rate at the district level.The average annual expenditure on drug use is USD 32.6 million in Hong Kong.Drug policies shall pay more attention to these at-risk groups,and shall consider more financial support to lower the drug use rates.

Rapid Screening of Nine Illicit Drugs in Human Blood and Urine by Direct Analysis in Real‑Time Mass Spectrometry

We aimed to establish for the rapid detection of morphine,O6‑monoacetylmorphine,heroin,codeine,cocaine,methamphetamine,ketamine,methadone,and dolantin in human blood and urine by direct analysis in real‑time coupled with tandem mass spectrometry(DART‑MS/MS).These samples were extracted by acetonitrile‑methanol(V/V=4:1),using DART 12 Dip‑it automatic sampling system.They were injected at 400℃,and analyzed by positive ion and multiple reaction monitoring mode.The detection limits of morphine,O6‑Monoacetylmorphine,heroin,codeine,cocaine,methamphetamine,ketamine,methadone,and dolantin were 100,50,50,100,20,20,10,1,and 0.01 ng/mL,respectively.The practical cases contained methamphetamine,codeine,cocaine,and O6‑monoacetylmorphine were detected accurately and rapidly.The method has the advantages of high sensitivity and good accuracy.The sample processing is simple and can be analyzed in a short time.This method is suitable for the analysis of morphine,O6‑monoacetylmorphine,heroin,codeine,cocaine,methamphetamine,ketamine,methadone,and dolantin in some practical cases.

污泥中的毒品检测研究进展

毒品及其代谢物通过排泄、倾倒等方式出现在污水、污泥中,不断积累并进入生态环境。污水管道及处理厂的沉积物中积累有大量的有机物,疏水性强的毒品及其代谢物难以在污水中检出,但可在污泥中检出,故开展污泥中的毒品检测研究非常必要,不仅能够用于快速、准确监测区域内的毒品滥用形势,而且可科学评估环境固体基质中毒品及其代谢物残留对生态环境的危害。污泥采样通常使用手持式抓斗,冷冻干燥后于-20℃条件下保存。污泥样本的前处理通常采用加压流体萃取、固液萃取和固相萃取等净化方式,仪器分析方法通常采用液相色谱-串联质谱法。通过对污泥的采集方式、样品前处理方法、污水中毒品及其代谢物的分析方法进行综述,对开展污泥中毒品及其代谢物的检测及生态环境风险评估具有借鉴意义。

家庭关怀度指数问卷在毒品滥用者中的信效度检验

目的分析家庭关怀度指数问卷(family APGAR index,APGAR)在评估毒品滥用者家庭功能方面的适用性,为毒品滥用者家庭功能测量工具选择提供参考。方法采用分层随机抽样方法,随机抽取600名毒品滥用者为研究对象。采用决断值和题总相关系数进行条目分析,采用因子分析和Pearson相关系数检验APGAR的效度,采用Cronbachα系数检验APGAR的信度。结果APGAR呈单因子结构。经因子分析交叉验证,APGAR的单因子结构模型拟合良好(χ^(2)/df=2.011,CFI=0.986,NNFI=0.971,SRMR=0.029,RMSEA=0.059,AIC=30.053),但删除“适应度”条目后的单因子结构模型更优(AIC=21.364)。APGAR总分与Rosenberg自尊量表和戒毒信心量表得分之间的Pearson相关系数均具有统计学意义(P<0.001)。5个条目的APGAR的Cronbachα系数为0.78,删除“适应度”条目后的APGAR的Cronbachα系数为0.79。结论APGAR在毒品滥用者中的信效度较好,但在评估该群体家庭功能时需注意“适应度”这一条目的适用性。

城市生活污水覆盖人口规模的估算方法研究进展

污水流行病学通过检测污水中的药物或其代谢物含量,进而反推人均药物消费量,该方法已成为全球监测非法药物的生产、消费以及公共卫生情况的重要手段。但在该方法中,人口数量的不确定性是影响推测结果的主要不确定因素。人口普查、污水处理厂设计能力和人口生物标志物这三种方法都可以为污水流行病学提供人口数量信息。通过对三种人口估算方法的特点简要描述,主要在人口生物标志物选择标准和分类、典型人口生物标志物的特点以及潜在人口生物标志物等方面进行了综述,为采用人口生物标志物进行人口数量估算的理论研究提供参考,以期在未来实现对非法药物的生产、消费以及公共卫生情况更准确的监测预警。

色谱-质谱联用法测定污水中毒品含量的方法比较

污水分析法因其客观、简便等优点,已被越来越多的地方政府用于区域毒情评估。此文建立了高效液相色谱-串联质谱法测定污水中13种毒品及其代谢物和人口标记物,并对离线方法和在线方法进行了比较。离线和在线方法的线性相关系数(R2)均≥0.9970,六次平行测定浓度的相对标准偏差(RSD)分别在0.2~2.5%和0.7~6.7%之间,低、中、高水平的加标回收率分别在88.3~109.8%和98.7~117.6%之间。离线方法对分析仪器的配置和灵敏度要求更低,在样品基质过于复杂、干扰峰难以分辨时更有优势,在线方法的前处理更简单,时间和人力成本更低。将以上方法应用于171个污水处理厂样品中毒品的检测,两种方法的检测结果无显著差别,均能满足污水样品中毒品检测的要求。同时,为了解决某些基质复杂的污水样品检测时存在干扰的问题,还介绍了一种针对特殊污水样品的毒品准确定量的色谱分析思路和策略,以提高方法的通用性、准确性和分析效率,为毒品滥用情况评估提供可靠、高效的分析手段。

“冰毒”掺杂剂的检测技术研究进展

苯丙胺类毒品已经成为21世纪全球范围内滥用最为广泛的毒品,其中以“冰毒”最为常见,长期使用该类毒品会对滥用者的身体和精神造成不同程度的损害。作为合成类毒品,由于制造“冰毒”的原料、工艺不同,涉毒案件中缴获的该毒品中往往会含有大量的掺杂剂,掺杂剂的种类与含量差异对于该类案件的侦破具有重要意义。本文通过对“冰毒”中掺杂剂的种类、性质与检测技术等研究进展进行综述,比较分析各类检测方法的差异,以期能为该类毒品的检验鉴定提供参考,进而为严厉打击毒品违法犯罪提供技术支持。

基于非目标筛查技术的甲基苯丙胺合成路线分析

本文基于气相色谱-质谱联用和多变量分析,建立对样品中痕量杂质成分的非目标筛查技术,实现制毒合成工艺路线推断。优化甲基苯丙胺中杂质成分的气相色谱-质谱联用分析条件,通过主成分分析(PCA)、正交偏最小二乘法判别分析(OPLS-DA)和层次聚类法(HCA)等多变量分析方法对已知合成工艺路线的甲基苯丙胺进行分类处理,进而对未知缴获样品进行关联性分析及合成工艺路线推断。结果显示,本方法可在缺少杂质成分标准物质的情况下,实现对缴获甲基苯丙胺关联性分析和合成工艺路线推断。所建立的非目标筛查技术具有操作简单、可靠性高、无需杂质的标准物质等优势,可为打击涉甲基苯丙胺犯罪提供情报支撑。

核磁共振波谱技术在药品质量与安全方面的应用研究

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