The chromatographic analysis of phencyclidine, its metabolites and analogs in biological fluids

Reviews data on analysis of narcotic phencyclidine and its main metabolites and analogs. Pharmacological and toxic characteristics of phencyclidine, conditions of its isolation from biological objects and its detection and measurement by thin layer and gas chromatography and by chromatographic mass-spectrometry are described. Analysis of phencyclidine metabolites is discussed and a scheme of its metabolism is presented. Statistical characteristics of methods of quantitative analysis of phencyclidine in biological objects are presented.     

体液中常见滥用药物的系统筛选分析

本文建立了体液中常见滥用药物的筛选分析体系.尿液或血液经固相萃取(SPE)或液提取(LLE)后,直接用GC/NPD分析或经TFA、BSTFA衍生化后用GC/MS分析.方法适用于同时分析甲基苯丙胺、MDMA、度冷丁、去甲度冷丁、曲马多、美沙酮、EDDP、可卡因、苯甲酰芽子碱、可待因、安定、氯丙嗪、吗啡、单乙酰吗啡等十四种常见滥用药物及代谢物.SPE法和LLE法回收率分别为66～102%和50～86%,最低检出限为2-5ng/ml尿.涉毒案件的鉴定应用表明该分析方法简便、快速、可靠.     

GC/MS研究海洛因代谢物在吸毒者体内的分布

应用GC／MS－SIM测定了海洛因代谢物吗啡在两例海洛因延缓死亡者的体内分布,并分析了收集到的7例案子的毛发（头发、腋毛和阴毛）中6-单乙酰吗啡和吗啡含量。生物检材和毛发经酸水解、提取、醋酸酐或双（三甲基硅基）三氟乙酰胺（BSTFA）衍生化,然后进行GC／MS-SIM分析。结果表明尿、胆汁和肝脏是判定死者是否曾使用海洛因的最佳检材;毛发分析与生物检材相比有其独特的优点,可提供数月甚至数年的用药情况。为公安司法机关打击吸毒、惩治犯罪提供更可靠、有效的证据。     

Detection of dipiridamol in biological fluids

Acetone is proposed as an isolating agent for dipiridamol isolation from biological fluids. Purification of the isolates was performed with liquid-liquid extraction and colon chromatography with silasorb C-18 sorbent. The technique of dipiridamol detection in the blood and urine is described. The assays results are presented.     

Detection of furadan in biological fluids

Optimal conditions have been determined for furadan isolation from biological fluids by means of the mixture of solvents ethyl acetate-acetone in volume 1:1. Possible purification of the compound from coextractive substances of biomaterial on the column with silica gel L 100/160 mcm is demonstrated. IR-spectrophotometric methods and high performace liquid chromatography with a detector of photodiode matrix are proposed for identification and quantitation of furadan in blood and urine specimens.     

The detection of nifedipine in biological materials

The objective of the present study was to find optimal conditions for the isolation of nifedipine from biological materials by ethylacetate. It was shown that nifedipine can be purified from co-extracted substances of the biological material on a Silasorb C-18 column with the size of the particles 30 microns. The authors propose to use thin-layer chromatography, IR spectrophotometry, and reverse-phase high performance liquid chromatography for the identification and quantitative determination of nifedipine extracted from cadaveric liver samples.     

A simple, rapid 125I radioimmunoassay for the detection of barbiturates in biological fluids.

A simple, rapid radioimmunoassay employing 125-I-labeled secobarbital derivative has been developed and has been shown to be capable of detecting at the nanogram level a variety of barbiturates in urine as well as in plasma.     

体液中微量士的宁的富集及同时检测

目的将分子印迹技术运用到法医毒物分析中,建立一种全新的测定体液中微量士的宁的方法。方法运用分子印迹原位聚合技术,在色谱柱中一步合成了对士的宁具有专属识别能力的分子印迹聚合物,以此聚合物为介质,装填一厘米的小柱,建立体液中微量士的宁的富集及同时检测方法。结果以士的宁分子印迹聚合物作为尿液和血浆中微量士的宁的富集和检测介质,方法的检出限为4.9ng,样品回收率均大于92%,相对标准偏差小于6.59%,工作曲线的线性相关系数分别为0.9991和0.9966。运用此方法对中毒家兔血浆和尿液中的士的宁进行了测定。结论建立的新方法可以实现对士的宁专属的、灵敏的检测,适合于法医学毒物分析运用。     

生物检材中氯胺酮及其代谢物的检测

近年来氯胺酮的滥用越来越普遍,建立快速、准确的检测方法越来越重要。氯胺酮在生物体内的代谢物主要有去甲氯胺酮、脱氢去甲氯胺酮等。目前,常用的生物检材有血液、尿液、毛发等。常用的检测方法有气相色谱法、气相色谱-质谱联用法、高效液相色谱法、液相色谱-质谱联用法、高效毛细管电泳法等。本文参考近年来的相关文献对生物检材中氯胺酮及其代谢物的检测方法作一综述,为法医毒物分析等相关领域提供参考。     

The characteristic morphological changes of the internal organs in certain forms of combined poisoning

The results of forensic medical investigations of 100 corpses of the persons who died from combined intoxication with two and more poisons are presented. They were compared with clinical observations and summarized uisng the methods of tanatogenetic analysis. The main variants of fatal combined poisoning and the underlying tanatogenetic mechanisms were categorized into cardiac (disturbances of rhythm and conductivity, progressive hypotension, flabby heart muscle, extensive fragmentation of cardiomyocytes), cerebral (coma and massive death of brainstem neurons), and pulmonary (of pneumonia- or pulmonary oedema-type with fibrin precipitation in the alveoli and formation of hyaline membranes). This classification was supplemented by a variety of combinations of the above variants with necrotic nephrosis and disseminated intravascular coagulation syndrome. It is concluded that the results of this study may be of use for forensic medical diagnostics of combined poisoning and the elucidation of the contribution of individual toxic substances to the fatal outcome bearing in mind the low informative value of the relevant forensic medical data.     

The application of chromatography and spectrometry for the analysis of ketorolac and diclofenac in biological fluids

The objective of the present work was to study conditions for isolation of ketorolac and diclofenac from biological fluids. A method of their extraction with a mixture of organic solvents has been developed and the conditions for the identification of these compounds are proposed with the use of high performance liquid chromatography (HPLC), UV spectroscopy, and gas chromatography with electron capture detection (GC/ECD). The possibilities of using HPLC, UV spectrometry, and GC/ECD for quantitative determination of ketorolac and diclofenac are illustrated.     

SPE-HPLC/MS/MS法检测人唾液中地西泮及其代谢物

目的采用固相萃取-高效液相色谱-串联质谱法(SPE-HPLC/MS/MS)检测人唾液中地西泮及其代谢物。方法采用固相萃取法(SPE)处理唾液,HPLC/MS/MS法检测,MRM记录方式,保留时间和定性离子对定性,内标法和标准曲线法定量。结果地西泮及其代谢物去甲地西泮、去甲羟基西泮、去甲羟基地西泮葡萄糖醛酸苷(OG)、羟基地西泮葡萄糖醛酸苷(TG)的检测限在0.01ng/m L~0.5ng/m L之间,线性范围0.1ng/m L或0.5ng/m L~100ng/m L,回收率为84.9%~106%。口服5mg地西泮后15d内唾液中可检出地西泮及去甲西泮,但检出时间有个体差异,但去甲羟基西泮、TG和OG则不能检出。结论 SPE-HPLC/MS/MS检测法可应用于人唾液中地西泮及其代谢物的检测。人口服常量地西泮后唾液中可检出地西泮和去甲西泮,且检测窗口期较宽,但存在个体差异。     

Immunochemical methods in detection of opiates in tissues and organs

Conditions of isolation of opiates from tissues and analysis of the resultant extracts by immunochemical methods are discussed. The main characteristics of OPIATES U kits (Pharmatech) for polarization fluorescent immunoanalysis of cadaveric material (liver) are determined. Immunochemical methods for forensic chemical analysis for opiates are experimentally compared.     

The detection of abortion agents in biological material]

Methods of extraction and detection of ascorbic acid, ergot alkaloids, cotarnine, microfollin, tinctures of marigold, peony, sage-brush, iodine, benzestrol, pachycarpine, hexestrol, folliculin, quinine, ethoxydiaminoacridine lactate were developed. Detection limits are 0.1-1 mg/100 g of object. Methods of manganese, iodine and soap detection are developed. Detection limits are 0.05-2 mg/100 g of object.     

The detection of aromatic substances in biological material]

The author presents experimental data and suggests a method for extraction of aromatic substances from the blood, urine, lavage water, stomach and its contents, liver and kidneys. The extract is dissolved in 96% ethanol and the aromatic substances are detected in reactions with hydrochloric acid, Marki's reagent, 2,4-dinitrophenylhydrazine, diazotized o-dianisidine, phthivazide, chromotropic acid by UV spectrophotometry, thin-layer and gas-liquid chromatography. The sensitivity of the method is 0.1-0.5 mg %.