生物样品中真菌毒素及其代谢物检测研究进展

真菌毒素是由植物病原真菌在适宜条件下产生的次生代谢物,广泛分布于粮食等农作物中,具有较强的化学稳定性和毒性。在实际案件中,生物样品中真菌毒素检测可以为司法审判提供更直接的证据,因此检测生物样品中真菌毒素已成为研究的重点。本文介绍了生物样品中常见真菌毒素及其代谢物,总结了液液萃取法、固相萃取法、沉淀蛋白法等前处理方法,综述了免疫法、荧光法、气质联用技术以及液质联用技术等检测方法,通过对生物样品中真菌毒素及其代谢物检测的前景进行展望,以期为法庭科学领域中真菌毒素的检测提供参考。     

人唾液中苯丙胺类药物检测方法进展

目前人唾液中苯丙胺类药物的检测研究较少,鉴于唾液检材具备很多的实用价值和优势,本文综述了国内外对唾液检材中苯丙胺类药物的检测研究进展,重点包括免疫分析筛选方法、液-液萃取法、固相微萃取法等萃取方法以及气相色谱/质谱联用法、液相色谱/质谱联用法等确证方法的发展情况。     

氟乐灵的检验

目的建立氟乐灵的提取方法和检验方法。方法用液-液萃取法、固相萃取法提取生物检材中氟乐灵,然后用气相色谱法及薄层色谱法进行分析。结果氟乐灵在强酸性条件下提取率最高,在乙醚和苯溶剂中提取率较高,并且用混合溶剂提取优于单一溶剂提取。固相萃取的优越性不明显,而液-液萃取法显得更简单、快速。结论所建立的方法快速准确,效果良好。     

反相固相萃取技术及其在毒物分析中的应用

一、前言在毒物分析工作中,尤其使广大分析工作者感到困难的一个问题是:生物样品的预处理。传统使用是液(?)液萃取法。进入八十年代后,随着色谱技术和固相填料的进一步发展和完善,出现了一种生物样品处理新厅法.即固相萃取技术(Solid Phase Extrac-     

固相萃取法在苯丙胺类药物提取中的应用

目的建立生物检材中苯丙胺类药物的定性定量分析方法;方法应用固相萃取法提取生物检材中苯丙胺类药物,比较了苯丙胺类药物固相萃取的最佳pH值、固相吸附柱等提取条件,比较了固相萃取法和传统的液液萃取法在提取回收率、净化效果等方面的特点;结果生物检材中苯丙胺类药物固相萃取pH11时效果最好,提取回收率达82.9%～93.2%;结论该方法实用,提取率高,杂质干扰少。     

快速溶剂萃取气相色谱法测定血尿中苯并二氮杂类药物

苯并二氮杂革类药物是临床应用较为广泛的抗焦虑、抗癫痫及催眠药物,常见于成瘾滥用、麻醉犯罪以及过量服用,故血、尿等体液中该类药物其及代谢物的检测在司法鉴定中具有重要的意义。血、尿中该类药物和代谢物的筛选分析方法一般都采用液液萃取法、固相萃取法、固相微萃取法等。     

固相萃取-GC/NPD法分析水中的毒鼠强

利用C18固相小柱萃取,咖啡因作内标,GC/NPD法分析水中的毒鼠强,方法简便、快速、灵敏、回收率高.检测限为O.25ng/μl,水样中毒鼠强回收率为84.12%,定量结果与用苯直接液液萃取法相近.     

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。     

尿液中几种碱性麻醉药物的检验

本文介绍了一种用 Sep-Pak C_(18)小柱,液-固萃取法提取尿液中几种碱性麻醉药物,以大口径毛细管气相色谱-氢火焰离子化检测器检验的方法。操作过程简单、迅速,各药物回收率高。     

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。     

Blowfly Larval Tissues as a Secondary Detector for Determining Paraquat-Related Death in Rabbit Carcass

Paraquat poisoning is commonly associated with suicide or homicide in Malaysia. In a case involving advanced body decomposition, pathological analysis regarding the cause of death may become difficult or almost impossible. Insects serve as common alternative matrix for poison detection in forensic analysis. Paraquat detection via secondary bioaccumulation in fly larvae tissue has never been reported. In this study, tissues from blowfly larvae collected from a rabbit carcass with paraquat poisoning were analyzed for secondary bioaccumulation. Larvae samples were collected and analyzed using liquid–liquid extraction. The detection was performed via reduction of quaternary ammonium presence in paraquat and analyzed using gas chromatography–mass spectrometry (GC-MS) with selected ion monitoring mode (SIM mode). GC-MS showed the elution of reduced paraquat was at retention time 12.8 min. Blowfly larvae tissue has proven useful as a secondary detector in paraquat-related deaths.     

The analysis of quaternary ammonium compounds in human urine by direct inlet electron impact ionization mass spectrometry.

An accurate and rapid screening test for nine quaternary ammonium compounds (suxamethonium chloride, pancuronium bromide, ambenonium chloride, benzethonium chloride, distigmine bromide, methylbenactyzium bromide, neostigmine bromide, propantheline bromide and pyridostigmine bromide) by direct inlet electron impact ionization mass spectrometry (DI/EI-MS) was investigated. Each compound was extracted from urine as an ion pair with KI3 into dichloromethane. The reliability of the identification of these compounds was verified by the mass chromatographic analysis of their characteristic fragment ions. The analysis of these drugs by DI/EI-MS could be performed within 5 min. The detection limits were between 20-150 ng/ml for the nine compounds. This method appears to be efficient, rapid and suitable as a screening procedure for the quaternary ammonium compounds found in urine.     

GC／MS检测尿中4种苯氧羧酸类除草剂

目的建立尿中2，4-D、2，4-DP、MCPA、MCPP等4种苯氧羧酸类除草剂的分析方法；方法液液提取分离，乙醚为提取液，DCPA为内标，硫酸正丁醇酯化衍生化，气质联用分析法分析；结果尿中4种除草剂添加样品的相对回收率在80％以上，检测限都在5ng／ml以下，对中毒兔尿样进行了分析；结论对实际发生的中毒案件分析有足够的灵敏度。     

不同消毒方式对现场DNA检出影响研究

目的探讨新型冠状病毒敏感的消毒方式对于常见现场生物物证如血、脱落细胞的检出影响,探索在疫情期间现场勘查、实验室检验及尸体解剖前后的合理消毒方式。方法采用《消毒剂使用指南》推荐的几种不同浓度化学消毒剂和紫外线照射等方式,对常量的血、口腔拭子和稀释的血、唾液斑进行作用后的样本DNA检出情况进行对比。结果常用消毒方式对常量血样本影响不大,大功率紫外线照射对脱落细胞有一定影响。稀释后的血、唾液斑样本75%乙醇、二氧化氯、单链季铵盐、复合季铵盐、过氧乙酸、对氯间二苯酚均正常检出,高浓度含氯消毒液、2%戊二醛和长时间紫外线照射影响较大。结论科学指导疫情期间在现场勘查和实验室等场所合理选择消毒方式对不同客体进行消毒和排除DNA污染。     

Comparison of extraction methods for methamphetamine and its metabolites in tissue

Five extraction methods were examined for analysis of methamphetamine and its major metabolites in tissue samples. The extraction methods studied were an acetone extraction method, an ethanol extraction method, an ammonium sulfate method, dialysis, and a direct solvent extraction. Acetone, ethanol, and dialysis methods showed no interference from endogenous components using thin-layer chromatography and gas chromatography, and gave satisfactory recovery of methamphetamine, amphetamine, and p-hydroxymethamphetamine when added to rabbit liver. These methods, however, proved time-consuming. The ammonium sulfate method and direct solvent extraction method were simple and more rapid, but recovery of the polar metabolite was poor.     

UPLC-MS/MS法同时检测全血中16种除草剂

目的建立全血中16种除草剂的超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测方法,为除草剂中毒案事件及其他刑事案件血液中该16种除草剂的检验鉴定提供依据。方法取200μL的血液,加入800μL乙腈-水(体积比80/20),进行蛋白沉淀后,采用Acquity BEH C18(2.1mm×100mm,1.7μm)色谱柱,以水(5mmol/L的甲酸铵,0.1%的甲酸)-乙腈为流动相进行梯度洗脱,采用电喷雾离子源(ESI)、多反应监测(MRM)正离子模式对16种化合物进行检测。结果在1~200ng/mL范围内线性关系良好,R2均大于0.996;基质效应(ME%)为85.2%~104.4%,相对标准偏差(RSD%)为0.72%~4.84%;仪器检出限(IDLs)为0.2~2 ng/mL(信噪比S/N≥3),方法检出限(MDLs)为0.5~3ng/mL(信噪比S/N≥3),最低定量限(LOQs)为1~7ng/mL(信噪比S/N≥10)。结论本实验建立的全血中16种除草剂同时检验方法,前处理简便快捷、回收率高、精密度好、方法检出限低,可作为该16种除草剂中(投)毒案件的检验方法。     

Halogenated solvent interactions with N,N-dimethyltryptamine: formation of quaternary ammonium salts and their artificially induced rearrangements during analysis

The psychoactive properties of N,N-dimethyltryptamine (DMT) 1a are known to induce altered states of consciousness in humans. This particular attribute attracts great interest from a variety of scientific and also clandestine communities. Our recent research has confirmed that DMT reacts with dichloromethane (DCM), either as a result of work-up or storage to give a quaternary N-chloromethyl ammonium salt 2a. Furthermore, this was observed to undergo rearrangement during analysis using gas chromatography-mass spectrometry (GC-MS) with products including 3-(2-chloroethyl)indole 3 and 2-methyltetrahydro-beta-carboline 4 (2-Me-THBC). This study further investigates this so far unexplored area of solvent interactions by the exposure of DMT to other halogenated solvents including dibromomethane and 1,2-dichloroethane (DCE). The N-bromomethyl- and N-chloroethyl quaternary ammonium derivatives were subsequently characterised by ion trap GC-MS in electron and chemical ionisation tandem MS mode and by NMR spectroscopy. The DCE-derived derivative formed at least six rearrangement products in the total ion chromatogram. Identification of mass spectrometry generated by-products was verified by conventional or microwave-accelerated synthesis. The use of deuterated DCM and deuterated DMT 1b provided insights into the mechanism of the rearrangements. The presence of potentially characteristic marker molecules may allow the identification of solvents used during the manufacture of controlled substances, which is often neglected since these are considered inert.     

Optimization of the conditions for extracting metronidazole with organic solvents]

Optimal conditions of metronidazole extraction from aqueous solutions by different solvents using a mathematical method of experiment planning (latin square) were studied. It was stated that optimal conditions of metronidazole extraction from aqueous solutions were: extraction time (5 min.), pH medium-6, extractant-isoamyl spirit in saturation of aqueous phase with ammonium sulfate.     

GC/MS、GC/NPD法检测血液中氯胺酮

目的利用GC/MS、GC/NPD与固相萃取（SPE）技术相结合,建立血液中氯胺酮的定性定量分析方法。方法选择4-苯基丁胺为内标,采用Bond-Elut Certify固相柱萃取、二氯甲烷：异丙醇：氨水（78∶20∶2,v/v/v）洗脱的固相萃取分离技术,比较不同pH体系、洗脱溶剂对回收率的影响,建立血液中氯胺酮的GC/MS、GC/NPD定性定量分析方法。结果以GC/NPD分析氯胺酮在6.0～5000ng/mL范围内线性关系良好,GC/MS-Scan定性检测限为20.0ng/mL。方法平均回收率达96.9%,标准偏差小于5%。结论此方法可满足氯胺酮毒品滥用者血液定性定量分析。     

SPE—GC／MS、GC／NPD法检测血液中苯丙胺类毒品

目的利用GC／MS、GC／NPD与固相萃取（SPE）技术相结合,建立血液中苯丙胺类毒品的定性定量分析方法。方法采用Bond—ElutCerti{y固相柱、甲醇淋洗、二氯甲烷／异丙醇／氨水（78／20／2）洗脱固相萃取分离提取,比较了不同PH体系、稀释状态、洗脱溶剂对提取回收率的影响,建立血液中苯丙胺类毒品的GC／MS、GC／NPD定性定量分析方法。结果以GC／NPD分析AM、MA、MDA和MDMA浓度在15ng／mL-2000ng／mL、10ng／mL～1600ng／mL、20ng／mL-3000ng／ml、20ng／mL-3000ng／mL范围内线性关系良好,AM、MA、MDA和MDMA的检测限分别为10ng／mL、8ng／mL、15ng／mL、15ng／mL,方法平均回收率大于85％,标准偏差小于5％,GC／MS-Scan检测限分别为40ng／mL、32．0ng／mL、60．0ng／mL、60．0ng／mL。结论此方法可满足苯丙胺类毒品滥用者的血液定性定量分析。