毛细管气相色谱法测定酱油中4-甲基咪唑的含量

目的建立毛细管气相色谱法定量分析酱油中有毒成分4-甲基咪唑的方法。方法酱油样品在层析柱中用二氯甲烷洗脱,洗脱液浓缩后加入N,N-二甲基苯胺作为内标,采用DB-FFAP毛细管柱分离样品,氮磷检测器测定4-甲基咪唑含量。结果方法线性范围为4.9~1.5×102μg/L;检测限为0.16μg/L;标准加入0.0102mg和0.0602mg 4-甲基咪唑的平均回收率为97.25%和99.44%。结论本文方法具有操作简便、快速、准确等优点,可用于检验酱油中的4-甲基咪唑。     

大鼠血液、尿液中阿米替林的气相色谱快速分析

目的建专：m液及尿液中阿米替林（AMTL）的气相色谱分析方法,、方法以正常大鼠m液及尿液为空F1样奉,分别添加AMTI-标准品和内标SKF525A。实验大鼠以AMTL2倍LD50灌胃,致大鼠急性中毒后提取血液及尿液。用乙醚提取样本中AMTL,采用GC／FID法进行定量分析,并考察实验条件,结果采用该方法,血液及尿液中AMTL线性池用分别为5～150μg／mL（r=0．993）和5～150μg／mL（r=0．998）;最低检测限（S／N／〉3）均为1．0陆g／mL;口内、口间精密度均小于6％,同收率存95.5％～105．6％之间。结论该方法方操作便捷、捧确度高,适用=fAMTL临床治疗中血药浓度快速监测和法医毒物分析鉴定。     

氟乙酰胺和氟乙酸的毛细管柱气相色谱检测

本文建立氟乙酰胺和氟乙酸的毛细管柱气相色谱检测方法，氟乙酰胺和氟乙酸的线性检测范围为0．0625mg/ml～4mg／ml和0．625mg／ml~20mg／ml，最小检出浓度为31．25ug／ml和625ng/ml．太原地区地摊所售鼠药87．5％含有氟乙酰胺，30％含有氟乙酸．     

Forensic applications of pyrolysis capillary gas chromatography

A simple system of pyrolysis capillary gas chromatography has been used to improve discrimination and long-term reproducibility in the analysis of polymers particularly alkyd based paints typically encountered in forensic casework. This involved the coupling of a Pye Curie-point pyrolyser to the inlet port of a capillary gas chromatograph operated in the splitless mode. Examples of pyrograms demonstrating improved differentiation of alkyd paints, and also examples of other architectural and automotive paints, automobile rubbers, adhesives, polyurethane foams and fibres are shown.     

Benzodiazepine findings in blood and urine by gas chromatography and immunoassay

Gas chromatography (GC) and immunoassay techniques applied to blood and urine specimens were compared for the screening of benzodiazepines in postmortem forensic toxicology. Five hundred and six such successive postmortem cases in which both urine and peripheral blood was sent for toxicological analysis by the medical examiners were selected. The urine specimens were tested by the Emit((R)) d.a.u. Benzodiazepine Assay, and in parallel, the blood and urine specimens were screened for benzodiazepine drugs and their metabolites by an established automated dual-column GC method. The lowest number of positives (153) was obtained when immunoassay was performed without enzyme hydrolysis. When urine samples were hydrolysed before immunoassay, the number of positives increased to 175. The highest number of positives (200) was obtained in urine by GC, and the screening of blood by GC yielded 185 quantitative results. Despite the urine GC screening produced the most positives, the quantitative screening of the blood by GC appears to be the most efficient approach in postmortem forensic toxicology, considering the fact that although urine findings confirm the presence of the drug, quantitative results in urine are irrelevant to acute toxicity.     

Analysis of methylbenactyzium bromide in human urine by thin-layer chromatography and pyrolysis gas chromatography.

A rapid and simple method of utilizing thin-layer chromatography (TLC) and pyrolysis gas chromatography (PyGC) for the identification and determination of methylbenactyzium bromide in human urine was studied in this report. Methylbenactyzium bromide was extracted from urine with ODS-cartridge (Sep-Pak C18), then spotted onto a silica gel 60 F254 TLC plate. After development, the separated spot of methylbenactyzium bromide was scraped and wrapped with a ferromagnetic foil without extraction by any organic solvents. The sample was applied into PyGC analysis. The optimum temperature for pyrolysis was 590 degrees C. The main degradation product of methylbenactyzium bromide was identified as diphenylmethane in this procedure by gas chromatography/mass spectrometry (GC/MS). A calibration graph prepared by absolute calibration method showed a good linearity over the concentration range of 1-75 micrograms/spot for methylbenactyzium bromide. The coefficient of variation obtained for eleven replicate analyses of the 3 micrograms/spot of standard methylbenactyzium bromide was 3.8%. The detection limit of this compound by this procedure was 0.1 micrograms/spot.     

人血、尿中富马酸喹硫平的气相色谱分析

目的建立人血、尿中富马酸喹硫平的气相色谱分析方法。方法用乙醚提取血、尿中的富马酸喹硫平，直接对其进行定性、定量分析。以正常人血、尿为空白样本，分别添加标准富马酸喹硫平，确定检材的前处理方法、色谱分析条件、工作曲线、线性范围、方法的精密度、回收率等，并对1例大剂量服用富马酸喹硫平中毒死者的体液浓度进行测定。结果该方法分析血、尿中富马酸喹硫平的线性范围分别为8．0～800．0μg／ml和20．0—800．0μg/ml；最低检测限分别为0．04μg／ml和0．10μg／ml（S／N≥3），日内、日间精密度均小于4％，回收率在97．08％-101．42％之间。结论该分析方法操作便捷、实用、准确度高，适用于富马酸喹硫平的临床血药浓度快速监测和法医毒物鉴定。     

液相微萃取-气相色谱法检测尿液中三唑仑药物

目的建立液相微萃取与气相色谱联用技术快速分析尿液中三唑仑的方法。方法本方法考察了萃取溶剂、体积、萃取时间、萃取振荡速度等条件对液相微萃取的影响,优化的实验条件为:萃取溶剂为0.5ml三氯甲烷,萃取时间25min,振荡速度200r/min。结果采用本文所建立的方法,三唑仑回收率为88.0%~90.5%。结论实验结果表明该方法简便、快速、灵敏、消耗有机溶剂少,是尿液中三唑仑检测的一种有效方法。     

尿中吗啡的氮磷检测——气相色谱分析法

目的建立尿中吗啡的简便快速、灵敏可靠的GC/NPD分析方法。方法样品尿加内标烯丙吗啡,酶或酸催化水解,氯仿-异丙醇(9:1)液液提取或GDX403树脂固相提取,BSA衍生化,HP-5柱和氮磷检测器进行分析。结果 提取率62％～85％,检出限1.2～3.1ng/ml,线性范围20～2000ng/ml,回收率(97％～99％)±(6％~9％)(Mean±cv,N=5)。结论 方法适合于实际案件中尿样的检验。     

尿中五氯酚和2.4-二氯-6-硝基苯酚气相色谱分析

目的建立利用气相色谱分析检测尿中五氯酚和2,4-二氯-6-硝基苯酚的方法。方法取空白尿液添加五氯酚和2.4-二氯-6-硝基苯酚标准品及内标2.4-二氯苯酚,经乙酸酐衍生化后,采用气相色谱法进行检测,并对提取方法、衍生化条件等进行考察。结果经气相色谱分析,尿中五氯酚和2.4-二氯-6-硝基苯酚可得到有效分离,无杂质干扰且峰形较好。在pH值为2条件下,以环己烷作为萃取溶剂为最佳萃取条件。衍生化优选条件为使用10灿乙酸酐并加入10μL无水吡啶,60℃反应30min。结论采用气相色谱法检测尿中五氯酚和2.4-二氯-6-硝基苯酚,方法简单、结果准确,可在实际办案中应用。     

Identification of inorganic anions by gas chromatography/mass spectrometry

Inorganic anions were identified by using gas chromatography/mass spectrometry (GC/MS). Derivatization of the anions was achieved with pentafluorobenzyl p-toluenesulphonate (PFB-Tos) as the reaction reagent and a crown ether as a phase transfer catalyst. When PFB-Br was used as the reaction reagent, the retention time of it was close to those of the derivatized inorganic anions and interfered with the analysis. In contrast, the retention time of PFB-Tos differed greatly from the PFB derivatives of the inorganic anions and the compounds of interest could be detected without interference. Although the PFB derivatives of SO4, S2O3, CO3, ClO4, and ClO3 could not be detected, the derivatives of F, Cl, Br, I, CN, OCN, SCN, N3, NO3, and NO2 were detected using PFB-Tos as the derivatizing reagent. The inorganic anions were detectable within 30 ng approximately, which is of sufficient sensitivity for use in forensic chemistry. Accurate mass number was measured for each PFB derivative by high-resolution mass spectrometry (HRMS) within a measurement error of 2 millimass units (mmu), which allowed determination of the compositional formula from the mass number. In addition, actual analysis was performed successively by our method using trial samples of matrix.     

Quantitative determination of strychnine in blood and urine by gas chromatography with mass-selective detector

A method for the quantitative determination of strychnine in biological fluids by gas chromatography--mass spectrometry is proposed. The preparation of samples for the analysis included extraction of strychnine from blood and urine with the use of AccuBond(II) EVIDEX cartridges for solid-phase extraction and SPEC MP3 disks respectively. The efficiency of extraction was estimated at 0.05 mg/l for blood and 0.02 mg/l for urine. The detection limit was 0.10 mg/l in blood and 0.05 mg/l in urine.     

DPX-GC/MS法分析尿液中新精神活性物质二苯基乙基哌啶

目的 建立一种枪头式分散固相微萃取-气相色谱质谱法,分析尿液中的二苯基乙基哌啶.方法 对影响萃取效果的吸附树脂种类、淋洗液种类、洗脱液种类和洗脱液用量进行优化考察.结果 在最佳实验条件下,尿液中二苯基乙基哌啶的线性范围为0.02～1.0 mg/L,相关系数r2>0.99,检出限为0.005mg/L,回收率在76.7％～...     

气相色谱-串联质谱法分析尿和血中除草剂百草枯

目的建立尿和血中百草枯的离子交换固相萃取-气相色谱-串联质谱分析方法。方法尿样加内标乙基百草枯,用732阳离子交换树脂提取;血样加内标乙基百草枯,用三氯乙酸凝聚蛋白质后取上清液用732阳离子交换树脂提取。提取物用硼氢化钠在水溶液中碱性条件下还原,还原物用有机溶剂提取进行气相色谱-串联质谱法分析。结果尿和血中百草枯的提取率分别为76％和74％,检测限分别为2ng／mL和10ng／mL,尿添加百草枯100ng／mL和血添加百草枯500ng／mL水平的回收率分别为99．6±5．6％和99．3±7．6％（Mean±CV）。结论本文建立的分析方法灵敏度高,能够满足中毒致死案件检验及临床毒物检验的需要。     

The analysis of clingfilms by infrared spectroscopy and thermal desorption capillary gas chromatography.

An automated thermal desorption gas chromatography technique has been adapted to analyse traces of volatile compounds in proprietary food-wrapping films. Fourteen brands of polyvinylchloride film, seven brands of polyethylene film and one polyvinylidene chloride film were discriminated. Prior infrared analysis was used to identify the polymer type. The chromatograms showed minor changes in volatiles along the length of a roll of film and major changes in films exposed to daylight or in contact with cannabis resin.     

尿中3,4-亚甲二氧基甲基苯丙胺的五氟苯甲酰衍生化-氮磷检测气相色谱分析法

本文建立了尿中3,4亚甲二氧基甲基苯丙胺(MDMA)的五氟苯甲酰衍生化-氮磷检测气相色谱分析方法,1ml检尿碱化、加氯化钠饱和、用0.2ml环己烷提取,提取液加4μl五氟苯甲酰氯于室温反应10min,过量试剂用0.1mol/L氢氧化钠溶液涡洗除去,有机相供进样分析.尿中MDMA的检测限为4.0ng/ml,较非衍生化、乙酰化、三氟乙酰化、五氟丙酰化和七氟丁酰衍生化等分析法灵敏.     

Analysis of amphetamines by supercritical fluid chromatography,high-performance liquid chromatography,gas chromatography and capillary zone electrophoresis; a preliminary comparison

A supercritical fluid chromatographic method with UV detection (SFC–UV) for the quantitative separation of phenylisothiocyanate (PITC)-derivatised amphetamines is described and compared to high-performance liquid chromatography–diode array detection (HPLC–DAD), gas chromatography–flame ionisation detection (GC–FID) and capillary zone electrophoresis–diode array detection (CZE–DAD) analyses of amphetamine and related compounds. Difficulties in the analysis of common amphetamines by SFC are discussed. Of the methods described in this paper, the SFC method offered the greatest sensitivity at 0.01–0.02 μg of drug on column. Suggestions are made for the use of combinations of these techniques for the identification of amphetamines when gas chromatography–mass spectrometry is not available.     

尿液中常见毒品的联合分析方法

目的研究尿液中甲基苯丙胺、氯胺酮、吗啡、海洛因的检验方法;方法时间编程和串联质谱技术联合分析;结果分析时间被划分成4个阶段,在每个阶段按照目标物的结构和性质确定母离子和碰撞诱导电压得到相应的子离子碎片信息;结论串联质谱和时间编程的联合分析不仅能有效的排除体内大量内源物的干扰并能同时分析多种物质,此方法应用于实际检案中快速、灵敏。     

Identification of haloperidol and tiapride in the urine with thin layer chromatography

How to identify haloperidol and tiapride in the urine by thin layer chromatography was proposed. Optimal systems of solvents were selected by chromatographic mobility of the substances studied in 14 solvents with different polarity. The findings allowed making an optimal choice of the composition and proportion of the solvents. Diethylamine, as a basic modifier, was introduced in the system of solvents. This improved chromatographic mobility of haloperidol and tiapride. Optimal mobile phases, developers were found, the threshold of detectability of the substances in the given conditions was established. The techniques were used for identification of haloperidol and tiapride in the samples from model urine mixture in the presence of non-identified endogenic compounds. They are characterized by rapid performance, selectivity, sensitivity and good reproducibility and can be introduced into practice of chemicotoxicological laboratories.