固相萃取技术在药(毒)物分析中的应用

用易处理的固相柱进行固相提取已成为毒物学分析中被广泛采用的样品预处理技术之一。此法用于生物样品中微量药、毒物的分离与传统的液一液革取法相比，具有操作简便、省时、省溶剂，不易产生乳化，缩短样品的挥干时间等优点，并可实现样品处理的自动化。在国外，固相革取技术已成为药（毒）物分析中样品须处理方法的一个主要工具。国内也曾有不少应用此方法进行研究和分析毒物的报道[1]。一、固相萃取技术的基本理论和萃取原理固相革取法（Solid－PhaseExtraction，SPE）也称液一固革取法，是根据液相色谱的理论，利用药物（液相）与吸…     

鱼塘水中六氯苯水解产物的检测

<正> 六氯苯(hexachlorobenzene,HCB),也称多氯苯,是一种常见的除草剂。鱼类对六氯苯的毒性比较敏感,常见于鱼塘水中毒鱼案中。本文作者采用固相萃取技术(SPE),分离富集鱼塘水中六氯苯的代谢产物——五氯苯酚,选用GC/MS技术进行分析,检出鱼塘水中的五氯苯酚。使用SPE技术分析检材中的五氯苯酚,具有快速、方便、省溶剂等优点,是一种具有潜力的实用的检验方法。     

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。     

生物样品中鸦片类毒品检验概述

概述了近 5年来生物样品中鸦片类毒品的检验情况 ,其中包括鸦片类毒品的主要种类及结构 ,鸦片类毒品在体内的代谢 ,LLE、SPE和SFE等提取净化技术 ,免疫测定、GC/MS、HPLC和LC/MS等检测方法。     

毒品来源推断技术进展

毒品来源推断技术在打击毒品犯罪中的作用日益引起了各国法庭科学专家们的关注 ,该技术正成为世界各地顶级毒品分析实验室的一项重要组成部分。毒品来源推断技术主要是利用各种先进的分析技术和手段对缴获的毒品样品进行全面的理化检验及组成分析 ,建立其样品指纹图 ,采用科学的统计和数据处理方法 ,推测毒品的可能产地、相关加工工艺和运输过程等毒品来源信息的综合技术。毒品来源推断技术的应用具有为禁毒执法部门提供法律服务和战略、战术情报服务的双重作用。尽管毒品来源推断技术是一种功能强大的工具 ,但应用成功与否取决于多种可变因…     

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.     

环境污水毒品检测技术在禁毒情报中的应用

本文以环境污水毒品检测技术为基础,结合相关法学和统计学理论,为毒品检测技术在禁毒情报的获取中提供了新的应用方式。本文首先介绍了环境污水分析技术的起源以及污水流行病学的研究方法,并对包括样品提取与保存、固相萃取、液相色谱串联质谱法分析在内的污水样品中毒品检测技术手段进行了详细的介绍;进而,对以禁毒情报工作的需求为着力点,通过动态广泛的污水中毒品检测,以大数据的方式获得关于不同种类毒品的时间空间分布情况的方法进行说明论述,充分展现了环境污水检测技术的应用潜力及前景;最后,对此项工作目前在理论和实践中存在的问题与不足进行了简要的汇总和分析。     

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。     

阳离子交换固相提取和HPLC二极管陈列检测快速筛选尿中100种碱性药物及代谢物

使用固相提取柱作为液-液提取分离尿中药物的一种改进已得到普及,因为其回收率高而且操作简便、快速、准确性好.省去了费时的离心、过滤步骤,并杜绝了由于乳化而引起的样品损失.另外,使用一次性提取柱可减少手接触生物样品的污染、固相提取方法(SPE)已报道用于单一药物或结构相关的一类药物,至今未有报道将一种固相提取方法用于多种碱性治疗药物的监测或滥用药物的检验.     

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。     

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.     

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.     

Optimization of Headspace Solid‐Phase Microextraction Technique for Extraction of Volatile Smokeless Powder Compounds in Forensic Applications

Smokeless powders are low explosives and are potentially found in cases involving firearms and improvised explosive devices. Apart from inorganic compound analysis, forensic determination of organic components of these materials appears as a promising alternative, especially the chromatographic techniques. This work describes the optimization of a solid‐phase microextraction technique using an 85 μm polyacrylate fiber followed by gas chromatography‐flame ionization detection for smokeless powder. A multivariate experimental design was performed to optimize extraction‐influencing parameters. A 2⁴ factorial first‐order design revealed that sample temperature and extraction time were the major influencing parameters. Doehlert matrix design has subsequently selected 66°C and 21 min as the compromised conditions for the two predetermined parameters. This extraction technique has successfully detected the headspace compounds of smokeless powders from different ammunition types and allowed for their differentiation. The novel technique allows more rapid sample preparation for chromatographic detection of smokeless powders.     

分子印迹技术在法庭毒物分析中的研究进展

分子印迹聚合物具有预识别性、高度选择性、实用性,已广泛应用在样本前处理中,可以选择性的识别复杂基质中低浓度目标物,提高检测灵敏度。本文旨在综述和探讨分子印迹技术的原理和在法庭科学领域毒物分析应用中的研究进展。     

液相色谱-串联质谱法分析生物检材中的河豚毒素

目的建立血液、尿液以及肝中河豚毒素(tetrodotoxin,TTX)的液相色谱-串联质谱分析方法,并进行方法学验证。方法血液、尿液和肝用1%乙酸甲醇溶液去蛋白后,上清液用固相萃取法净化,LC-MS/MS检测。结果血液、尿液和肝中TTX检出限分别为2ng/mL、2ng/mL和4ng/g。血液和尿液在4～100ng/mL、肝在5～100ng/g的范围内线性关系良好,相关系数r≥0.9973;日内精密度和日间精密度均在12.80%以内;回收率大于47.2%。结论所建方法高效、灵敏、准确,可以为河豚毒素中毒的法医学鉴定、临床诊治以及食品安全的监控提供技术保障。     

A rapid method for the extraction of cocaine and benzoylecgonine from body fluids

A method has been developed for the rapid extraction of cocaine and benzoylecgonine from post-mortem blood and urine samples. Solid phase columns containing C8 packing material gave clean, emulsion free extracts from body fluids. The total time for each extraction was approx. 10 min and the system has the capacity for the simultaneous extraction of up to 10 samples. Urine can be extracted directly, blood samples were sonicated before extraction to allow for their easy passage through the columns. The method gave excellent recoveries of cocaine (98-100%) from spiked samples at concentrations of between 50 ng/ml and 10 micrograms/ml. Analysis of the extracts was by high performance liquid chromatography (HPLC).     

Preferential extraction of hydrocarbons from fire debris samples by solid phase microextraction

Headspace analysis by extraction/GC-MS is a common method of detecting volatile hydrocarbon accelerants in fire debris samples. Solid-phase microextraction was tested to determine if there is selective extraction of chemically distinct compounds. It was found that both the polydimethylsiloxane (PDMS) and Carboxen/PDMS solid phase microextraction fibers show preferential extraction of aliphatic or aromatic compounds from the headspace depending on fiber type and temperature. The Carboxen/PDMS fiber type showed particular (although not exclusive) selectivity for extraction of aromatic hydrocarbons. Other experimental considerations of SPME are noted.     

SPME结合衍生化检测尿液中吗啡成份

目的　建立尿液中吗啡检验的方法。方法　利用固相微萃取头富集尿液中吗啡 ,经醋酸酐衍生后进行GC/MS分析。结果　利用此方法可检测到吗啡含量为 5ug/ml的尿样。结论　该方法可用于吸毒人员尿液中吗啡的快速检验。     

Extraction of 2-nitroaniline and 2-nitro-4-methylaniline from aqueous solutions

Results of extraction of 2-nitroaniline and 2-nitro-4-methylaniline from aqueous solutions with organic solvents are shown to depend on the nature of extractants, pH of the aqueous phase, its saturation with water and electrolytes. The optimal conditions for the extraction of the compounds of interest are created by using water-saturated ethylacetate as the extractant at a pH value in the range from 1.0 to 12.0. The rate of extraction was calculated necessary to remove the desired amounts of 2-nitroaniline and 2-nitro-4-methylaniline from aqueous solutions using the above solvents.     

Extraction of 2-methyl-hydroxybenzene and 3-methyl-hydroxybenzene from water solutions

The results related with extracting 2- and 3-methyloxibenzole from water solutions by 5 hydrophobic and 2 hydrophilic organic solvents are described in the paper. A variety of factors are shown to exert influence on an extraction degree: extraction agent (EA) nature, water-phase medium pH, EA saturation with water and adding of electrolytes to the water phase. A repetition factor needed to extract the preset quantities of studied compounds is estimated.