体内磷化氢的定量测定——用次亚磷酸钠为标准品的定量方法

本文作者提出用次亚磷酸钠为标准品,作体内磷化氢的定量测定。探讨了采用气相色谱法、硝酸银比色法及AgDDC分光光度法定量测定体内磷化氢的条件及其线性范围。作者认为,此法有两个优点:一是可避免将磷化氢氧化成磷酸根的繁琐操作;二是简化了定量方法。     

反相高效液相色谱法同时测定人血清中氯丙嗪与氯扎平的浓度

作者建立了同时测定人血清中氯丙嗪与氯扎平浓度的反相高效液相色谱(RP—HPLC)法。以利眠宁为内标,用环己烷—乙醚(1:1)混合溶剂提取血清中氯丙嗪和氯扎平。高浓度中毒者血清(>1ug/ml)则用乙腈沉淀后直接进行色谱测定。血清中氯丙嗪、氯扎平的方法回收率乎均各为98.5±4.0(SD)%,CV4.2%;99.9±4.1(SD)%,CV4.1%。两药在血清中的最低检测浓度为10ng/ml。本法应用于临床氯丙嗪、氯扎平合用药物的血浓度监测及司法中毒案例的分析,结果满意。     

An evaluation of matching unknown writing inks with the United States International Ink Library

Utilizing a database of standards for forensic casework is a valuable resource. Undoubtedly, as more standards (and corresponding information about the specimens) are collected, there is a greater certainty of identification when a questioned and a known item cannot be distinguished after a series of analyses. The United States Secret Service and the Internal Revenue Service National Forensic Laboratory jointly maintain the largest known forensic collection of writing inks in the world, which is comprised of over 8500 ink standards collected worldwide, dating back to the 1920s. This study was conducted to evaluate the reliability of matching arbitrarily purchased pens with known inks from a database. One hundred pens were randomly obtained from a variety of sources and their respective ink compositions were compared with standards. Eighty-five of the inks were determined to be suitable for comparison utilizing optical examinations and thin-layer chromatography. Three of the inks did not match any of the specimens on record; one of these inks was similar to an ink from an identical brand of pen that was in the database, but had a modified formulation.     

用固相萃取法提取净化生物检材中拟除虫菊酯类杀虫剂的实验研究

固相萃取法（Sep－PakC18小柱）同时萃取净化生物检材（血浆、尿）中的甲醚菊酯、灭扫利、功夫、二氯苯醚菊酯、安绿宝、速灭杀丁和敌杀死。通过气相色谱氢焰检测器、非极性熔融石英大口径毛细管柱及程序升温色谱条件，得到较好的系统分离，并测定萃取回收率在81％～93％（血浆）和90％～102％之间（尿）。实验证明，用70％甲醇稀释检材并用氯仿洗脱可得到较完全的吸附和最佳回收率。     

Drugs in motorists traveling Swedish roads: on-the-road-detection of intoxicated drivers and screening for drugs in these offenders

This paper deals with the police officer's or police doctor's ability to find drivers under the influence of drugs. We have also studied whether the protocol on the driver's previous histories of drug intake is useful for directing the chemist in his analytical approach to revealing intoxicants in the suspects' body fluids. A comprehensive procedure for screening traffic-hazardous drugs in the urine was found necessary and is described. By using this method, we have studied the incidence of drunken drivers with detectable medicinal or illicit agents. The results demonstrate that 91% of those drivers found by the officer or doctor of the police to be on intoxicants other than ethanol, carried some kind of traffic-hazardous drug in their body fluids, and that the doctor was a better judge than the police in identifying these offenders. By using a series of chemical methods for drug screening, we found that every third driver suspected of drunken driving due to ethanol, but not to other intoxicants, held some kind of a traffic-hazardous drug substance in his urine; benzodiazepines and cannabinoids were the most common findings. The data imply that 34% of these suspects revealed their intakes of traffic-dangerous intoxicants. We conclude that the judgements of both the officer and doctor of the police are needed for an efficacious detection of drivers under the influence of drugs. Moreover, the results infer that the chemist has to screen for intoxicants to reveal these in a suspect driver. We also conclude that drugs, particularly the benzodiazepines or cannabinoids, may be commonly encountered in drunken drivers, suspected of being inebriated by ethanol but no other toxicants.     

高效液相色谱法分离测定药酒中乌头碱的含量

目的建立药酒中乌头碱的高效液相色谱快速分析方法。方法以白酒添加乌头碱对照品对药酒样品的前处理方法、仪器测试条件、线性范围、精密度、回收率进行全面考察,建立定量分析方法。对药酒中所含乌头碱的浓度进行测定。结果该方法乌头碱在药酒中的线性范围是0.45～9.0μg·mL-1;日内、日间精密度分别小于3.1%和4.7%;回收率在(97.3±2.8)%以上。结论所建方法实用、便捷,可对药酒中乌头碱的含量进行快速检测。     

Trace detection of meglumine and diatrizoate from Bacillus spore samples using liquid chromatography/mass spectrometry

Following the September 11, 2001 terrorist attacks, letters containing Bacillus anthracis were distributed through the United States postal system killing five people. A complex forensic investigation commenced to identify the perpetrator of these mailings. A novel liquid chromatography/mass spectrometry protocol for the qualitative detection of trace levels of meglumine and diatrizoate in dried spore preparations of B. anthracis was developed. Meglumine and diatrizoate are components of radiographic imaging products that have been used to purify bacterial spores. Two separate chromatographic assays using multiple mass spectrometric analyses were developed for the detection of meglumine and diatrizoate. The assays achieved limits of detection for meglumine and diatrizoate of 1.00 and 10.0 ng/mL, respectively. Bacillus cereus T strain spores were effectively used as a surrogate for B. anthracis spores during method development and validation. This protocol was successfully applied to limited evidentiary B. anthracis spore material, providing probative information to the investigators.     

Evolution of the content of THC and other major cannabinoids in drug-type cannabis cuttings and seedlings during growth of plants

In Europe, authorities frequently ask forensic laboratories to analyze seized cannabis plants to prove that cultivation was illegal (drug type and not fiber type). This is generally done with mature and flowering plants. However, authorities are often confronted with very young specimens. The aim of our study was to evaluate when the chemotype of cannabis plantlets can be surely determined through analysis of eight major cannabinoids content during growth. Drug-type seedlings and cuttings were cultivated, sampled each week, and analyzed by high-performance liquid chromatography with diode array detection. The chemotype of clones was recognizable at any developmental stage because of high total Δ(9)-tetrahydrocannabinol (THC) concentrations even at the start of the cultivation. Conversely, right after germination seedlings contained a low total THC content, but it increased quickly with plant age up, allowing chemotype determination after 3 weeks. In conclusion, it is not necessary to wait for plants' flowering to identify drug-type cannabis generally cultivated in Europe.     

Drug-facilitated sexual assault using tetrahydrozoline

Drug-facilitated sexual assault (DFSA) has been defined as the use of a chemical agent to facilitate a sexual assault. We report two cases of the use of tetrahydrozoline for DFSA. We believe this is the first report with urinary quantification of tetrahydrozoline levels postassault. Blood and urine were obtained c. 20 h postexposure in two cases of reported DFSA. Tetrahydrozoline was not detected in blood but was identified in urine in both victims. After initial identification in the urine using the 2010 update to the AAFS mass spectrometry database library, tetrahydrozoline was quantified at 114 and 150 ng/mL, respectively, using GC/MS. Two unique clinical features reported in these cases were intermittent periods of consciousness and postexposure vomiting. Use of GC/MS was successful in identifying tetrahydrozoline in the 100 ng/mL range up to 20 h postexposure. For victims with late presentation, urine may be a better sample for evaluation for tetrahydrozoline.     

Cyanide and amygdalin as indicators of the presence of bitter almonds in imported raw almonds

Abstract: Consumer complaints received by the U.S. Food and Drug Administration in August 2010 about raw organic almonds tasting “bitter” opened an investigation into the presence of bitter almonds in the imported product. Bitter almonds (Prunus amygdalus) contain the cyanogenic glucoside amygdalin, which hydrolyzes to produce cyanide. Ultraviolet–visible spectrophotometry was used to detect and quantitate cyanide, and liquid chromatography‐mass spectrometry was utilized to detect amygdalin in the submitted samples. Control bitter almonds were found to contain 1.4 mg cyanide/g and an estimated level of 20–25 mg amygdalin/g. The questioned samples contained between 14 and 42 μg cyanide/g and were positive for the presence of amygdalin. Sweet almonds were found to be negative for both compounds, at levels of detection of 4 μg cyanide/g and 200 μg amygdalin/g.