Determination of trasodone in cadaveric material

Methods of trasodone isolation from cadaveric material by water and acetonitrile at pH-2.0, which may be used in expert practice, were developed. Acetonitrile method is recommended for everyday practice as it allows one to isolate about 60% of trasodone and to obtain extracts with lower content of extractive substances. Detection limit in case of trasodone isolation by acidified water is 50 micrograms in 25 g of the liver and by acetonitrile--25 micrograms in 25 g of the liver and kidney.     

The forensic chemical analysis of cadaveric material for the presence of drug and narcotic compounds]

The authors consider that the list of drugs and narcotics which can be reliably identified in a general forensic chemical analysis of cadaveric material (not a purposeful screening) should be changed. Isolation by acidified water, hydrochloric acid hydrolysis, and by acetonitrile should be used for isolation of drugs and narcotic compounds in forensic chemical analysis of cadaveric material.     

High-performance liquid chromatography-ultraviolet-visible spectroscopy-electrospray ionization mass spectrometry method for acrylic and polyester forensic fiber dye analysis

A critical point of comparison between a fiber collected from a crime scene and a fiber from a known source is the color. Fiber dye analysis using thin-layer chromatography or ultraviolet (UV)-visible (Vis) microspectrophotometry provides useful, although limited, data for comparison. High-performance liquid chromatography-electrospray ionization mass spectrometry (LC/MS) overcomes these limitations by integrating chromatography, ultraviolet-visible spectroscopy, and mass spectrometry into a single instrument. In order to evaluate the applicability of the LC/MS to forensic fiber dye analysis, a multi-stage chromatographic method using acidified water and acidified acetonitrile was developed that separated and identified a mixture of 15 basic and 13 disperse dye standards. The LC/MS also detected and analyzed dyes extracted from individual 0.5 cm acrylic and polyester fibers, demonstrating its applicability to this type of analysis. With regard to the analysis of disperse dyes in polyester fibers, the replacement of pyridine with acetonitrile in the extraction system allowed direct injection of the extracts into the LC/MS. The advantage of the LC/MS over other instrumental methods of textile dye analysis is demonstrated by the analysis and differentiation of three black acrylic fibers: two fibers had similar UV-Vis spectra but were differentiated with chromatography and two had similar UV-Vis spectra and chromatograms but were differentiated using the mass spectrometer.     

Achiral and chiral quantification of methamphetamine and amphetamine in human urine by semi-micro column high-performance liquid chromatography and fluorescence detection

In this paper, miniaturized achiral and chiral high-performance liquid chromatographic procedures for the determination of methamphetamine and amphetamine in human urine are described. After a simple pretreatment of human urine (i.e., 10 microL of urine or diluted urine were acidified and dried-up under N2 at room temperature) and fluorescence derivatization with 4-(4,5-diphenyl-1H-imidazol-2-yl)-benzoyl chloride under mild conditions (pH 9.0, 10 min at room temperature), the derivatives were isocratically separated on a semi-micro ODS column with Tris-HCl buffer (0.1 M, pH 7.0): acetonitrile (45 + 55 v/v) at a flow rate of 0.2 mL/min or their enantiomers were separated on a semi-micro OD-RH column with sodium hexafluorophosphate (0.3 M aq.): acetonitrile (44 + 56 v/v) at a flow rate of 0.1 mL/min as the mobile phase. Wide-ranged calibration curves were obtained with detection limits for the achiral and chiral analyses in the atto and femtomol levels, respectively, per injected volume. Satisfactory within- and between-day reproducibility data were obtained with both the methods with the highest relative standard deviation being 9.6%. The methods were applied to the determination of methamphetamine and amphetamine in human urine samples and the concentrations determined by the two methods were well correlated (r = 0.994).     

液液萃取-超高效液相色谱-串联质谱法测定常见食用植物油中5种鸦片生物碱

目的建立酸化甲醇(pH=3)液液萃取-超高效液相色谱-串联三重四极杆质谱(UPLC-MS/MS)测定常见食用植物油中5种鸦片生物碱吗啡、可待因、蒂巴因、罂粟碱、那可汀的检验方法。方法样品加入正己烷摇匀后用酸化甲醇(pH=3)提取,BEH C18色谱柱分离,乙腈(0.01%甲酸)-水(0.01%甲酸+0.05%氨水,体积比)梯度洗脱,电喷雾离子源正离子(ESI+)及多反应监测模式检测。结果结果显示5种待测成分在0.5~300ng/g范围内线性关系良好;方法检出限(S/N=3)在0.1~2ng/g间、定量限(S/N=10)在0.5~3ng/g间;回收率(20ng/g,200ng/g)在82.0%~101.4%间,相对标准偏差(RSD,n=6)为1.4%~4.2%,基质效应(20ng/g,200ng/g)在-5.3%~5.8%间,日间精密度为2.8%~6.7%。结论本方法前处理简单、耗时短,溶剂使用量少,灵敏度高,适合大批量常见食用植物油中5种鸦片生物碱的同时检测。     

Study of TATP: stability of TATP solutions

Stability of raw TATP (3,3,6,6,9,9-hexamethyl-1,2,4,5,7,8-hexoxonane) samples in solutions of common solvents was studied to highlight problems faced by forensic labs in identification and analysis of organic peroxide samples. The TATP samples were prepared by reaction of acetone and hydrogen peroxide (30%) with the aid of following catalysts: hydrochloric, sulfuric, nitric, perchloric and methanesulfonic acid. Acetone, acetonitrile, methanol and acetonitrile/water solutions of TATP samples were prepared and stored at 50°C. Various degrees of stability were observed for particular combination of catalyst and solvent ranging from totally unstable (catalyst-H(2)SO(4)/any solvent) to very stable (catalyst-HCl/solvent acetonitrile). Purification of crude TATP by re-crystallization results in product stable in all investigated solvents. Stability of solution prepared from re-crystallized DADP (3,3,6,6-tetramethyl-1,2,4,5-tetroxane) was found to be on the same level as the stability of solution of re-crystallized TATP.     

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%).     

A Comparison of Common Swabbing Materials for the Recovery of Organic and Inorganic Explosive Residues

The efficiency of solvent based extraction methods used to remove explosive residues from four different swab types was investigated. Known amounts of organic and inorganic residues were spiked onto a swab surface with acetonitrile or ethanol:water combined with ultrasonication or physical manipulation used to extract the residues from each swab. The efficiency of each procedure was then calculated using liquid chromatography‐ultraviolet detection for organic residues and ion chromatography for inorganic residues. Results indicated that acetonitrile combined with physical agitation proved to be the most efficient method; returning analyte recoveries c. 95% for both alcohol based swabs and cotton balls. Inorganic residues were efficiently extracted using ethanol:water, while the use of acetonitrile followed by water significantly reduced the recovery of inorganic residues. Swab storage conditions were then investigated with results indicating decreased storage temperatures are required to retain the more volatile explosives.     

Determination of amphetamine by HPLC after acetylation

An analytical procedure has been developed for the HPLC determination of amphetamine by off-line pre-column derivatization. The proposed procedure consists of sample preparation by acetylation of amphetamine with acetic anhydride and a subsequent reversed-phase HPLC separation on an octadecyl silica stationary phase with salt-free mobile phase (tetrahydrofuran, acetonitrile, 0.1% triethylamine in water, 15:15:70 v/v) applying UV-detection. The applicability of the elaborated procedure is demonstrated with results obtained by analysis of real samples seized in the Hungarian black market.     

超高效液相色谱-串联质谱法同时测定尿液中16种抗生素

目的 建立同时分析尿液中16种抗生素的超高效液相色谱-串联质谱(UPLC-MS、MS)方法.方法 以哌拉西林为内标.尿样中的目标化合物经Oasis HLB固相萃取柱富集、纯化,利用ZORBAX SB-C18色谱柱,以0.1%的甲酸溶液-乙腈为流动相经梯度洗脱分离,采用多反应监测(MRM)模式进行分析.结果各化合物的最低...     

Extraction of trifluralin from acetonitrile solutions

Results of extraction of trifluralin from an aqueous acetonitrile solution using various organic solvents are presented. The degree of extraction was shown to depend on the nature of extractant and the water/acetonitrile ratio. An optimal electrolyte and the degree of saturation of the water-acetonitrile layer with this electrolyte were selected. The highest efficiency of extraction was achieved by using water-saturated ethylacetate as an extractant. The indices of extraction were calculated as necessary for the isolation of a given amount of trifluralin from aqueous acetonitrile (4:1) solutions with the solvents considered in the present study.     

Toxicologic studies in a fatal overdose of 2,4-D, mecoprop, and dicamba

A suicidal poisoning committed by a 61-year-old woman, who ingested an unknown quantity of Killex, containing in aqueous solution 100 g/L of (2,4-dichlorophenox)acetic acid (2,4-D), 50 g/L of mecoprop, and 9 g/L of dicamba as amine salts is described. Quantitation of chlorophenoxy acids was performed by extraction from an acidified mixture and concentration before high performance liquid chromatography analysis. All three herbicides were separated in a phosphate buffer/acetonitrile mixture at 280 nm on a RP-8 column. Concentrations of herbicides found were: in blood--520-mg/L 2,4-D, 530-mg/L mecoprop, and 170-mg/L dicamba; in urine--670-mg/L 2,4-D and 520-mg/L mecoprop; in bile--340-mg/L 2,4-D, 530-mg/L mecoprop, and 140-mg/L dicamba; and in liver--540-mg/Kg 2,4-D, 500-mg/Kg mecoprop, and less than 100-mg/Kg dicamba. Liquid chromatography was found to be a reliable method for herbicide quantitation in biological tissues and fluids. The technique offered definite advantages over ultraviolet spectrophotometry and avoids the derivatization requirement for gas chromatography.     

Methods for detecting diazoline in chemicotoxicological studies]

New specific methods of diazolin detection by microcrystalline and chromogenic reactions as well as by thin-layer sorbent chromatography were developed. These methods were used to detect diazolin, isolated from biological object by water acidified with oxalic acid. It was stated that diazolin is detectable in chlorophorm extraction obtained both from acidic and from alkaline aqueous solutions.     

A rapid screening procedure for drugs and poisons in gastric contents by direct injection-HPLC analysis

A high performance liquid chromatographic method for toxicological drug screening of gastric content has been developed. The samples were diluted (1:3-1:30) in 0.01 N hydrochloric acid and injected into a reverse phase column for separation by gradient elution. Mobile phase consisted of solvent A (acetonitrile/water 90:10, 0.01 M sodium dodecylsulphate, 0.5% v/v glacial acetic acid) and solvent B (water/acetonitrile 90:10, 0.01 M sodium dodecylsulphate, 0.5% v/v glacial acetic acid); the gradient was programmed from 20 to 80% A in 30 min. The flow was kept constant at 1.5 ml/min. Two home-made internal standards, butyrylsalicylic acid and diacetyltubocurarine with retention times of 5.6 and 21.4 min, respectively, were used. Drugs are identified by matching their relative retention times and UV spectra (200-400 nm) with those contained in a home made library of more than 340 reference compounds (9 analgesics, 22 antidepressants, 30 antihistamines, 14 antihypertensives, 21 antirheumatics, 15 beta-blockers, 9 bronchodilators, 10 Ca antagonists, 14 diuretics, 26 neuroleptics, 25 tranquilizers, and other significant xenobiotic compounds). The fluorometric (FLD) emission spectrum (280-700 nm; excitation wavelength, 230 nm) was used as a further identification. At 50mg/l analyte concentrations, the injection of gastric content after dilution (1:3) produced S/N ratios in the range 8-140. The method is simple, rapid, rather inexpensive and proved to be a useful means of investigation if used in combination with GC-MS screening in blood. On the other hand, the system suffers from a relatively limited sensitivity for compounds with a low UV absorption and from interferences due to the presence in the matrix of some highly UV- and FL-responsive compounds (e.g. tryptophan).     

全血中西地那非的HPLC分析

目的建立血中西地那非的HPLC-DAD检测方法。方法用硅胶小柱分离提取血中的西地那非,HPLC-DAD分析。分析柱：Nova-pak C18（150×3.9mm）,5.0μm;保护柱：Phenom enex C18（ODS,4.0×3.0mm,Octade-cyl）;流动相A：0.06%三氟乙酸＋0.06%三乙胺＋0.25%乙腈,B：乙腈,梯度程序分离;DAD：230nm。结果血中西地那非线性检测范围为1.5-80.0μg/mL,最小检出限量为5ng,平均回收率：82.45%。结论本检验方法简单、准确、快速,适合于临床检测及刑事案件的快速分析。     

UPLC-MS/MS测定全血中的氯丙嗪

目的建立全血中氯丙嗪的UPLC-MS/MS分析方法。方法采用乙腈沉淀蛋白,以Waters ACQUITY UPLCBEH C18柱(2.1mm×50mm,1.7μm)分离,乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,正离子方式检测,多反应离子监测模式(MRM)。结果血液中氯丙嗪在1～100ng/mL范围内线形关系良好,检出限为0.01ng/mL,回收率为81.81%～89.36%,日内、日间精密度分别为9.3%、12.1%。结论本方法准确、快速,可用于全血中氯丙嗪的定性定量分析。     

离子色谱法检测全血中的亚硝酸盐及其代谢产物

目的建立全血中亚硝酸盐的离子色谱分析方法。方法将0.5mL全血和1mL水混合,用乙腈沉淀血液中的蛋白质后依次过C18柱、Ag柱和Na柱,用于去除其中的有机物和氯离子后进行离子色谱检测,并对蛋白沉淀溶剂、前处理柱等最佳实验条件进行考察。结果采用本文方法对空白添加全血进行检测,在色谱图上亚硝酸根离子及其氧化产物硝酸根离子的保留时间分别为10.02min、19.21min。选择乙腈作为蛋白沉淀剂,C18柱去除有机物,Ag柱去除氯离子,Na柱去除银离子。全血中亚硝酸根离子的检出限为0.05μg/mL,亚硝酸根和硝酸根的总回收率为95.9%~117.3%。结论本文方法简便,回收率好,灵敏度高,适用于中毒者血液中亚硝酸盐的检测。     

高效液相色谱法鉴别指甲油的种类

目的建立一种简便快速、灵敏准确的鉴别指甲油样品的方法。方法以乙腈为提取剂,在乙腈/水（80∶20）,检测波长为UV-220nm的色谱条件下,对22种不同产地、不同品牌的指甲油样品进行HPLC分析。结果依据指甲油中组分的不同,可将其分为5大类,每类中各个样品又可根据其色谱峰峰面积比的不同,进一步进行种类的鉴别。结论该方法是一种简便、快速、准确的鉴别指甲油的方法。     

A quantitative method for simultaneous determination of 5-methoxy-N,N-diisopropyltryptamine and its metabolites in urine using liquid chromatography-electrospray ionization-tandem mass spectrometry

5-Methoxy-N,N-diisopropyltryptamine (5-MeO-DIPT) is a designer hallucinogen derived from tryptamine and is reportedly abused and involved in criminal activities. For the detection of 5-MeO-DIPT use, a liquid chromatography-tandem mass spectrometric method for 5-MeO-DIPT and its metabolites, 5-hydroxy-N,N-diisopropyltryptamine (5-OH-DIPT) and 5-methoxy-N,N-isopropyltryptamine (5-MeO-IPT) was developed and validated in rat urine. The urine samples were pretreated by protein precipitation with acetonitrile and introduced into a BDS HYPERSIL C(18) column (50 × 2.0 mm, 5 μm) for chromatographic separation. Mobile phases consisted of methanol, water, and 1% formic acid, and gradient elution was used at a flow rate of 0.2 mL/min. For the MS detection, multiple-reaction monitoring analysis was adopted. The linear range was 0.01-10 μg/mL, and the lower limit of quantification was 10 ng/mL for all analytes. The intra- and interday accuracies and precisions met the criteria (<15%). The developed method was successfully applied to the drug-treated rat urine.     

A rapid and simplified extraction of haloperidol from plasma or serum with bond elut C18 cartridge for analysis by high performance liquid chromatography

This method for the determination of haloperidol (HAL) in plasma is based on high-performance liquid chromatography (HPLC) with a reversed-phase column, ODS-C18. HAL is rapidly extracted from human plasma by using Bond Elut C18 cartridge and its recovery is over 90%. The mobile phase is a mixture of 1% acetate/acetonitrile/tetrahydrofuran/triethylamine (69.5: 28.2:1.9:0.4, by vol.). The method is rapid, simple and free from intereferences and gives good precision.