固相微萃取在苯丙胺类毒品分析中的应用

固相微萃取(solid phase microextraction, SPME)作为一种新型样品前处理技术已受到广泛关注。由于SPME集采样、萃取、浓缩、进样于一体,克服了传统样品前处理技术步骤繁琐、耗时耗力、所需样品量大等诸多缺点,因此在对生物样品中毒品等目标物的分析中具有巨大的应用潜力。本文以纤维SPME技术为例,综述了该技术在苯丙胺类毒品分析中的研究进展,并对其发展方向进行了展望。     

固相微萃取在司法化学鉴定中应用的进展

固相微萃取(SPME)是近年来发展起来的集采样、萃取、浓缩、进样于一体的综合技术。SPME在司法化学鉴定领域有着很好的发展前景,它的主要优点是分析速度快、方法简便、无需溶剂、灵敏度高、所需样品体积小,易于实现仪器化和自动化,适用于现场分析。SPME在司法化学鉴定中的应用十分广泛,用于可燃性的液体残留物、残留爆炸物、生物样品中的毒、药物以及其他物质分析。本文主要对SPME技术及其在司法化学鉴定中的应用与进展做一综述。     

有机爆炸物的现场非介入性检测——顶空固相微萃取一真空气相色谱质谱法

本文考察了顶空固相微萃取在有机爆炸物现场非介入性检测中的适用性。由固相萃取（SPME）纤维头吸附的有机爆炸物用真空气相色谱一质谱联用仪进行检测。该方法所需的洗脱温度低,色谱分离时间短。SPME适用于提取蒸汽压不低于2．4,6-三硝基甲苯（TNT）的挥发性和半挥发性有机爆炸物,如较易挥发且不稳定的化合物三过氧化三丙酮（TATP）的非介入性检测就可以应用该方法。本研究使用静态顶空,尽可能地减少顶空体积,实现了较高的灵敏度。在现场,SPME方法的灵敏度受环境温度的影响较大：由于样品的蒸汽压未达到平衡,在固定顶空体积和萃取时间的条件下,SPME纤维头萃取的样品总量随温度的提高而增加。在有合适容器的情况下SPME纤维头上萃取的样品在取样3天后仍然能顺利检测。     

固相微萃取技术在毛发药物分析中的应用

固相微萃取（SPME）可与GC/MS、HPLC/MS等在线联用,实现分离、分析一体化的特点为其在毛发药物分析中的应用提供了可能性和良好的应用前景。本文对SPME技术在毛发中滥用药物如苯丙胺类、美沙酮、大麻、可卡因、利多卡因等及其相应代谢产物的分析研究及应用进展做一综述。     

固相微萃取法在生物样品前处理中的应用

<正> 固相微萃取法(Solid phase microextraction,SPME)是一种新型的无溶剂萃取技术,它通过在一根长1 cm、直径约为0.3 mm 的溶融石英纤维(Fiber)表面覆渍厚度为5～100μm 不等的高分子聚合材料作为固定相(涂层),采用顶空(HeadSpace,HS)或直接浸入(Direct Immerstion,DI)方式与样品接触,萃取气相或液相中的目标化合物。萃取头连接在一个不锈钢管套上并与手柄连动,整个 SPME 装置类似于一个微量进样器,使用时,把针头刺入已装入样品的密闭容器中,按下手柄,萃取头从针头中探出。当取样结束时,萃取头收纳于针头内,迅速从容器中拔出,不经任何溶剂洗脱而直接     

SPME与GC/MS相结合检验尿液中的氯胺酮

目的应用固相微萃取与气相色谱-质谱联用技术分析尿液中的氯胺酮。方法对影响SPME萃取效果的萃取头类型、萃取时间、解析时间、离子强度等因素条件进行优化,分析尿中氯胺酮。结果在0.5~2.5μg/m l范围内线性关系良好,线性相关系数为0.995 6;最小检出限为2.5μg/L。结论该方法具有预处理简单、分析速度快、灵敏度高等优点,适合实际案件尿样的检验。     

SPME—GC／MS／MS法分析血中助燃剂残留物

目的探讨检验血中助燃剂残留物的分析方法。方法运用SPME(固相微萃取)技术,利用100μmPDMS萃取纤维,于室温条件下以顶空方式直接从血中萃取、浓缩挥发性碳氢化合物,用GC/MS/MS检测分析助燃剂。结果从检验的实际案例显示,可从0.1ml血中检出痕量的助燃剂。结论该方法操作时间短,检材用量少,分析结果较理想。     

应用一滴溶剂萃取（SDE）技术提取尿样中苯丙胺类毒品

目的建立一滴溶剂萃取技术（SDE）在尿样中苯丙胺类毒品检验的提取优化方法。方法通过GC／NPD分析，系统考察了溶剂体积，萃取溶剂，搅拌速度，萃取时间等参数对苯丙胺类毒品的SDE萃取效率的影响。结果经实验研究，建立了SDE最优化方法。结论SDE技术是一种新型样品前处理技术，具有操作简单快速，成本低廉等特点，在毒物毒品检验中具有广泛的应用前景。     

生物样品中苯二氮卓类药物检验概述

概述了苯二氮卓类药物的种类、性质和生物样品中苯二氮卓类药物的提取净化及检验方法。提取净化方法包括液-液萃取法、固相萃取(SPE)、固相微萃取(SPME)。检验方法有免疫测定法、TLC、GC、HPLC、GC/MS等。     

顶空固相微萃取气相色谱法快速检测尿液中氯胺酮

目的建立快速检测吸毒人员尿液中氯胺酮的顶空固相微萃取(HS/SPME)-GC/NPD的方法。方法样品瓶中加入尿液、氢氧化钠溶液、氯化钠,在95℃下加热搅拌,用聚二甲基硅氧烷SPME萃取头(100μm)顶空萃取20min,气相色谱氮磷检测器检测,外标法定量。结果尿液中氯胺酮浓度在0.2~20.0μg/ml范围内呈现线性关系(r2=0.9965),尿液添加1.0μg氯胺酮,平均回收率102.6%,RSD=3.39%(n=7),检测限1.13ng/ml(S/N=3)。结论建立的方法简单、快速、灵敏、准确,十分适合尿液等生物检材中氯胺酮的快速定性定量分析。     

Determination of cannabinoids in biological samples using a new solid phase micro-extraction membrane and liquid chromatography-mass spectrometry

A simple, rapid and relatively solventless method for extraction of objective compounds would be useful for forensic, judicial and clinical purposes. Solid phase micro-extraction membrane (SPMEM) is one such extraction technique that integrates sampling, extraction and concentration into a single step, and combines the advantages of both the solid phase micro-extraction (SPME) and membrane separation. In this study, a new kind of membrane was prepared using polyamide and Tenax compounds, and applied to solid phase micro-extraction. Characteristics of the membrane such as adsorption capacity were tested. Extraction conditions such as adsorption time, desorption solvents, desorption time and assisted desorption treatment methods were studied and optimized. Tetrahydrocannabinol (THC) and cannabidiol (CBD) in blood and brain of the injected male mice, and in spiked human urine were extracted using this solid phase micro-extraction membrane method. The extracted THC and CBD were further determined with LC-MS using APCI. Ions analyzed in single ion monitoring mode were 315 for THC and CBD, and 318 for the deuterated THC internal standard.     

Preparation and usage of a new solid phase micro-extraction membrane

Liquid-liquid or solid phase extraction methods are widely used for isolating analytes from urine, blood and other samples. But the preparation procedures of the samples are laborious, intensive, and costly. In addition, the organic solvents used are toxic to both the human body and the environment. An accurate, simple and rapid method for analysis of some compounds is required for forensic, judicial, and clinical purposes. Solid phase micro-extraction membrane (SPMEM) is a new, simple and solventless preparation technique. It integrates sampling, extraction and concentration into a single step and has the advantages of both the solid phase micro-extraction (SPME) and membrane separation. In this paper, a new kind of membrane used for the solid phase micro-extraction was prepared with amide compounds. The extraction conditions such as adsorption time, desorption solvents, methods and time are studied and optimized. The dichlorvos in the blood, morphine and phenobarbital in the urine were perfectly separated by using this solid phase micro-extraction membrane, and were tested by gas chromatograph-mass spectrometer (GC-MS). All the data were acquired in scan mode except that of morphine which was obtained in a selected ion monitoring (SIM) mode. Ions used for identification were those with m/z 57, 115, 162, 215, 285.     

SPME-GC analysis of THC in saliva samples collected with "EPITOPE" device

In this study we examined the presence of cannabinoids in saliva samples obtained from 24 drug-abusers. The saliva specimens were collected by "EPITOPE" system and the subsequent elution of samples was achieved by centrifugation. The resulting ultrafiltrates have been directly sampled with solid phase micro-extraction (SPME) and then analyzed by GC/MS. Saliva sampling is less invasive than collection of blood.     

The Differentiation of the Volatile Organic Signatures of Individuals Through SPME-GC/MS of Characteristic Human Scent Compounds

Abstract:  Human scent evidence is utilized as an investigative tool through canine scent discriminations based on the premise that human scent is an individualizing characteristic. This study describes the development of what is effectively a human scent barcode consisting of the relative ratios of an individual's "primary odor" compounds utilized to determine a reproducible and individualizing profile which can be stored in a searchable database for a proof of concept of human scent as a biometric measure. Triplicate hand odor samples were evaluated from 10 subjects utilizing solid phase micro-extraction gas chromatography/mass spectrometry (SPME-GC/MS) and compared via Spearman Rank Correlations. Narrowing the compounds considered for each subject to only those common in all three samples, or a subject's "primary odor constituents," produced a greater degree of both individualization and discrimination; at both correlation thresholds of 0.9 and 0.8, the individuals were correctly discriminated and identified in 99.54% of the cases.     

SPME-GC-MS及相似度计算法对内衣中人体气味的分析鉴别

目的探讨内衣中人体气味的分析鉴别方法。方法采用顶空固相微萃取及气-质联用法（SIM）对不同人体内衣中的主要人体气味指标性成分：醇、醛、酮、酯四类物质同时进行测定,同时采用指纹图谱相似度计算法对不同个体的内衣样本的色谱图进行统计分析。结果不同个体的内衣样本中,其人体气味成分差别较为明显,因而是能够通过这四类物质的差别来达到区分鉴别不同个体内衣样本的目的。结论本方法灵敏度高、重现性好,可作为内衣中人体气味的分析鉴别方法。     

SPME-GC\NPD法快速分析尿液中苯丙胺类化合物

建立了ＳＰＭＥ－ＧＣ／ＮＰＤ法同时分析尿液中九种苯丙胺类化合物的方法。取１ｍｌ尿样以４－苯基丁胺为内标,在碱性条件下,将１００μｍＰＤＭＳ纤维头浸入尿液中２０ｍｉｎ,气相色谱进样后热解吸３ｍｉｎ,用ＧＣ／ＮＰＤ进行测定。九种苯丙胺类化合物及内标完全分离,五种苯丙胺类化合物分别在０．０５～１５、０．１～１５、０．２～１５μｇ／ｍｌ浓度范围内线性良好,ｒ为０．９９２８～０．９９９５,变异系数均小于１０％。方法简便、快速、准确,可用于尿液中苯丙胺类违禁药物的检测     

Quantification of propane in biological materials by head-space GC

Propane was measured in specimens taken from two persons who died from a LPG explosion in an apartment using head-space-GC/FID. Because of the variation of instrument performance and sample injection, the internal standard pentane was used. Calibration standards were prepared by injecting each calculated volume of pure propane gas into capped vials containing 2 ml of blood and 5 microl of internal standard. The calibration curve revealed good linearity from 0.09 microg/ml to at least 90 microg/ml. The method validation data also included repeatability and recovery. The propane quantities in blood, fat and brain tissue were between 0.27 and 71 microg/ml (microg/g) with the highest concentration observed in fat. The confirmation of propane was conducted by the means of solid phase micro-extraction and mass spectrometry.     

The evaluation of human hand odor volatiles on various textiles: a comparison between contact and noncontact sampling methods

The focus of this study is to compare contact and noncontact human scent collection procedures across an array of textiles (cotton, rayon, polyester, and wool) to determine an optimized collection method for human scent evidence. Six subjects were sampled in triplicate for each textile and collection mode, and the samples were then analyzed through headspace solid-phase micro-extraction in combination with gas chromatography/mass spectrometry (SPME-GC/MS). Contact sampling with cotton material has been shown to be the collection method that yielded the greatest number of volatile compounds and the highest scent mass amounts. Through Spearman rank correlations, it was shown that an individual's scent profile is more reproducible within samples collected on the same textile type than between different materials. Furthermore, contact sampling with cotton fabric demonstrated the greatest reproducibility producing the lowest amount of type I and type II errors with 90.85% of the samples distinguished at the 0.9 match/no match threshold.     

Determination of tetramethylenedisulfotetramine in human urine with gas chromatograph-flame thermionic detection coupling with direct immersed solid-phase micro-extraction

An analytical method for determination of tetramethylenedisulfotetramine (tetramine) in human urine by gas chromatography-flame thermionic detection (GC-FTD) coupling with a direct immersed solid-phase micro-extraction (DI-SPME) was developed. The enrichment effects of three fiber coatings of SPME for tetramine were compared. Results showed that the enrichment effect of polar 85 microm polyacrylate (PA) coating was better than that of apolar 100 and 7 microm polydimethylsiloxane (PDMS) coatings. Other experimental parameters, such as ionic strength, volume, temperature of sample solution and time for extraction, time and temperature for desorption, were also optimized. The correlation coefficient of the calibration curve was 0.9998 in the range of 0.082-41.0 ng/mL for tetramine. The limit of quantitation of tetramine in urine was 0.082 ng/mL. In this method, the sample pretreatment is simple and convenient. As a monitoring means, it has been successfully applied to detection of tetramine toxicosis in criminal cases, as well as clinical therapy of poisoned sufferer.