A novel method for cyanide quantification in human whole blood using ion chromatography with amperometric detection and its application to cyanide intoxication cases

Cyanide is a highly toxic agent that has been frequently used for suicide in South Korea. It is also used in various industrial fields, such as metal plating, in which many accidental cyanide intoxications have occurred. To overcome the disadvantages of conventional cyanide analysis methods, a simple and fast method for the analysis of cyanide in whole blood using ion chromatography (IC) with amperometric detection was developed in this study. Whole blood samples were deproteinized, diluted, and analyzed using an IC–amperometric detection system. The limits of detection and quantitation were 0.1 and 0.2 mg/L, respectively. The method showed good linearity in the range of 0.2 to 50 mg/L with R² > 0.99. The intra- and inter-assay precision and accuracy values were <10%. The established method was successfully applied to analyze whole blood samples from three cyanide intoxication cases.     

High performance liquid chromatographic determination of alcohols with reference to body distribution of methanol

A method has been developed on reverse phase high performance liquid chromatography for simultaneous determination of methyl, ethyl and isopropyl alcohols under refractive index detection using pure water as the mobile phase. A good separation has been achieved between these alcohols. Detector response was linear with a detection limit of 5 mg/100 ml. Recovery studies were performed by adding known amounts of methyl and ethyl alcohols to blood, lung and liver within the range 80–90%. The reproducibility of the results was always >90%. The quantitative distribution of methyl alcohol in postmortem body tissues and fluids has been reported in three cases of poisoning.     

Acidic and neutral drugs screen in blood with quantitation using microbore high-performance liquid chromatography–diode array detection and capillary gas chromatography–flame ionization detection

Blood previously acidified with aqueous saturated ammonium chloride solution was extracted with ethyl acetate. The dried extract was subjected to acetonitrile–hexane partition. The acetonitrile portion was analysed for the presence of acidic and neutral drugs by HPLC–DAD (200 mm×2.1 mm I.D. microbore ODS-Hypersil column) and GC–FID (25 m narrow-bore×0.25 mm I.D. HP-5 column with 0.33 μm film thickness). The protocol was found to be suitable for both clinical toxicology (including emergency toxicology) and postmortem toxicology. At least 66 drugs of interest were unequivocally identified by RRTs (HPLC) and UV spectra (DAD) match while another 12 were unequivocally identified by double RRTs match (HPLC and GC). Quantitation was facilitated by incorporating calibration blood standards in each assay batch. The five drugs most commonly encountered in clinical blood specimens (1150 cases) were: paracetamol (47.4% of the cases); chlormezanone (6.6%), theophylline (1.74%), naproxen (1.65%) and mefenamic acid (1.56%). The following drugs were detected in toxicologically significant quantities in postmortem blood specimens (245 cases): phenobarbitone (1.22% of the cases), naproxen (0.82%), chlormezanone (0.82%), theophylline (0.82%), carbamazepine (0.41%) and paracetamol (0.41%).     

高效薄层色谱法检测尿中硝西泮的代谢物7-氨基硝西泮

目的 建立用高效薄层色谱法定性及半定量测定人尿中硝西泮的代谢物7-氨基硝西泮(7ANIZ)含量的方法。方法 人口服治疗量10 mg硝西泮后,在pH 9条件下用乙醚进行提取,分析物斑点用氟罗里丝进行荧光显色,紫外灯下(366nm)观察荧光斑点;根据斑点荧光显色情况及强度进行7ANIZ定性及半定量检测。结果 尿中硝西泮代谢物7ANIZ检出限为5 ng/ml,测量限为15 ng/ml。结论 人口服治疗量10 mg硝西泮,用高效薄层色谱法可定性及半定量测定48 h内排泄尿中的7ANIZ。     

中毒死者体内毒鼠强的GC/MS-SIM分析

一 1 9岁男子赌气吞服一白色粉末 ,1 0min后口鼻流血、抽搐 ,迅速送医院 ,经催吐、透析等方法治疗 5天后死亡。根据中毒症状和经验怀疑为毒鼠强中毒。用GC/NPD检验肝中毒鼠强有干扰。改用GC/MS -SIM法分析 ,心血、肝和胃组织中全部检出毒鼠强 ,浓度分别为 0 5 1 μg .mL- 1、0 4 5 μg .g- 1和 0 33μg .g- 1,和文献结果在同一水平。GC/MS -SIM对复杂检材中低含量毒鼠强测定具有更高的选择性 ,也具有较高的灵敏度 ,同时进一步证实毒鼠强排泄较慢 ,经过较长时间后在体内分布比较均匀     

酮洛芬注射液在乳牛体内的残留消除研究

为建立牛乳中酮洛芬的液相色谱-串联质谱(LC-MS/MS)检测方法,牛乳样品经甲醇提取,C18色谱柱分离,采用正离子模式,多反应监测,内标法定量。结果表明,牛乳中酮洛芬的检出限为1μg/kg,定量限为5μg/kg,在5~200μg/kg范围内线性关系良好,相关系数大于0.99。在25~100μg/kg添加水平的回收率为93.3%~107.5%,批内、批间相对标准偏差分别为1.72%~5.46%、1.13%~7.04%。该方法高效、灵敏、准确,可作为牛乳中酮洛芬的检测方法。选用20头健康的泌乳期荷斯坦乳牛,高产、低产各10头,以3 mg/kg剂量肌内注射给药,每天1次,连用3 d,分别于每次给药后第2、15小时采集乳样。每次给药后2 h牛乳中可检出酮洛芬,最高质量分数为(38.43±3.90)μg/kg,停药后15 h均未检出。所有时间点牛乳中酮洛芬质量分数的实测结果均低于加拿大规定的最高残留限量50μg/kg,建议弃乳期为0 d。     

Combined Collection and Analysis of Inorganic and Organic Gunshot Residues

Gunshot residue (GSR) analysis and their interpretation provide crucial information on a criminal investigation involving the use of firearms. To date, several approaches have been proposed for the implementation of a combined sampling and analysis of inorganic (IGSR) and organic GSR (OGSR). However, it is not clear at this stage if concurrent analyses of both types of residue might be detrimental to the analysis of IGSR currently applied in forensic laboratories. Thus, this work aims to compare and evaluate three different protocols for the combined collection and analysis of IGSR and OGSR. These methods, respectively, involve the use of a modified stub (with two halves, one for the detection of IGSR and the other for the analysis of OGSR); the sequential recovery of GSR with two stubs mounted with different adhesives (double-sided carbon tape and Tesa® TACK) and the sequential analysis of IGSR and OGSR from a single carbon stub following carbon deposition. The detection of IGSR was carried out using SEM-EDX, while OGSR analysis was performed using ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). Obtained results for experiments performed using Geco Sinoxid^® ammunition indicated that sequential analysis was the most suitable protocol for the combined collection and analysis of both IGSR and OGSR. A higher number of inorganic (characteristic and consistent) particles and higher concentrations of ethylcentralite, N-nitrosodiphenylamine, diphenylamine, and nitroglycerin were recovered with this method.     

The Effect of Temperature and Exposure Time on Stability of Cholesterol and Squalene in Latent Fingermarks Deposited on PVDF Membrane

Cholesterol and squalene are fatty materials of latent fingermarks that can be utilized for dating methodologies and visualization techniques. Previous studies have suggested these compounds undergo degradation in fingermarks as a function of time (days) and light at ambient temperature. However, studies assessing how their composition changes at low and high temperatures over short periods of time (hours) have not been published previously. Here, we performed quantitative analysis of cholesterol and squalene in natural fingermark residue using PVDF membrane, after exposure to a range of temperatures (−20 to 100°C) for 4 and 8 h. We found that levels of both fatty materials remained constant at −20 to 60°C, but both showed significant reduction at 100°C, over short exposure times. These results indicate that cholesterol and squalene are detectable at −20 to 60°C, whereas at 100°C or higher, both are lost due to rapid thermal degradation.     

Sample Mining and Data Mining: Combined Real-Time and Retrospective Approaches for the Identification of Emerging Novel Psychoactive Substances

Novel psychoactive substances (NPS) are synthetic drugs that pose serious public health and safety concerns. A multitude of NPS have been identified in the United States, often implicated in forensic investigations. The most common and effective manner for identifying NPS is by use of mass spectrometry and the true utility lies within nontargeted acquisition techniques. During this study, a liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) assay was developed, validated, and implemented for forensic toxicology testing. A SCIEX TripleTOF™ 5600 + with SWATH^® acquisition was used. Resulting data were compared against an extensive library database containing more than 800 compounds. The LC-QTOF-MS assay was applied to the reanalysis of biological sample extracts to discover emergent NPS. More than 3,000 sample extracts were analyzed, and more than 20 emerging NPS were detected for the first time. Among these were isopropyl-U-47700, 3,4-methylenedioxy-U-47700, fluorofuranylfentanyl, N-methyl norfentanyl, 2F-deschloroketamine, 3,4-methylenedioxy-alpha-PHP, eutylone, and N-ethyl hexedrone.     

不同炮制温度和时间对炮姜中姜酮含量的影响

目的 考察不同炮制温度和时间对炮姜中姜酮含量的影响。方法 采用超高效液相色谱法对15份不同炮制温度和炮制时间的炮姜样品中姜酮含量进行测定。色谱条件：色谱柱为Acquity BEH C18（100 mm×2.1 mm,1.7 μm）;流动相为乙腈-水,梯度洗脱;流速0.3 ml/min,检测波长280 nm,柱温30 ℃。结果 姜酮进样量在0.073 2～0.366 0 μg时与峰面积呈良好的线性关系（r=0.999 8）,平均加样回收率为97.42%（RSD=2.35%）。炮姜中姜酮含量随着炮制温度和时间的变化明显,以炮制温度为200 ℃、炮制时间为6 min时样品中姜酮含量最高。结论 炮制过程中姜酮含量随着温度升高和时间延长呈现先升高后降低的趋势,所建立的超高液相色谱法简便、准确、重现性好,可用于炮姜中新生成分姜酮的测定。