Determination of a newly encountered designer drug "p-methoxyethylamphetamine" and its metabolites in human urine and blood

A newly synthesized designer drug, para-methoxyethylamphetamine (PMEA) was unexpectedly detected in the postmortem specimens of fatality involving drug intoxication in 2005, Japan. For unequivocal identification, the isomeric discrimination of PMEA and its positional-isomers was performed by GC/MS with the trifluoroacetylation. In order to prove the intake of PMEA, the characteristic metabolites of PMEA were also identified by GC/MS analysis of the urine specimen with trifluoroacetylation. As a result, para-methoxyamphetamine, para-hydroxyethylamphetamine (POHEA) and para-hydroxyamphetamine were identified as the major metabolites of PMEA. For the quantitative analyses of PMEA and its three metabolites in body fluids, an automated column-switching LC/MS procedure was developed, and applied to the postmortem blood and urine specimens. In this fatal case, blood concentration of PMEA was estimated to be 12.2 microg/mL and this level seemed extremely high in comparison with lethal blood-levels of its analogues, representing acute-intoxication of the victim. Based on the quantitative results, PMEA was found to be extensively metabolized to POHEA via O-demethylation, partly followed by its conjugation.     

Detection and quantification of low levels of benzoylecgonine in equine urine

Cocaine (COC) is a highly addictive plant alkaloid expressing strong psychostimulatory effect. It has no medical use in equine veterinary practice. The contamination of the environment with cocaine such as its presence on the US paper currency has been reported few times. There are anecdotal reports of low benzoylecgonine (BE) concentrations (usually much less than 100 ng/mL) being found in urine of race horses. In order to protect horsemen against harsh penalties associated with the presence of trace amounts of BE in horse urine as a result of environmental contamination, in February 2005 the Illinois Racing Board issued new medication rules that established the threshold level of 150 ng/mL for BE in equine urine. The penalties associated with this rule provide for increasing fines ($250, $500, $1000) with successive positive reports against a trainer for levels of BE below 150 ng/mL. A total of 19,315 urine samples were collected over the 2-year period of time from winning horses (both harness and thoroughbred) at race tracks in Illinois for routine drug screening (ELISA). The presence of BE was confirmed by GC/MS in 28 urine samples (0.14%). The concentration range for BE in harness horses (21 detections) was < 5-91 ng/mL, and for thoroughbred (seven detections) was 7-52 ng/mL. To date, the laboratory has not reported concentrations of BE that exceed the established threshold concentration of 150 ng/mL.     

GC—MS／MS法检验生物检材中的无机氰化物

目的建立一种检验生物检材中无机氰化物的GCMS／MS方法。方法首先将生物检材中的无机氰化物在酸性条件下蒸馏出,用碱性溶液吸收后,氰离子在相转移催化剂作用下被五氟苄基溴（PFB-Br）衍生化,最后用GC-MS／MS法分析衍生化产物。结果衍生化产物PFB-CN的MS／MS质谱图特征性强,定性准确;在20-1500ng／g浓度范围内呈良好的线性关系（r＝0．998）,最低检测限为5ng／g,回收率为82．3％－98．6％。结论本方法简单实用,灵敏度高,准确可靠,适用于生物检材中无机氰化物的检验。     

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。     

快速溶剂萃取-GC／MS法测定全血中沙蚕毒素

目的采用快速溶剂萃取-GC／MS分析方法检验血液中杀虫双代谢产物沙蚕毒素。方法样本用硅藻土、中性三氧化二铝处理，用乙酸乙酯：环己烷：丙酮（2：2：1）进行萃取，GC／MS方法进行测定，并考察实验最佳条件。结果沙蚕毒素在50～2000ng／mL范围内线性关系良好，相关系数为0．999，检测限为15ng／mL，平均回收率为98．22％，相对标准偏差为4．6％。结论速溶剂萃取-GC／MS分析方法简便，快速，准确、灵敏度高，可在血中沙蚕毒素检验中选用。     

水胺硫磷中毒气相色谱/质谱检验

用GC/MS检验水胺硫磷,由于水胺硫磷热稳定性差,且质谱谱库无水胺硫磷的结构,笔者用质谱离子碎片峰解析,确认了水胺硫磷.     

利用GC／MS分析尿中的安全分解产物

用气相色谱/质谱联用方法在一起死亡案中检验出安定的分解产物,并确定了分解产物的结构.     

毛细管气相色谱柱的保养与维护

综述了毛细管气相色谱柱的保养与维护.就毛细管柱分析使用中常遇到的一些问题,例如如何避免色谱柱的断裂,固定相的损伤,色谱柱的污染以及如何解决一些不能避免的问题和应采取的措施、步骤.     

生物样品中曲马多的分离和鉴定

简要地介绍了曲马多的药理性质和在生物样品中的分离方法,给出了其在GC和TLC法中的分析数据,所介绍的方法具有操作简单回收率高等优点.     

杀虫双的检验和质谱解析

本文用气相色谱/质谱联用方法检验杀虫双,并解析杀虫双的质谱图.