同位素比值质谱法鉴别缴获的海洛因来源2．海洛因的碳同位素比值质谱法研究

利用气相色谱-燃烧-同位素比值质谱法(GC-C-IRMS)对缴获的海洛因毒品进行来源鉴别。按照测得的海洛因和吗啡的δ13C值,对缴获的海洛因毒品作分类,并根据每对海洛因-吗啡之间的差值,给出了生产的批次信息。本文还提供了GC-C-IRMS法的测定精度并讨论了影响测定精度的诸因素。     

同位素比值质谱法鉴别海洛因来源——1.海洛因水解制备吗啡的研究

同位素比值质谱法(IRMS)是目前鉴别缴获的海洛因来源的三种主要方法之一。用该法研究海洛因的来源应分别考虑吗啡来源地和乙酰化试剂来源二方面的因素。本文以缴获的海洛因毒品制备吗啡的方法着手,从酸性和碱性两条路线考察了海洛因水解制备吗啡的方法。研究水解的实验条件,达到了码啡90%以上的产率和95%以上的纯度。首次提出了最佳的反应参数组合,它们分别为:反应温度100℃,反应时间30min,海洛因样品(包括海洛因盐酸盐和游离碱)与盐酸的摩尔比1:3.0;反应温度100℃,时间45min,海洛因盐酸盐与KOH的摩尔比1:4.4,海洛因游离碱与KOH的摩尔比1:3.4。本文还考察了吗啡气相色谱(GC)定量的工作曲线,并对吗啡的TMS衍生物的GC、GC/MS测定结果进行了比较。     

海洛因毒品中残留有机溶剂的检测方法与结果分析

目的建立固体海洛因毒品中残留有机溶剂的顶空-气相色谱和顶空-气相色谱-质谱联用检测方法。方法采用干法和湿法处理42份样品,密封后90℃加热振荡20min,抽取顶空气体用气相色谱法（DB-WAX毛细柱,30m×0.25mm,0.25μm）和气相色谱-质谱联用法（HP-5MS毛细柱,30m×0.25mm,0.25μm）检测,以已知17种有机溶剂外标法定性。在样品中加水后检测,根据峰高估算5种共有成分的含量。结果在42份海洛因毒品中检出乙酸、乙醚、乙醇、乙酸乙酯、乙醛、三氯甲烷等12种有机溶剂成分,5种主要共有成分相对含量有差别。结论本研究建立的检测方法快速、简便,定性可靠,可用于固体海洛因毒品的来源与批次分析。     

“金三角”来源海洛因样品的关联性判别及来源推断

目的海洛因是最常被广泛滥用的毒品之一,具有高度成瘾性、难以戒断性和严重的社会危害性。本文建立"金三角"海洛因样品Pearson相关性数学模型,对云南6个边境州市公安机关缴获的海洛因样品进行了关联性判别及样品来源推断。方法实验将海洛因样品溶于酸性溶剂中并用有机溶剂进行萃取富集,采用超高效液相色谱-串联质谱法(UPLC-MS/MS)对海洛因样品中15种中性/酸性特征杂质进行检测分析,结合数理统计分析方法完成样品分析。结果通过计算,选定0.965为关联性阈值,并筛选出关联性极强的样品组。同时,采用主成分分析法(PCA)初步将样品划分为Ⅰ、Ⅱ、Ⅲ三个区域。结论结合案件信息、关联性分组及主成分分析结果,实现了对489份"金三角"来源海洛因样品的特征分析。     

为他人藏匿毒品的行为如何定性

犯罪嫌疑人粟某知道其丈夫扈某把大量毒品放在家中抽屉的三个香烟盒中并在家中吸毒．但对毒品的来源并不清楚且对扈某在家中吸毒也不干涉。在扈某被公安机关抓获后，公安机关又去搜查其住处。粟某为使其丈夫逃避处罚．将扈某放在香烟盒中的毒品海洛因藏匿在身上，并在民警带其上警车的过程中趁机把毒品扔掉．被民警当场发现。经依法鉴定，从粟某身上查获的毒品海洛因重82．3克。经审理，扈某涉嫌非法持有毒品罪。     

毒品样品的稳定性研究

对毒品进行同一认定是禁毒工作的一个重要方面。关于毒品稳定性的研究,文献报道尚少,仅见毒品水溶液或在有机溶剂中的稳定性研究。本文研究了目前社会上最常见的海洛因、甲基苯丙胺及氯胺酮样品在固体状态下的稳定性,包括室温和冰箱两种存放条件,结果发现上述毒品的固体样品在室温和冰箱中存放1年其含量无明显变化。     

是吸毒、贩卖毒品还是非法持有毒品

被告人张××、郑×。蔡××。于1994年6月12日12时在张××的小卖部吸食海洛因毒品时，被公安机关当场抓获，并在张××身上缴获毒品海洛因：37小包．重量为168克，海洛因含量为20．8％，在郑×身上缴获毒品海洛因12包81克，海洛因含量为22％，在蔡××身上缴获毒品海洛因9包72克，海洛因含量为19．5％。张、郑、蔡三被告人在公安机关对其提审时，他们还供认各自相互间在吸．食海洛因时以每克50元买入、以每克60元结算互吸，三被告人还称被缴获毒品海洛因是用于自己吸食的。为此，司法机关在对本案的定性时存在三种不同意见。第一种意见认…     

毒品及毒品鉴定(Ⅱ)

2　常见毒品概述　　鸦片类毒品、苯丙胺类毒品、可卡因类毒品、大麻类毒品、常见致幻剂等常见毒品的来源、特性及滥用情况如下分述。2.1　鸦片类毒品目前,鸦片类物质从来源上可以分为天然、半合成和全合成3大类。天然鸦片类又分为外源性和内源性2种。外源性物质包括鸦片、吗啡和可待因等;内源性物质包括天然存在于人和动物的脑中的内啡肽、脑啡肽、强啡肽,在人体中起着镇痛和调节多种生理代谢的作用。半合成代表物是海洛因,全合成代表物是杜冷丁、美沙酮、镇通新等。2.1.1　鸦片、吗啡及海洛因　鸦片类毒品主要来源于原生植物——罂粟。罂…     

唾液检材在毒品检测中的应用

近年来,毒品滥用问题日益突出,提高生物样品中毒品检测技术的性能是法庭毒物学研究的重点。相比于血液和尿液样品,唾液在的样品采集和毒品检测中具有诸多优势,因而逐渐受到重视。本文对近年来国内外唾液样本用于毒品检测方面的研究成果进行综述,介绍唾液毒品检测的发展情况以及相关的代谢动力学研究状况,旨在为相关研究和实践提供参考。     

GC法和GC/MS法在地区毒品情报分析中的应用

目的探讨气相色谱法(GC)和气相色谱/质谱联用法(GC/MS)在地区毒品情报分析中的应用,并用于实际样品分析。方法采用GC/MS法定性分析毒品样品中的主成分、痕量杂质、掺假剂和稀释剂,并选择GC/FID法和内标标准曲线法定量分析上述各组分,通过定性和定量数据的统计和分析,推断该地区的毒品状况。结果用GC/MS定性分析、GC/FID定量分析,和数据的统计比对,获得了某省某年27起海洛因毒品大案样品主成分、痕量杂质、掺假剂和稀释剂组成及含量的特征,发现该省缴获的大宗海洛因毒品主要以掺假和稀释后的产品出现,且咖啡因和扑热息痛为两种主要的掺假剂和稀释剂。结论GC/MS和GC/FID法在地区毒品情报分析和打击毒品犯罪中可以发挥重要作用。     

Detection of counterfeit antiviral drug Heptodin™ and classification of counterfeits using isotope amount ratio measurements by multicollector inductively coupled plasma mass spectrometry (MC-ICPMS) and isotope ratio mass spectrometry (IRMS)

Isotope ratio mass spectrometry (IRMS) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) are highly important techniques that can provide forensic evidence that otherwise would not be available. MC-ICP-MS has proved to be a very powerful tool for measuring high precision and accuracy isotope amount ratios. In this work, the potential of combining isotope amount ratio measurements performed by MC-ICP-MS and IRMS for the detection of counterfeit pharmaceutical tablets has been investigated.An extensive study for the antiviral drug Heptodin™ has been performed for several isotopic ratios combining MC-ICP-MS and an elemental analyser EA-IRMS for stable isotope amount ratio measurements. The study has been carried out for 139 batches of the antiviral drug and analyses have been performed for C, S, N and Mg isotope ratios. Authenticity ranges have been obtained for each isotopic system and combined to generate a unique multi-isotopic pattern only present in the genuine tablets. Counterfeit tablets have then been identified as those tablets with an isotopic fingerprint outside the genuine isotopic range.The combination of those two techniques has therefore great potential for pharmaceutical counterfeit detection. A much greater power of discrimination is obtained when at least three isotopic systems are combined. The data from these studies could be presented as evidence in court and therefore methods need to be validated to support their credibility. It is also crucial to be able to produce uncertainty values associated to the isotope amount ratio measurements so that significant differences can be identified and the genuineness of a sample can be assessed.     

Stable isotope ratios as a tool in microbial forensics--Part 2. Isotopic variation among different growth media as a tool for sourcing origins of bacterial cells or spores

Since the anthrax attacks of 2001 the need for methods to trace the origins of microbial agents has become urgent. The stable isotope ratios of bacteria record information from both the nutrients and the water used to make their culture media and could potentially be used to provide information about their growth environment. We present a survey of carbon (C), nitrogen (N), and hydrogen (H) stable isotope ratios in 516 samples of bacteriological culture media. The observed variation was consistent with expected isotopic variation in the plant and animal products upon which the media are based. The variation is sufficient to translate into substantial isotope variation in cultures grown on different batches of media, and thus to allow investigators to determine whether seized media could have been used to produce seized bioweapons agents.     

Linking ammonium nitrate-aluminum (AN-AL) post-blast residues to pre-blast explosive materials using isotope ratio and trace elemental analysis for source attribution

Forensic science practitioners are often called upon to attribute crimes using trace evidence, such as explosive remnants, with the ultimate goal of associating a crime with a suspect or suspects in order to prevent further attacks. The explosive charge is an attractive component for attribution in crimes involving explosives as there are limited pathways for acquisition. However, there is currently no capability to link an explosive charge to its source via post-blast trace residues using isotope ratios or trace elements. Here, we sought to determine if pre-blast attribution signatures are preserved after detonation and can be subsequently recovered and detected. A field study was conducted to recover samples of post-blast explosives from controlled detonations of ammonium nitrate-aluminum (AN-Al), which were then analyzed via isotope ratio mass spectrometry (IRMS) and inductively coupled plasma-mass spectrometry (ICP-MS) for quantitation and profiling of isotopes ratio and trace element signatures, respectively. Oxygen and nitrogen isotope ratios from AN-Al yielded some of the most promising results with considerable overlap within one standard deviation of the reference between the spreads of pre- and post-blast data. Trace element results from AN-Al support the findings in the isotope ratio data, with 26 elements detected in both pre- and post-blast samples, and several elements including B, Cd, Cr, Ni, Sn, V, and Zn showing considerable overlap. These preliminary results provide a proof-of-concept for the development of forensic examinations that can attribute signatures from post-blast debris to signatures in pre-blast explosive materials for use in future investigations.     

Stable isotope analyses of heroin seized from the merchant vessel Pong Su

A new type of heroin HCl seized in Australia was examined by stable isotope analysis. The final origin/process classification of these samples by chromatographic signature profiles of the impurity/manufacturing by-products was previously determined to be "unknown" by two independent national laboratories. Various drug enforcement authorities speculated that the heroin might be from a new region or new illicit process due to the unusual chromatographic impurity profiles that were present. Samples from 20 different kilogram packages were examined for isotopic content to determine if the samples fit isotopic patterns of known origins or if they were unique to any known origins. Authentic specimens from Southeast Asian (N=59), Southwest Asia (N=37), South America (N=104), and Mexico (N=21) we concomitantly examined for comparison purposes. Both continuous flow elemental analysis-isotope ratio mass spectrometry and gas chromatography-isotope ratio mass spectrometry techniques were utilized. Heroin samples were also converted to morphine, without apparent isotopic fractionation, utilizing methanolic HCl for gas chromatography-isotope ratio mass spectrometry. The Pong Su samples were found to be isotopically and isotopically/alkaloidally distinct from the known origin/process classifications of Southwest Asian, Southeast Asian, South American, and Mexican.     

MS31A位点MVR-PCR技术在法医学鉴定中的应用

应用小卫星特异性引物31A、31A -A、31A -G与α -32PdCTP掺入扩增技术对MS31A(位于D7S21位点)进行MVR -PCR分析 ,成功地建立了一套适合于刑事案件中微量血痕、混合斑、毛发、骨组织等样品鉴定的快速、简便、准确的分析技术。灵敏度分析表明 ,该方法能检测出低至1ng的基因组DNA ,具有较高的灵敏性。本技术在40余起强奸、凶杀等疑难案件中应用均获得成功。本研究还利用MVR数据库资料对实际案件中的犯罪嫌疑人成功地进行了筛选、排查以及串并案工作。     

利用现代物证分析技术推断毒品的来源

利用现代物证分析技术推断毒品的来源,是侦查毒品案件的客观要求,对打击毒品犯罪具有重大意义。随着气相色谱同 位素比值质谱、电感耦合等离子体质谱等现代分析技术的出现,使得我们利用现代物证分析技术推断毒品来源成为可能。     

GC和GC/MS技术在毒品来源推断中的应用

目的应用气相色谱(GC)和气相色谱/质谱联用(GC/MS)技术,定性、定量分析毒品案例,推断毒品来源。方法采用GC/MS法定性分析毒品样品中的主成分、痕量杂质、掺假剂和稀释剂,并选择GC/FID和外标法定量分析上述各组分,通过定性和定量数据的统计比对,并用SPSS10.0数据统计分析软件对分组结果进行验证,推断毒品样品之间来源的区别与联系。结果用GC/MS定性分析、GC/FID定量分析和SPSS10.0数据统计分析软件将12个案件的毒品按来源分成7组,其中1、6、7、11号样品和10A、10B样品分成两组,2、3、5、9号样品各成一组,4号和8号样品分成一组。上述12起案件的毒品来源分析和比对结果,经送检部门反馈的破案信息证明,与案件的真实情况十分吻合。结论应用GC/MS、GC/FID技术分析毒品,可准确推断毒品来源。     

Stable isotope analysis of white paints and likelihood ratios

Architectural paints are commonly found as trace evidence at scenes of crime. Currently the most widely used technique for the analysis of architectural paints is Fourier Transformed Infra-Red Spectroscopy (FTIR). There are, however, limitations to the forensic analysis of white paints, and the ability to discriminate between samples.Isotope ratio mass spectrometry (IRMS) has been investigated as a potential tool for the analysis of architectural white paints, where no preparation of samples prior to analysis is required. When stable isotope profiles (SIPs) are compared, there appears to be no relationship between paints from the same manufacturer, or between paints of the same type. Unlike existing techniques, IRMS does not differentiate resin samples solely on the basis of modifier or oil-type, but exploits additional factors linked to samples such as geo-location where oils added to alkyd formulations were grown. In combination with the use of likelihood ratios, IRMS shows potential, with a false positive rate of 2.6% from a total of 1275 comparisons.     

Illegal Route Estimation of the Seized Illicit Drug, Methamphetamine, by the Comparison of Striation Marks on Plastic Packaging Films

Abstract:  In Japan, the most common illicit drug is methamphetamine. It is possible to trace the origin of this drug by analyzing its organic and inorganic impurities and/or byproducts using several methods, such as GC, GC/MS, and inductively coupled plasma-mass spectrometry (ICP-MS). As reported here, one other method includes comparison of the striation lines of polymer sheet layers from packaging using a polarized light method. Other alternative methods include analyzing the heat sealer pattern, layer thickness surface characteristics, and/or components of polymer sheet layers using infrared spectroscopy. Several of these alternative methods were used to analyze the origins of 29 packages confiscated from three regions over a 1000 km distance in Japan. Results indicated that packages seized from different regions had some polymer sheet layers which contained striation lines and heat sealer patterns that were similar.     

Ultra-trace analysis of illicit drugs from transfer of an electrostatic lift

This article introduces a method of collecting and analysing drug residues that integrates both electrostatic lifting and nanomanipulation-coupled to nanospray ionization mass spectrometry. The application of this hyphenated technique exhibits a useful means of collection and extraction of drug residues with ease and efficiency along with decreased limits of detection. From this method, it will be shown how increased sensitivity of analysis and lower limits of detection for drug analysis can be achieved. The same principles that allow lifting of dust prints by electrostatic lifting can be applied to lifting drug residues. Probing of the drug residues by nanomanipulation occurs directly from the lift, which provides a great platform for extraction. Nanomanipulation-coupled to nanospray ionization-mass spectrometry has been used for the extraction of trace analytes in previous experiments and is known as a very sensitive technique for the detection of ultra-trace residue. This method will demonstrate the electrostatic lifting of drug residue particles from a surface followed by extraction and ionization with nanomanipulation-nanospray ionization. The utility of this novel methodology allows for a more productive analysis when presented with ultra-trace amounts of sample.