Analyse von heroinproben mit der Kapillargaschromatographie. Vergleich von Glaskapillartrennsäule und gepackter Säule

In forensic examination of illicit heroin samples high-resolution capillary gas chromatography is compared with gas chromatography with packed columns. Separation efficiency, reproducibility of qualitative and quantitative determinations and stability of the columns are examined.A practical method with silylation of the samples is presented which allows safe identification and quantification of many various compounds contained in illicit heroin samples. The gas chromatographic data of 35 substances (opium alkaloids and synthetic derivatives, adulterants and diluents) are listed. The method also allows the quantification of morphine, opium, and cocaine samples.     

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.     

Trends in Substance Use by Gender Among Participants in a Jail-Based Substance Use Disorder Treatment Program: 1998–2016

Understanding trends in substance use by gender among jail-based treatment program participants can inform policies and programs tailored to this population. Preprogram assessment data from 3509 individuals entering a jail-based substance use disorder treatment program in Missouri between 1998 and 2016 were analyzed. Primary outcome was program participants’ strongly preferred substances. Demographic covariates and drug preferences were compared between males and females. Average yearly trends in preferred substances were calculated. While 25.8% of the sample preferred heroin, it was more strongly preferred by women (36.4%) than men (22.0%, p < 0.0001). Alcohol and marijuana were preferred more by males. Overall, preferences for heroin and methamphetamine increased over time while alcohol, marijuana, and other stimulants decreased. Women being more likely to prefer heroin and the increasing preference for heroin over time are consistent with national trends. Offering evidence-based treatment like pharmacotherapy and gender-sensitive approaches can help address the needs of this vulnerable population.     

Comparative gas chromatographic studies of heroin samples. Results of a pilot project in West Germany in 1982

From 1.4. -30.10.1982 all heroin samples weighing more than 5 g seized in the States of Baden-Württemberg, Hesse and by the Bundeskriminalamt were analyzed by capillary gas chromatography during a pilot project. For comparison of samples ratios of concentrations of heroin (including its decomposition products 0(6)-acetylmorphine and morphine) and its natural by-products of synthesis acetylcodeine, papaverine, and narcotine (noscapine) were determined. The application of these parameters and further qualitative and quantitative criteria for heroin comparison for investigative and legal purposes are discussed.     

Analysis of volatile compounds in heroin samples

Volatile compounds of 32 street heroin samples were analyzed by head space gas-chromatographic (HSGC) technique. The reliability of this procedure coupled with thin-layer chromatography (TLC), gas chromatography (GC), high performance liquid chromatography (HPLC), and its application to forensic casework (comparative sample analysis) is discussed.     

Particle size analysis of six illicit heroin preparations seized in the U.K.

Illicit heroin is rarely pure and may contain a number of other substances. The total particle size distribution in six illicit heroin preparations was analysed using a Malvern 2600 Particle Analyser and by sieving. The pattern of heroin distribution amongst these particles was determined by HPLC. The results show that a representative illicit heroin particle is approximately 45 μm in diameter (137 pmol heroin) and that particles occur over a wide size range, from at least 5.8 to 564 μm in diameter. Aggregated data for the samples studied showed that the overall distribution of heroin particle size largely follows the total particle size distribution, but that this correlation is not necessarily true for individual drug preparations. These results have important implications for any system designed to detect concealed illicit heroin preparations by collection and analysis of drug particles.     

Heroin, morphine, and hydromorphone determination in postmortem material by high performance liquid chromatography

A procedure has been developed for the simultaneous determination of heroin, morphine, and hydromorphone from postmortem tissues by reversed phase high performance liquid chromatography (HPLC) using electrochemical detection. This method permits the direct determination of unmetabolized heroin from antemortem or postmortem urine as evidence of illegal drug use. Presumptive confirmation of heroin was based on the ability to hydrolyze the HPLC heroin fraction to morphine. Heroin was also confirmed in urine by gas chromatographic/mass spectroscopic (GC/MS) analysis of the HPLC fraction. Analysis of postmortem blood, gastric contents, urine, and injection site tissues have revealed the presence of morphine and hydromorphone, while heroin has only been identified in urine.     

Detection of Cutting Agents in Drug‐Positive Seized Exhibits within the United States

The following report summarizes a study performed on seized drug exhibits collected in two U.S. states to evaluate the presence and identification of cutting agents. Aliquots of seized drug materials from Kentucky (n = 200) and Vermont (n = 315) were prepared using a dilute‐and‐shoot procedure. Initial analysis was performed using gas chromatography–mass spectrometry (GC‐MS) followed by analysis using liquid chromatography quadrupole time‐of‐flight mass spectrometry (LC‐QTOF). Active compounds detected overall included caffeine (31.0%), quinine/quinidine (24.7%), levamisole (11.6%), acetaminophen, (8.2%) and procaine (8.2%). These compounds were found with several drugs of abuse, such as heroin, fentanyl, methamphetamine, and cocaine. This novel information about cutting agents used to dilute or alter drugs of abuse is important to criminal investigations and in the management of acute intoxications at health centers. However, common methodologies for analysis and standard reporting practices frequently do not include cutting agents, resulting in lacking or inadequate information regarding prevalence of these substances.     

Impurities, adulterants and diluents of illicit heroin in Denmark (Jutland and Funen)

The contents of impurities, adulterants and diluents in 77 samples of illicit heroin were determined by a combination of high-performance liquid chromatography and gas chromatography. The origin of each sample was characterized by calculating the content of the opium alkaloids in relation to the heroin content. The routes of distribution were compared by determination of the contents of caffeine, procaine and sugars. The results were used as a "chemical fingerprint" of each sample. The results indicate that it is difficult to prove, with certainty, that two samples are identical. However, in most cases, by determining the amounts of impurities, adulterants and diluents in heroin samples, it will be possible to ascertain whether two samples are different and, in many cases, to determine with reasonable certainty whether two samples are identical.     

Near‐fatal Intoxication with the “New” Synthetic Opioid U‐47700: The First Reported Case in the Czech Republic

Recreational use of the potent synthetic opioid 3,4‐ dichloro‐N‐(2‐(dimethylamino)cyclohexyl)‐N‐methylbenzamide (U‐47700) is rising, accompanied by increasingly frequent cases of serious intoxication. This article reports a case of near‐fatal U‐47700 intoxication. A man was found unconscious (with drug powder residues). After 40 h in hospital (including 12 h of supported ventilation), he recovered and was discharged. Liquid chromatography/high‐resolution mass spectrometry (LC/HRMS) or gas chromatography/mass spectrometry (GC/MS) were used to detect and quantify substances in powders, serum and urine. Powders contained U‐47700 and two synthetic cannabinoids. Serum and urine were positive for U‐47700 (351.0 ng/mL), citalopram (<LOQ), tetrahydrocannabinol (THC: 3.3 ng/mL), midazolam (<LOQ) and a novel benzodiazepine, clonazolam (6.8 ng/mL) and their metabolites but negative for synthetic cannabinoids. If potent synthetic opioids become cheaper and more easily obtainable than their classical counterparts (e.g., heroin), they will inevitably replace them and users may be exposed to elevated risks of addiction and overdose.     

In common batch searching of illicit heroin samples--evaluation of data by chemometrics methods

In this study three illicit heroin samples which belonged to three different batches were subdivided into eight samples each. To simulate the dealers' chain, and to check the influence (if any) of diluents on the analytical results, some of the samples were cut with the most frequently used cutting substances, whereas the others were left unchanged. Samples were analysed (within a 10-week period of time) by gas chromatography-mass spectrometry (GC-MS) and characterised by seven variables each. To recover batch links among investigated heroin samples three multivariate methods, i.e. hierarchical clustering (HCA), principal component analysis (PCA) and k-nearest neighbours (k-NN), were applied on to the normalised and scaled analytical dataset. The classification abilities of the HCA, PCA and k-NN were in the range from 95 to 100%. Disturbing effects due to the dilution of samples have not been observed.     

GC/MS determination of pyrolysis products from diacetylmorphine and adulterants of street heroin samples

The inhalation of heroin vapors after heating on aluminium foil ("chasing the dragon") is gaining popularity nowadays among heroin users seeking to avoid the risks of parenteral drug administration. The heroin-smoking procedure was simulated under laboratory conditions by heating the samples on aluminium foil at 250 to 400 degrees C and collecting the vapors in a condenser trap. A total of 72 pyrolysis products of diacetylmorphine, street heroin, residues from aluminium foils used to smoke street heroin, typical by-products, and adulterants were detected by gas chromatography/mass spectrometry (GC/MS). About half of these compounds could be identified. Diacetylmorphine (base and salt) undergoes substantial to complete degradation. Some typical street heroin constituents, like morphine, codeine, acetylcodeine, papaverine, and caffeine, are rather heat-stable. Other compounds, like noscapine and paracetamol, are pyrolyzed to a greater extent. The principal chemical reactions leading to the formation of pyrolysis products are desacetylation, transacetylation, N-demethylation, O-methylation, ring cleavage and oxydation.     

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。     

Comparative analysis of illicit heroin samples

The comparative analysis of street heroin samples is still an object of scientific discussion. A combination of a wide range of analytical techniques is necessary to obtain a valid amount of information about the sample composition, and it is impossible to define an unique analytical approach. We suggest a complete analytical sequence based on analysis of volatile compounds, opiates, diluents, adulterants and metals, by head space gas chromatography (HS/GC), gas chromatography mass spectrometry (GC/MS), thin layer chromatography (TLC), high pressure liquid chromatography (HPLC) and atomic absorption (AA) using a sample amount as low as 50-100 mg. The outlined procedure can be successfully applied to routine work, thus obtaining suitable information about a sample's chemical composition. This helps to attribute or exclude common sources of separate specimens. Results obtained on 33 street heroin samples confiscated in the metropolitan area of Rome are listed.     

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     

idPAD: Paper Analytical Device for Presumptive Identification of Illicit Drugs

As drug overdose deaths across the United States continue to rise, there is increasing interest in field testing of illicit substances. This work discusses a paper-based analytical device (idPAD) that can run a library of 12 colorimetric tests at the same time, each detecting different chemical functional groups and materials found in illicit drugs, distractor substances, and cutting agents. The idPAD requires no electricity, costs less than $2 USD, and requires minimal training to operate. The results of the 12 tests form a color barcode which is “read” by comparison to standard images. The accuracy of the idPAD was assessed using samples of heroin, cocaine HCl, crack, and methamphetamine at concentrations of 25%–100% in a lactose matrix, as well as pure lactose. Based on 840 “reads” by three different users, the idPAD showed 95% sensitivity and 100% specificity for detecting these drugs; the most common error was mistaking cocaine HCl for crack or crack for cocaine HCl. In a second step, samples of heroin, cocaine, and methamphetamine (n = 30) and distractor substances (pharmaceuticals, cutting agents, and other illicit drugs, n = 64) were tested by two readers, yielding a sensitivity of 100% and specificity of 97%. Targeted substances were detected reliably at 55–180 μg/lane, and the idPAD was found to be stable for at least 3 months when stored at room temperature. The library approach used in the idPAD may provide the accuracy and robustness necessary for a presumptive field drug test.     

The routine profiling of forensic heroin samples

A method for the routine profiling of illicit heroin samples received in casework has been developed which depends on simple and straightforward sample pretreatment, followed by gas chromatography on a capillary column using flame-ionization detection. The factors affecting the choice of each aspect of the procedure are discussed, as are the statistical data for sampling and the chromatography. Components of illicit heroin derived from opium and other adulterants have been identified. The significance of data from samples examined in 1986 is discussed.     

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.     

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.     

高效液相色谱法测定海洛因含量的不确定度评定

目的建立高效液相色谱法测定海洛因含量的不确定度评定的方法。方法结合海洛因含量测定的全部过程,假设传播系数为1,对产生不确定度的各分量因子进行分析计算与合成。结果不确定度的来源主要包含样品检测时产生的误差值、检测仪器的精密度、天平和使用的容量器皿等的不确定度。结论本评定方法得出检测的误差来自于两个平行样品检测时产生的误差值。