血、尿中常见吩噻嗪类药物的高效液相色谱分析

吩噻嗪类安眠镇静药物易受光、热分解,气相色谱分析法受一定限制。而采用反相离子对液相色谱技术,使七种常见吩噻嗪类药物得到较好的分离。使用紫外及荧光分光光度计测定,可作为血、尿中此类药物的快速定性、定量分析方法之一。本法已在刑事中毒案件与临床抡救化验中应用。     

甲氰菊酯在家兔体内的死后分布研究

目的建立甲氰菊酯家兔灌胃染毒致死模型和生物检材中甲氰菊酯的气相色谱和气相色谱-质谱联用检测方法,研究甲氰菊酯在家兔体内的死后分布规律。方法家兔6只,甲氰菊酯经口灌胃染毒,死亡后迅速解剖,取心血、外周血、肝等组织,气相色谱和气相色谱-质谱联用法检测甲氰菊酯含量;部分组织经甲醛固定,HE染色,光镜观察其病理改变。结果家兔染毒后2～3h出现中毒表现,染毒后4.5～8h死亡。气相色谱和气相色谱-质谱联用法均检测到甲氰菊酯。甲氰菊酯在家兔体内死后分布为胃壁（458.92±32.82）μg/g、肾（46.47±6.30）μg/g、肝（35.79±20.11）μg/g、大脑（28.77±10.52）μg/g、心（26.49±4.10）μg/g、脾（22.23±5.37）μg/g、胆汁（10.87±1.42）μg/mL、肺（10.32±0.78）μg/g、周围血（8.14±1.12）μg/mL和心血（8.20±1.83）μg/mL。结论甲氰菊酯的灌胃染毒致死模型、气相色谱和气相色谱-质谱联用检测方法及死后分布规律可应用于甲氰菊酯中毒死亡案件的法医学鉴定及法医毒物动力学研究。     

液相色谱-串联质谱法检测生物样品中百草枯及其代谢物

目的建立生物样品中百草枯(paraquat,PQ)及其2种主要代谢物monoquat,paraquatmonopyridone(MP)的液相色谱-串联质谱(LC-MS/MS)检测方法,应用于百草枯中毒案件的法医学鉴定。方法生物样品经乙腈或甲醇沉淀蛋白,使用Agilent HILIC Plus(4.6×100mm,3.5μm)色谱柱,以0.1%甲酸水溶液～0.1%甲酸乙腈溶液(v/v)为流动相进行洗脱,在多反应监测模式下检测。结果百草枯及其代谢物在1～1000ng/mL内线性关系良好,相关系数(r)≥0.9996,最低检出限为0.34～6.00ng/mL,检测准确度为91.25%～113.44%,日内及日间精密度分别为1.51%～3.99%和1.92%～4.93%。结论本文建立的LC-MS/MS法具有灵敏度高、特异性好的特点,可应用于百草枯中毒相关案件的法医学鉴定。     

甲拌磷在大鼠体内的死后分布研究

目的建立甲拌磷灌胃染毒致死的大鼠动物模型,建立生物检材中甲拌磷的气相色谱和气相色谱质谱联用检测方法 ,观察甲拌磷在3种剂量染毒大鼠体内的死后分布特点。方法大鼠2LD50、4LD50或8LD50甲拌磷灌胃染毒,死后立即解剖,采集心、肝、脾、肺、肾、脑、肌肉、睾丸、心血和胃组织,GC/MS、GC/FPD法定性定量检测各组织和心血中甲拌磷。结果大鼠2LD50、4LD50和8LD50甲拌磷染毒后31±3min、19±4min和11±6min死亡。气相色谱和气相色谱质谱联用法均可检到甲拌磷。染毒死亡大鼠体内甲拌磷的含量由高到低顺序依次为：2LD50组：胃组织〉肝〉脾〉肾〉肺〉脑〉睾丸〉肌肉〉心〉心血。4LD50组：胃组织〉肝〉肺〉脾〉肾〉睾丸〉肌肉〉脑〉心〉心血。8LD50组：胃组织〉肝〉肾〉脾〉肺〉心〉肌肉〉睾丸〉心血〉脑。结论甲拌磷在大鼠体内死后分布不均匀。胃组织中含量最高,其次是肝、脾、肺和肾,脑、肌肉和睾丸含量最低。甲拌磷的灌胃染毒致死动物模型、气相色谱和气相色谱质谱联用方法及死后分布规律可应用于甲拌磷中毒死亡案件的法医学鉴定和法医毒物动力学研究。     

超高效液相色谱-高分辨质谱联用技术分析地芬尼多代谢产物

目的分析地芬尼多在血液中的代谢产物。方法采用高分辨液质联用仪对中毒死亡人员血液进行检测,样品经乙腈沉淀蛋白后使用液相色谱-高分辨质谱联用仪检验,根据高分辨的质谱碎片信息和解析软件分析其结构。结果经过仪器检测和数据分析,推断出血液中三种地芬尼多的代谢产物。结论该方法为地芬尼多中毒案件判定和代谢产物检验提供了新的参考。     

HPLC-MS/MS法快速检测人体血液中的夹竹桃毒素

目的采用高效液相色谱-串联质谱法(HPLC-MS/MS)检测人体血液中夹竹桃苷、夹竹桃苷乙。方法采用乙腈沉淀蛋白法处理血液,HPLC-MS/MS法检测,采用MRM记录方式,保留时间和定性离子对定性,标准曲线法定量。结果夹竹桃苷、夹竹桃苷乙的检测限均在0.5ng/m L,线性范围在1ng/m L~1mg/m L,回收率为75.2%~95.7%。结论本方法操作简便,灵敏度高,可应用于中毒案件中人体血液中两种夹竹桃毒素(夹竹桃苷和夹竹桃苷乙)的快速检测。     

SPE-HPLC/MS/MS检验体液中赛拉嗪及DMA

目的建立了一种高效液相色谱串联三重四极杆质谱同时测定体液中赛拉嗪及2,6-二甲基苯胺的分析方法。方法样品经HLB固相萃取柱提取净化,Waters Atlantis d C18色谱柱分离,正电离条件下进行选择监视扫描模式检测。结果方法的回收率为70.5%~79.8%,RSD为8.2%~10.5%。赛拉嗪及2,6-二甲基苯胺在血液和尿液中的检出限分别为0.4 ng/mL和0.3 ng/mL,定量限分别为1.2 ng/mL和1.0 ng/mL。结论本方法灵敏度高、特异性好、重现性好,适用于赛拉嗪中毒的血液和尿液检测。     

超高效液相色谱-质谱法测定人全血中甲胺磷、乙酰甲胺磷含量

目的应用超高效液相色谱-质谱法(UPLC-MS/MS)对人全血中甲胺磷、乙酰甲胺磷进行定量测定。方法采用去离子水直接稀释人全血,提取血中的甲胺磷及乙酰甲胺磷,以甲醇-水(含0.1%甲酸)为流动相梯度洗脱,正离子化多反应监测(MRM)模式测定。结果甲胺磷、乙酰甲胺磷的回收率均高于87%。在选定条件下全血中甲胺磷、乙酰甲胺磷的线性范围为2～200ng/ml,最小定量限为2ng/ml。结论将全血样品进行直接稀释并应用液相色谱-质谱法进行检测可作为甲胺磷及乙酰甲胺磷中毒的快速检测方法。     

UPLC-MS/MS测定人血中15种有机磷农药

目的 建立超高效液相色谱-串联质谱法（UPLC-MS/MS）测定人血中15种有机磷农药的分析方法。方法 血液样品经乙腈沉淀蛋白,采用Waters ACQUITY UPLC HSS T3(2.1 mm×100 mm×1.8μm)色谱柱进行分离,以甲醇/水体系进行梯度洗脱,流速0.35 mL/min。以电喷雾离子源正离子（ESI+）和多反应监测（MRM）模式进行检测,内标法定量。结果 在优化的仪器条件下,15种有机磷农药均能有效检出,且分离良好。在所测质量浓度范围内,15种有机磷农药均呈现良好的线性关系,相关系数r均> 0.99,加标回收率为80.1%～117.9%,相对标准偏差（RSD）为0.36%～9.06%。结论 该方法选择性强、精密度高、重现性好,能同时检测人血中15种有机磷农药成分,可有效应用于有机磷农药中毒的快速筛查和中毒案（事）件的法医学鉴定。     

生物检材中F^-的离子色谱检出法

采用低压离子色谱从生物检材中检出F~-,克服了氟乙酰胺中毒案件检验中,因氟乙酰胺性质不稳定,易分解变为氟化物而难以用GC,CC/MS,TLC等方法检出的缺点,同时该方法也适用于氟化物中毒的检验。     

用快速高效液相色谱系统分离纯化Gc蛋白

报告Gc蛋白的一种分离方法，为免疫制备抗Gc血清制备抗原。硫酸该分级沉淀出含Gc的人血清组份，BlueSepharoseCL－6B亲和色谱除去含Gc硫酸铸分级沉淀的人血清组份中的白蛋白，快速高效液相色谱系统过Alkyl-SuperoseTMHR5／5疏水色谱柱和MonoQHR5／5离子交换柱。聚丙烯酸胺凝胶解离、非解离电泳证明，Gc蛋白得到了彻底纯化。免疫固定显示：纯化出的蛋白确实是Gc蛋白．为1-1型。快速高效液相色谱为蛋白质的纯化提供了新的技术及仪器手段。     

Analysis of lipsticks

A combination of thin-layer and gas chromatography has been shown to be suitable for the analysis, characterisation and discrimination of the small quantities of lipsticks which may be encountered in forensic casework.     

中毒家兔血清中地芬尼多检测研究

采用气相色谱法分析了中毒家兔血清中地芬尼多浓度的经时变化，研究了其毒代动力学过程，测定了尿、胆汁中地芬尼多的含量。     

A Comparison of Common Swabbing Materials for the Recovery of Organic and Inorganic Explosive Residues

The efficiency of solvent based extraction methods used to remove explosive residues from four different swab types was investigated. Known amounts of organic and inorganic residues were spiked onto a swab surface with acetonitrile or ethanol:water combined with ultrasonication or physical manipulation used to extract the residues from each swab. The efficiency of each procedure was then calculated using liquid chromatography‐ultraviolet detection for organic residues and ion chromatography for inorganic residues. Results indicated that acetonitrile combined with physical agitation proved to be the most efficient method; returning analyte recoveries c. 95% for both alcohol based swabs and cotton balls. Inorganic residues were efficiently extracted using ethanol:water, while the use of acetonitrile followed by water significantly reduced the recovery of inorganic residues. Swab storage conditions were then investigated with results indicating decreased storage temperatures are required to retain the more volatile explosives.     

离子交换柱法萃取血样中4种巴比妥类药物

目的建立血样中4种常见巴比妥类药物的固相萃取方法。方法采用Oasis MAX固相萃取柱对样品进行预处理,以2%氨水淋洗2,%甲酸-甲醇洗脱,GC/NPD定量检验,GC/MS定性检验。结果血样中4种常见巴比妥类药物平均萃取回收率达80%以上,以信噪比10/1计,最小定量限为1～2μg/mL,以信噪比3/1计,检出限为0.5～1μg/mL,在1～50μg/mL范围内,线性相关系数均在0.99以上。结论本文固相萃取方法检出限低,回收率高,选择性强,可应用于血样中4种常见巴比妥类药物的检测。     

大麻概况及其气相分析方法综述

随着大麻走私的日益猖獗,对大麻进行快速准确的定性定量分析,为司法部门量刑提供准确可靠的依据显得尤为重要。本文对大麻的化学成分、检材种类、滥用方式进行介绍,并对气相色谱分析方法中涉及的检材提取方法、内标物、色谱柱和质谱图等进行综述。     

自含墨印章印文盖印时间受老化条件的影响

目的探索利用气相色谱法较精确、定量测定自含墨印章印文盖印时间受人为老化条件的影响。方法分别在恒温烘烤、紫外线照射、纯水浸泡等人为老化条件下,测定自含墨印章印油中所含有的主要相关溶剂成份的含量变化。结果得出了主要溶剂成份在人为老化条件下其含量的变化规律以及人为老化与自然老化的对应关系。结论利用气相色谱法可以对不同保存条件下自含墨印章印文的盖印时间进行测定,为实际相关案件的检验提供了依据。     

固相萃取-气相色谱法检测生物检材中斑蝥素

目的建立固相萃取-气相色谱法检测生物检材中斑蝥素的方法。方法采用HLB固相萃取柱提取,气相色谱-内标法检测。结果斑蝥素在0.1～200mg/L范围内呈良好的线性关系,相关系数为0.999以上;精密度（RSD）小于5%。对于添加血样,方法检出限为0.05μg/mL,加标回收率范围为93.03%～98.29%。结论该方法操作简便、快速、灵敏,提取回收率高,提取物含杂质较少,可用于实际案件中全血和尿样中斑蝥素的检测。     

The Quantitation of Cocaine on U.S. Currency: Survey and Significance of the Levels of Contamination

It has long been suspected that the illicit distribution of cocaine in the United States has led to a large‐scale contamination of the currency supply. To investigate the extent of contamination, 418 currency samples (4174 bills) were collected from 90 locations around the United States from 1993 to 2009. The extent of their cocaine contamination was quantitated via gas chromatography/mass spectrometry or liquid chromatography/mass spectrometry. The level of cocaine contamination was determined to average 2.34 ng/bill across all denominations ($1, $5, $10, $20, $50, and $100). Levels of cocaine contamination on currency submitted to the Federal Bureau of Investigation Laboratory in criminal cases over the 1993–2001 timeframe had significantly higher contamination than currency in general circulation. A mathematical model was developed based on the background survey that indicates the likelihood of drawing a bill in specific concentration ranges. For example, there is a 0.8349 likelihood that random bill will have contamination less than 20 ng.     

Analysis of pain management drugs, specifically fentanyl, in hair: application to forensic specimens

This article discusses the immunoassay screening of pain management drugs, and the mass spectrometric confirmation of fentanyl in human hair. Hair specimens were screened for fentanyl, opiates (including oxycodone), tramadol, propoxyphene, carisoprodol, methadone, and benzodiazepines and any positive results were confirmed using gas chromatography or liquid chromatography with mass spectral detection. The specific focus of the work was the determination of fentanyl in hair, since autopsy specimens were also available for comparison with hair concentrations. Using two-dimensional gas chromatography with electron impact mass spectrometric detection, fentanyl was confirmed in four of nine hair specimens collected at autopsy. The accuracy of the assay at 10 pg/mg was 95.17% and the inter-day and intra-day precision was 5.04 and 13.24%, respectively (n=5). The assay was linear over the range 5-200 pg/mg with a correlation of r(2)>0.99. The equation of the calibration curve forced through the origin was y=0.0053x and the limit of quantitation of the assay was 5 pg/mg. The fentanyl concentrations detected were 12, 17, 490, and 1930 pg/mg and the results were compared with toxicology from routine post-mortem analysis. The screening of pain management drugs in hair is useful in cases where other matrices may not be available, and in routine testing of hair for abused drugs.