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.

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.

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.

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.

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。

Intravenous drug abuse and tricuspid valve endocarditis: Growing trends in the Middle East Gulf region

Traditionally, tricuspid valve endocarditis is uncommon in the Middle East region. However, recent global data indicate growing trends in the use of illicit drug abuse, specifically injectable heroin, in the Middle East Gulf region. The presence of many transit port services in the Middle East Gulf States has led to smuggling of substance abuse drugs in the region. The Middle East Gulf States, currently a transit market, are also becoming a growing consumer market in view of the increased substance abuse in the youth. However, there is a paucity of data with respect to the prevalence or incidence of tricuspid valve endocarditis in the region, probably due to underdiagnosis or underreporting. A high index of suspicion of tricuspid valve endocarditis is essential in patients with a history of intravenous drug abuse. This article reviews the epidemiology of illicit drug abuse in the Middle East Gulf region, as well as the diagnosis and treatment of tricuspid valve endocarditis, and calls for all physicians in the region to be vigilant while dealing with intravenous drug abuse.

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。

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。

“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。

核磁共振波谱技术在药品质量与安全方面的应用研究

本文介绍了核磁共振波谱技术的原理特点和在国内外的发展现状,以及在化学药品、中药与保健品中药物分析等质量与安全方面的应用。通过核磁共振波谱技术具有可深入探测物质内部结构而不破坏样品,并具有准确、快速和对复杂样品不需要预处理就能进行分析等特点建立药品中的检测方法。为解决药品质量监管中出现的化学药品药效不足、中药以次充好以假乱真现象、非法添加未知药物等问题提供必要的分析技术储备。

部分国家大麻合法化对国内运动员的影响和对策研究

在部分国家大麻合法化趋势愈演愈烈的背景下,运动员涉大麻问题日益凸显。为应对大麻合法化趋势对国内体育领域带来的风险和挑战,预防、治理我国运动员涉大麻问题刻不容缓。对此,应全面强化体育、禁毒两部门的协作,一方面落实反兴奋剂教育,推动反兴奋剂立法建设,加强WADA框架下的反兴奋剂协作;另一方面强化对涉大麻违法行为的打击力度,严格落实“外防输入、内防扩散”策略,抵制大麻亚文化侵蚀,全面营造健康体育的良好氛围。

我国部分地区成瘾物质使用的纵向研究第三部分:吸毒人员的人口学特征

目的 :了解我国部分地区吸毒人群的人口学特征、探讨其变化趋势。方法 :采用单因素分析方法 ,对三次不同时间药物流行病学调查的非法成瘾物质滥用者人口学指标进行纵向比较。结果 :三次调查吸毒人群中 ,女性所占比例逐次增加 ,分别为 10 1%、17 1%和 2 2 4 % ;吸毒人员中 ,2 0 - 2 9a和 30 - 39a两年龄组人员最多 ,且年龄呈增加趋势。约 5 0 %吸毒人员未婚 ,离婚比例逐次增加 (3 3%、7 2 %和 17 0 % ) ,分居比率后两次调查 (6 2 %和5 9% )高于首次调查 (2 3% )。 1993年调查小学或以下文化的吸毒人员占 86 4 % ,后两次调查初中文化者分别占6 5 0 %和 6 2 3%。无业、工人或个体户是吸毒人员最常见的职业 ,无业者逐次增加。年收入 10 0 0元以下者和 70 0 0元以上者是吸毒者主体 ,随调查逐次增加 ,吸毒与经济收入呈“U”字关系。结论 :青中年男性、受教育程度较低者、无业或非固定性职业、未婚或非稳定婚姻形式人员是吸毒的高危人群 ;女性使用非法物质者越来越多 ,应加强对她们的关注。吸毒人群年轻化在研究中没有得到证实。

常见毒品的毛细管电泳分析

系统地研究了毛细管电泳分析中各种因素对常见毒品混合物分析的影响，用均匀设计确定了适用几类毒品分离分析的最佳电泳条件。并采用固相提取技术、毛细管区带电泳检测方法对血和尿生物检材中的冰毒、吗啡、单乙酰吗啡、可待因、海洛因等毒品进行了测定。通过对各种提取剂回收率的测定，认为ＧＤＸ３０１和反相Ｃ１８提取效果较好；并考察了几种毒品的线性关系、最小检测量等。

北京市城市河流中精神活性物质的污染水平及环境风险

为评价北京市城市河流地表水体中5种精神活性物质〔METH（甲基苯丙胺）、AMP（苯丙胺）、KET（氯胺酮）、EPH（麻黄碱）和HA（羟亚胺）〕的环境风险,通过对固相萃取柱（Oasis HLB、Oasis MCX、Oasis WAX和Oasis PRi ME HLB）类型、水样酸化、洗脱剂类型及体积等条件的确定,建立了同时测定水环境中精神活性物质的固相萃取-液相色谱-质谱（SPE-LC-MS/MS）联用方法,并对北京市城市河流地表水体中5种精神活性物质的质量浓度水平进行了调查,采用RQ（风险熵）法进行了风险评价.结果表明,在水样未酸化条件下,Oasis MCX柱对精神活性物质的回收率最高,使用含5%（V/V）氨水的甲醇作为洗脱液,5种精神活性物质的回收率可以达到81.8%~91.1%.地表水水体基质加标结果表明,5种精神活性物质的加标回收率均大于75.5%,相对标准偏差均小于10.0%.方法检出限为0.30~0.80 ng/L,定量限为1.00~2.68 ng/L.北京市7条城市河流中5种精神活性物质的质量浓度在1.00~99.51 ng/L之间.EPH在所有采样点均被检出且质量浓度较高,ρ（EPH）平均值为22.79 ng/L;ρ（AMP）相对较低,在1.54~11.23 ng/L之间,但AMP检出率为97.06%;ρ（METH）较高,平均值为14.63 ng/L,最高值（99.51 ng/L）出现在坝河.研究显示,北京市地表水中5种精神活性物质的RQ均小于0.1,表明其可能的环境风险较低,但由于精神活性物质本身具有生物活性,它们对城市河流水生生态系统产生的潜在危害不容忽视.