红外光谱法用于安钠咖中咖啡因和苯甲酸钠快速定性和定量分析

目的建立安钠咖样品中咖啡因和苯甲酸钠快速定性和定量分析的红外光谱方法。方法采用高纯度咖啡因和苯甲酸钠混合制样的方法制备定性和定量建模样品,通过分析混合样品的红外光谱图,确定安钠咖样品中咖啡因和苯甲酸钠的特征吸收峰。采用偏最小二乘法(partial least squares,PLS)建立红外光谱定量模型。结果通过分析17个咖啡因和苯甲酸钠混合样品(咖啡因纯度范围10%~80%)的红外光谱图,确定了咖啡因的特征吸收峰为1698、1650、1237、972、743、609cm-1;苯甲酸钠的特征吸收峰为1596、1548、1406、845、708、679cm-1。将所有特征吸收峰均检出作为阳性判断依据时,48个安钠咖缴获样品中咖啡因和苯甲酸钠的阳性检出率均为100%。咖啡因PLS定量模型的线性范围为10%~80%,决定系数(R2)为99.9%,交叉验证均方差(root mean square error of cross validation,RMSECV)为0.68%,预测均方差(root mean square error of prediction,RMSEP)为0.91%;苯甲酸钠PLS定量模型的线性范围为20%~90%,R2为99.9%,RMSECV为0.91%,RMSEP为1.11%。配对样本t检验结果显示,高效液相色谱法和红外光谱法的测定结果差异无统计学意义。采用所建立的红外定量方法分析48个安钠咖缴获样品,咖啡因的纯度为27.6%~63.1%,苯甲酸钠的纯度为36.9%~72.3%。结论采用红外光谱法对安钠咖样品中的咖啡因和苯甲酸钠进行快速定性和定量分析,可提高检验鉴定效率、降低检验成本。     

FTIR法检验海洛因中的淀粉、葡萄糖、蔗糖

目的建立检验掺有淀粉、葡萄糖、蔗糖的海洛因的新方法。方法红外光谱。结果给出了用FTIR检验掺有淀粉、葡萄糖、蔗糖的海洛因的判据。结论用红外光谱法可以准确、无损鉴定掺杂淀粉、葡萄糖、蔗糖的海洛因。     

红外光谱在毒药物检验中的应用

目的　建立毒药物检验的红外光谱测定方法。　方法　用液液萃取法提取检材中的安眠药、精神药品、农药、杀鼠剂和无机毒物 ,然后应用红外光谱法进行定性分析。　结果　常见毒药物均有其特征红外吸收峰 ,通过其特征吸收峰可以区分不同毒药物。　结论红外光谱法快速、准确 ,适用于干扰较轻检材中毒药物的定性分析。     

刺激性毒剂杀埃斯（CS）的检验

用化学显色法、红外光谱法，以及色－质联用技术分析具有强烈刺激性气味的毒剂希埃斯，在缺少已知对照样的情况下，用以上方法，可做出准确的鉴定。     

甲基苯丙胺和海洛因标准物质研究进展

甲基苯丙胺和海洛因是禁毒斗争的重要打击目标。毒品检测实验室在对甲基苯丙胺、海洛因相关检材进行定性定量分析时,必须依靠相应的高纯度标准物质作为分析参照,才能得出正确的检测结果。目前,尚未出现针对甲基苯丙胺和海洛因标准物质相关研究进展的报道。国内外现有生物基质甲基苯丙胺标准物质以及甲基苯丙胺纯度标准物质,可应用于体内外甲基苯丙胺的检测鉴定工作。其中,生物基质包括冻干尿液、毛发以及冷冻人体血清。海洛因除纯度标准物质外,已制备出了¹³C标记的海洛因标准物质,¹³C标记后的标准物质较氘代衍生物具有更高的分析精度。制备后的标准物质需经气相色谱-质谱法、液相色谱-质谱法、核磁共振波谱法、傅里叶变换红外光谱法等进行结构确认,同时通过气相色谱、液相色谱等不同定量分析方法进行量值。本文对上述国内外甲基苯丙胺和海洛因标准物质的研究情况进行概述,并展望了未来的研究方向。     

刺激性毒剂希埃斯(CS)的检验

用化学显色法、红外光谱法(IR),以及色-质联用技术(GC/MS)分析具有强烈刺激性气味的毒剂希埃斯(CS),在缺少已知对照样的情况下,用以上方法,可做出准确的鉴定.     

3,4-亚甲二氧基甲卡西酮的鉴定

目的 建立基于傅里叶变换红外光谱(FTIR)、气相色谱-质谱(GC-MS)结合高分辨质谱技术联合鉴定未知样品的方法.方法 未知样品采用红外专用取样器直接检测;甲醇溶解后采用GC-MS和组合型高分辨质谱检测,以MDMA为内标物.结果 未知样品获得的红外光谱特征吸收峰为1679(C=O键),1603,1502,1453,1423,1259,1121,1090,1035,930,887,838,768,742和717cm-1,质谱特征碎片峰(m/z)为58.1,91.0,120.9,149.0和207.0,测得的精确质量数[M+H]+为208.0966.经信息分析未知样品鉴定为3,4-亚甲二氧基甲卡西酮,该物质属于新型化学合成卡西酮类精神活性物质,已经列入部分欧盟国家的管制药物目录.结论 本方法可用于3,4-亚甲二氧基甲卡西酮的鉴定.     

红外光谱技术在毒品分析中的应用

红外光谱法是常用的一种定性检验方法。自毒品分析技术开始发展以来,红外光谱技术就已成为许多国家进行毒品鉴定的一种常用方法。该技术分析毒品主要具有以下特点：所需检材量小,无损,进行红外分析之后所用样本仍可用其他方法进行分析;操作简便、快捷,几分钟就可以完成一个样品分析;环保,不需要其它试剂,不污染环境,有益于操作人员健康;重现性好,特异性强;适应性强,应用范围广泛。     

海洛因真伪及掺假成分的光谱分析

本文在ＰＥ９８３ＧＩＲ－ＰＥ７５００数据站上以海洛因标准光谱图为准，研究了海洛因真伪及掺假成分的红外光谱特征．     

红外光谱微量水平衰减全反射技术检验常见胶水的应用研究

目的建立无损快速检验胶水红外光谱法。方法利用红外光谱衰减全反射技术（ATR）对8种常见胶水样品进行光谱分析,根据出峰位置差异,对8种胶水样品进行鉴别,并建立相应的红外光谱数据库。结果不同类型的胶水其红外图谱有明显差异,而同一类胶水在某些波数区间也存在着一定的差异。结论利用红外光谱衰减全反射技术可以快速、准确、无损的检验鉴别胶水样品。     

140例海洛因毒品案鉴定结果分析

１４０例海洛因毒品案鉴定结果分析张润生（上海市刑事科学技术研究所;上海２０００８３）ＡＮＡＬＹＳＩＳＯＦ１４０ＣＡＳＥＳＯＦＨＥＲＯＩＮ￥ＺｈａｎｇＲｕｎｓｈｅｎｇ（ＳｈａｎｇｈａｉＩｎｓｔｉｔｕｔｅｏｆＦｏｒｅｎｓｉｃＳｃｉｅｎｃｅｓ;Ｓｈａｎｇｈ...     

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.     

Is There a Relationship Between Street Heroin Purity and Drug‐Related Emergencies and/or Drug‐Related Deaths? An Analysis from Vienna,Austria*

This study examines the quality of street heroin seized in Vienna in 1999 and whether there was a relationship between the purity of street heroin and the number of heroin-related emergencies as well as the number of heroin-related deaths. Street heroin confiscated by the Viennese police, run-sheets of drug-related emergencies, and postmortem reports of drug-related deaths in Vienna in 1999 were analyzed. A total of 415 retail samples with a total weight of 128.02 g contained a median percentage of 6.5% diacetylmorphine (range: 0.0-47.0%). All the samples contained a diluent, mainly lactose, as well as adulterants, such as caffeine and/or paracetamol. During the study period, 75 heroin-related deaths and 387 heroin-related emergencies were registered in Vienna. Time-series analysis revealed no statistically significant relationship between the rate of heroin-related incidents and the diacetylmorphine concentration of street heroin samples confiscated in Vienna in 1999. The widely held belief that the number of heroin-related deaths could be explained simply through fluctuations in the purity of street heroin could not be substantiated, even though the results of this study do not rule out an association between the purity of heroin and heroin-related deaths/emergencies.     

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.     

Hmong folk remedies: limited acetylation of opium by aspirin and acetaminophen.

The traditional folk medicine of the Hmong and other Southeast Asian refugees has accompanied them during their immigration in this country over the past two decades. In two recent cases involving Hmong defendants, unknown solids, resembling charcoal in consistency and purported to be "backache remedies," were analyzed and found to be complex mixtures of aspirin, acetaminophen, caffeine and partly acetylated opium. In particular, significant amounts of acetylacetaminophen, 3-O-acetylmorphine, 6-O-acetylcodeine, 6-O-acetylmorphine, and heroin were identified by gas chromatography/mass spectrometry. Heating approximately equal weights of solid opium, aspirin, and acetaminophen at 130 degrees C for several hours produced a mixture of compounds showing a similar acetylation pattern.     

Heroin abuse and a gas chromatographic method for determining illicit heroin samples in Singapore.

The abuse of heroin (diacetylmorphine) in Singapore escalated sharply in 1975 and 1976, as indicated by the 35-fold increase in the number of heroin seizures and the 20-fold increase in the urine samples containing morphine since 1974. A rapid and simple GC method has been described to estimate diacetylmorphine (and caffeine). Monoacetylmorphine and acetylcodeine may be ascertained by an additional step involving acetylation. All gas chromatograms of a large number of samples analyzed consistently had the same pattern, indicating that they possibly had a common origin. This GC "fingerprint," together with the quantitative data, appears to be characteristic of the illicit Asian or Chinese type of heroin found in Singapore. The proportions of the four major ingredients in some twelve typical samples have been tabulated. Statistical data confirming the accuracy and reproducibility of the analytical method have also been presented.     

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.     

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.     

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.     

Isolation, extractive concentration, and determination of caffeine in the studies of blood plasma

The optimal conditions for the isolation of caffeine from human blood by means of acetone extraction are described with special reference to the peculiarities of extraction from aqueous solutions. The possibility of concentration and purification of caffeine from blood plasma using acetone and aceton-chlorophorm mixture (2:8) as the solvents is illustrated. In addition, purification by silica-gel thin layer chromatography is discussed. Thin layer chromatography, UV-spectrophotometry, and high performance liquid chromatography are considered as potential methods for the identification and quantitative determination of caffeine.