M48磁珠法和Chelex-100法提取脱落细胞DNA的初步比较

目的对M48磁珠法和Chelex-100法提取脱落细胞DNA的检验效果进行比较,为优化提取方法提供参考。方法选取案件受理检材50例烟蒂、50例纺织物品、50例作案工具,根据不同条件分别用吸附法、沾附法获得DNA,采用磁珠法（M48）和Chelex-100法提取后,常规STR检测。结果烟蒂类检材采用2种方法提取DNA,所得结果没有明显差异;纺织物品和作案工具上脱落细胞DNA的提取采用M48磁珠法提取的效果明显优于Chelex-100法。结论相对而言,M48磁珠法更具优势。     

HPLC法分析海洛因中毒死亡后生物检材中的吗啡

初步建立了以HPLC方法检测海洛因中毒生物检材中的吗啡方法,给出两种比较理想、可供定性、定量分析的色谱条件;生物检材处理,提取净化方法简便快速,并通过对10例海洛因中毒死亡者血液的检测,效果理想,实践证明方法可靠,适用于实际案件的鉴定。     

内标法固相提取-GC/MS检测海洛因吸食者尿液中代谢物

本文建立了以SKF-525A作内标、GDX－301作固相提取剂、用GC／MS方法测定海洛因吸食者尿液中代谢物浓度的方法。系统考查了吗啡、单乙酰吗啡的提取回收率、线性关系等指标。所建立的方法对吗啡和单乙酰吗啡的回收率均大于80％;最小检测浓度小于0.1μg／ml;用代谢物特征离子与内标物特征离子峰高比法测定吗啡与单乙酰吗啡的浓度,在每ml尿添加0．25μg～250μg范围内,二者均有良好的提取线性关系。并对几例海洛因滥用者的尿液进行了检测。     

自制海洛因标准品在常用有机溶剂中稳定性研究

目的 研发海洛因标准品及优化分析方法,以对云南缴获海洛因样本提纯制备成的自制海洛因对照品在常用有机溶剂中的稳定性进一步研究.方法 采用内标及GC、GC/MS方法,通过对提纯制备的海洛因在5种有机溶剂中冷藏保存后含量的变化,观察海洛因在常用有机溶剂中的稳定性.结果 乙醇、三氯甲烷及乙腈为溶剂的自制海洛因对照品储备液,保存30天时间范围内海洛因含量未发生明显变化;以丙酮作为溶剂的自制海洛因对照品储备液,在7至30天时间范围内,海洛因含量明显升高;以甲醇作为溶剂的自制海洛因对照品储备液,在0小时至30天时间范围内,海洛因含量一直呈明显的下降趋势.结论 乙醇、三氯甲烷及乙腈可以作为海洛因样品储备液溶剂使用,丙酮、甲醇不适合作为海洛因样品储备液溶剂使用.     

海洛因来源鉴定的新方法

毒品来源的鉴定是指对毒品样品中包含的来源信息进行提取拜分析,这有助于打击毒品犯罪.海洛因是危害我国的主要毒品,它的来源鉴定更引起人们的关注.本文介绍了国际上研究海洛因来源的三种方法,即研究海洛因样品中的各种有机杂质及其相对比例;研究海洛因样品中的痕量无机元素;研究海洛因及吗啡的稳定同位素相对比值.第三种方法能够反映样品的地域性特点,因而在来源鉴定方面有突出的优势.气相色谱-燃烧-同位素比值质谱法是同位素比值测定方法中用于海洛因来源鉴定的最佳手段.这一技术还可用于其他微量物证(如炸药、药品、油品等)的来源鉴别,因而在法庭科学领域内显示了广阔的应用前景.     

快速溶剂萃取-气相色谱/质谱法分析血液中的4种滥用药物

目的 建立生物检材血液中滥用药物的快速溶剂萃取（ASE）方法.方法 通过优化快速溶剂萃取各参数,提取血液中的滥用药物进行GC/MS定性定量分析.结果 血液中美沙酮、可卡因、蒂巴因、海洛因4种滥用药物的平均回收率在87.8％～97.5％之间,滥用药物在0.4μg/mL～4.0μg/mL的浓度范围内线性良好.结论 该方法具有操作简便快捷,回收率高、重现性好等特点,可广泛应用于生物检材血液中滥用药物的检验鉴定.     

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…     

体内海洛因代谢产物的分析研究

本文介绍了从海洛因成瘾者尿中提取净化和定性定量分析海洛因主要代谢产物单乙酰吗啡和吗啡的方法．阳性尿以乙基吗啡为内标．水解后液－液提取或液－固提取，经衍生化后采用ＧＣ／ＭＳ，ＧＣ／ＦＩＤ，ＧＣ／ＮＰＤ法分析，方法简便、准确、灵敏、重现性好．应用本法对八十余例吸毒成瘾者尿样进行测定，取得了令人满意的结果．     

171例滥用海洛因者的尿样分析

通过 GC/MS分析方法,对 171例滥用海洛因者的尿样进行了分析、统计,结果显示：在所检样品中检出吗啡的占 74.2％,检出海洛因的占 17.6％,检出 O6－单乙酰吗啡的占 52.1％,检出可待因的占 86.5％。因此,从统计学上说,在滥用海洛因者的尿样中检出海洛因是完全可能的。     

吸毒案件中的尿吗啡检测

目的　研究吸毒人员停止使用毒品海洛因后 ,尿吗啡含量自然递减的一般规律。方法　对确证的 1 82名吸毒 (海洛因 )人员在停止使用毒品后连续 9天采集尿样 ,用放射免疫分析法检测尿吗啡含量。结果　 1 82名吸毒 (海洛因 )人员在停止吸毒后第 8天 ,尿吗啡平均含量降至 30ng/ml。 结论　在办案中 ,吸毒 (海洛因 )人员的尿样检测 ,建议最好在末次使用海洛因 8天之内     

Isolation and purification of heroin from heroin street samples by preparative high performance liquid chromatography

The present study established a novel method using preparative high performance liquid chromatography to isolate and purify heroin·HCl from heroin street samples to be used as a reference standard. Different kinds of mobile phases and columns were used, ultimately the mobile phase consisting of hexane-isopropanol-methanol (65:28:7, v/v) and the SIL preparative column prepared in laboratory were selected as the final condition. Heroin was further purified by the drowning-out crystallization method using isopropanol-methanol (50:1, v/v) and hexane as drowning-out anti-solvents and salting-out agents, respectively. The purity was assessed by analytical high performance liquid chromatography and the confirmation of the chemical structure was performed by IR and NMR. About 110.7mg of heroin·HCl at a purity of over 99.52% was obtained from 180mg of heroin street samples which contained 156.15mg of heroin·HCl component by preparative high performance liquid chromatography. This method is suitable for preparing heroin standards in forensic science area.     

汽油中的毒品还原分析

目的建立汽油中海洛因的检验方法及还原方法。方法利用无水乙醇挥发汽油混合物中的汽油,通过TLC、IR、GC、GC/MS对汽油混合物中溶剂和毒品成份进行了定性定量分析。结果利用该方法对涉案检材成功进行了毒品还原及检验分析。结论该方法适合于此类案件检验。     

Analysis of carbohydrates in seized heroin using capillary electrophoresis

Illicitly produced heroin is commonly cut with carbohydrates to increase bulk. The analysis of these solutes is important for legal and intelligence purposes. A capillary electrophoresis (CE) method was developed for the qualitative analysis of dextrose, lactose, sucrose, inositol, and mannitol in heroin exhibits. For this method, a 64 cm (55.5 cm to detector window) by 50 mum capillary was used with the Agilent Basic Anion Buffer modified to pH 12.1. This separation was performed at 25 degrees C with a voltage of 20 kV and indirect detection with 2,6-pyridinedicarboxylic acid as the visualization reagent. The methodology is also applicable for the screening of inorganic and organic anions using indirect detection, and acidic adulterants using direct detection. For a run time of 13 min, the relative standard deviation (n = 6) of the methodology was better than 0.36% for migration times and less than 2.6% for corrected peak areas. For the analysis of carbohydrates and acidic adulterants in seized heroin, excellent agreement was obtained between CE and nuclear magnetic resonance spectroscopy.     

尿样中海洛因代谢物的测定及海洛因滥用的确认

用ＳＰＥ－ＧＣ－ＮＰＤ法建立了尿样中吗啡、６－单乙酰吗啡及可待因的定性分析方法,适用于海洛因滥用者的尿样分析。尿样中吗啡及可待因的最小检测限均为５０ｎｇ／ｍｌ。方法的相对标准偏差分别为：吗啡１１．３％（ｎ＝５）,可待因１４．２％（ｎ＝５）。方法简便、灵敏、快速,１５ｍｉｎ可完成一例尿样的分析。研究了服用含可待因成分的复方甘草合剂后,尿样中的吗啡及可待因的峰面积比为０．４５７±０．１９７（Ｐ＝９９％）;统计了４０例明确滥用海洛因尿液的分析结果,吗啡与可待因的峰面积比为３．４６±０．８９４,Ｐ＝９９％。可作为判断海洛因滥用的依据。同时与免疫板法比较,附５５例免疫板法阳性尿样的分析结果     

A 'cold synthesis' of heroin and implications in heroin signature analysis utility of trifluoroacetic/acetic anhydride in the acetylation of morphine

Treatment of morphine, at room temperature, with a mixture of trifluoroacetic anhydride (TFAA) and acetic acid (20-30min) affords good yields of heroin. GC-MS and HPLC examination shows that heroin produced by this route to be extremely clean, but the product contains slightly less heroin than observed via the more traditional acetic anhydride (AA) route (76.1% versus 83.55%); and greater quantities of 3-MAM and 6-MAM (6.9% versus 0.75% and 7.13% versus 0.63%). The concentration ratios of the major alkaloid impurities were found to be both production method (TFAA and AA) as well as morphine extraction methodology dependant. Data contained herein describe the impact of this new production method on current intelligence efforts, largely by-passing existing heroin signature programs and the UNDCP's efforts to restrict access to key synthetic precursors. Given the methodology dependency we find that examination of the major alkaloid ratios is unsuitable for the development of a new heroin signature program. Further examination of the TFAA methodology allowed the identification of TFAA specific marker compounds, namely bis-trifluoroacetylmorphine (30), 3-trifluoroacetyl-6-acetylmorphine (31), 3-acetyl-6-trifluoroacetylmorphine (32) and trifluoroacetylcodeine (33). However, the hydrolytic lability of trifluroacetyl esters requires careful treatment of suspect samples, thus we propose a modification to existing HSP's in instances were the 6-MAM/WM ratio falls within the average minimum and maximum values of 6.17 and 17.32.     

Neutral heroin impurities from tetrahydrobenzylisoquinoline alkaloids

Laudanosine, reticuline, codamine, and laudanine are members of the tetrahydrobenzylisoquinoline family of natural products. These alkaloids are present in the opium poppy, Papaver somniferum, and are subsequently found as impurities in clandestinely processed morphine. Morphine is then synthesized to heroin using hot acetic anhydride. During the course of this study, it was determined that these four tetrahydrobenzylisoquinolines undergo degradation to a series of 18 neutral impurities when subjected to hot acetic anhydride. Based on the degradation pathway, these new impurities were categorized into two sets of impurities called the C1-acetates compounds and the stilbene compounds. Synthesis, isolation, and structural elucidation information is provided for the tetrahydrobenzylisoquinoline alkaloids, and the new neutral impurities have been studied. Several hundred authentic heroin samples were analyzed using an established heroin signature program method. This methodology features the detection of trace neutral impurities present in heroin samples. It was determined that all 18 new impurities were detected in various quantities in four different types of heroin samples. Analytical results featuring these new impurities are reported for South American-, Southwest Asian-, Mexican-, and Southeast Asian-type heroin samples. These new impurities, coupled with other established forensic markers, enhance the ability to classify illicit heroin samples.     

The rapid analysis of heroin drug seizures using micellar electrokinetic chromatography with short-end injection

A simple and rapid method for the analysis of heroin seizures by micellar electrokinetic chromatography with short-end injection is described. Separations were performed using an uncoated fused silica capillary, 50 cm x 50 microm I.D. x 360 microm O.D. with an effective separation length of 8 cm. The system was run at 25 degrees C with an applied negative voltage of -25 kilovolts. Injection of each sample was for 2 s at -50 mbar. UV detection was employed with the wavelength set at 210 nm. The background electrolyte consisted of 85:15 (water:acetonitrile, v/v) containing final concentrations of 25 mM SDS and 15 mM sodium borate, pH 9.5. Samples and standards were prepared in 0.1% v/v acetic acid and diluted in the run buffer containing 1 mg/ml of N,N-dimethyl-5-methoxytryptamine as an internal standard. Under these conditions a text mixture containing caffeine, paracetamol, morphine, codeine, heroin, and acetylcodeine was resolved within 1.5 min. The method was used to determine the concentration of heroin in heroin seizure samples, and the results were in good agreement with those obtained by a validated gas chromatographic method.     

Component analysis of illicit heroin samples with GC/MS and its application in source identification

A novel method based on GC/MS and GC for component analyses of seized illicit heroin was established by using SKF525A as an internal standard. The main components in illicit heroin products such as heroin, O3-acetylmorphine, monoacetylcodeine, and O6-acetylmorphine were determined quantitatively and the organic adulterants such as paracetamol, acetaminophen caffeine and theophylline were detected qualitatively using the developed method. With these obtained data, 500 seized illicit heroin samples were divided into nine groups. The decomposition pattern of heroin was studied. The dependencies of both the decomposition pattern and the content ratios of monoacetylcodeine to heroin and monoacetylcodeine to O6-acetylmorphine on the source of the seized illicit heroin were observed. This information was used to develop a novel method for its source identification. The examination results were in agreement with the practical cases, thus providing significant information for detection of criminal cases involving illicit heroin.     

Gas chromatographic method validation for the analysis of major components in illicit heroin seized in Malaysia

Apart from routine analysis of total morphine content required by the criminal justice system, quantification of other major components in illicit heroin has not been considered by the Malaysian enforcement laboratory. In order to quantify various other cutting agents in addition to alkaloids, a gas chromatographic (GC) method was developed to facilitate simultaneous quantification of eight target analytes commonly found in illicit heroin seized in Malaysia within a 12 min run time. The validation results demonstrated high selectivity with the use of an HP Ultra 2 capillary column. Different solvents were studied and methanol:chloroform (1:9) proved best for sample dissolution. The method was repeatable and reproducible. The study ranges covering 50-150% of the preferred concentrations of the eight analytes obtained r(2)>0.9997. Limits of detection up to 6μg/mL were also obtained and the method achieved 99-102% recovery. The capability of the method in heroin profiling was verified using samples from ten case samples.