共查询到19条相似文献,搜索用时 171 毫秒
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目的用五氟丙酰衍生化-气相色谱/质谱联用法分析尿液中硝西泮的主要代谢物7-氨基硝西泮。方法尿液经乙醚萃取后,用五氟丙酰酸酐(PFPA)进行衍生化,得到7-氨基硝西泮衍生化物的总离子流色谱图和质谱图。结果根据7-氨基硝西泮衍生化物色谱的保留时间和质谱中主要特征离子的质荷比进行定性分析;用7-氨基氟硝西泮做内标,以7-氨基硝西泮和内标衍生化物定量离子的色谱峰面积比与浓度的关系进行定量分析。结论用五氟丙酰衍生化-GC/MS分析尿液中硝西泮的主要代谢物7-氨基硝西泮的方法定性、定量灵敏准确,测定结果可应用于司法鉴定。 相似文献
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GDX-403固相萃取分析尿、血中安非他明类毒品 总被引:3,自引:0,他引:3
在国外安非他明类毒品的滥用很严重,有关尿、血等生物检材中该类毒品的提取及分析方法国外报道很多。国内因滥用情况较少,有关分析方法报道较少。该类毒品的提取方法主要有液.液革取{‘j,固相革取[‘,’1,固相微革取[‘]等。对于安非他明类毒品的GCMS确认分析,衍生化是必要步骤,因衍生物的色谱峰较原体色谱峰尖锐,灵敏度高,且特征离子比衍生化前的干扰少。目前国内外报道的该类毒品的衍生化方法主要是用吐陡一醋酸醉,三氟乙酸醉,五氟丙酸研,七氟丁酸酥等做衍生化试剂,衍生化方式有加热及微波照射。本文研究了用国产GDX… 相似文献
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用GC/ECD方法分析海洛因中毒尿液吗啡代谢物 总被引:2,自引:2,他引:0
目的 考查尿检材中海洛因的代谢物吗啡和单乙酰吗啡的液液萃取条件、三氟乙酰化和气相色谱电子捕获检测 (GC/ECD)条件。方法 以烯丙吗啡为内标 ,氯仿∶异丙醇 (9∶1)为液相萃取剂萃取尿中的吗啡和单乙酰吗啡 ,采用MBTFA衍生化 (三氟乙酰化 ) ,GC/ECD检测。结果 尿中加样相对回收率吗啡 89% ,单乙酰吗啡 75 % ,最小检测量吗啡 5 0ng ,单乙酰吗啡 10 0ng。通过实验兔的中毒实验 ,对尿检材进行了分析。 结论 所建立的萃取与检测方法分析海洛因中毒尿检材中的吗啡准确、灵敏 ,可用于海洛因的吸毒检验 相似文献
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GC和GC/MS技术在毒品来源推断中的应用 总被引:1,自引:0,他引:1
目的应用气相色谱(GC)和气相色谱/质谱联用(GC/MS)技术,定性、定量分析毒品案例,推断毒品来源。方法采用GC/MS法定性分析毒品样品中的主成分、痕量杂质、掺假剂和稀释剂,并选择GC/FID和外标法定量分析上述各组分,通过定性和定量数据的统计比对,并用SPSS10.0数据统计分析软件对分组结果进行验证,推断毒品样品之间来源的区别与联系。结果用GC/MS定性分析、GC/FID定量分析和SPSS10.0数据统计分析软件将12个案件的毒品按来源分成7组,其中1、6、7、11号样品和10A、10B样品分成两组,2、3、5、9号样品各成一组,4号和8号样品分成一组。上述12起案件的毒品来源分析和比对结果,经送检部门反馈的破案信息证明,与案件的真实情况十分吻合。结论应用GC/MS、GC/FID技术分析毒品,可准确推断毒品来源。 相似文献
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An extraction and determination method of most important amphetamine derivatives in serum has been developed. The procedure comprises liquid-liquid extraction with tert-butyl methyl ether of the sample under basic conditions, centrifugation, formation of hydrochloric salts after the separation of organic phase, vacuum evaporation of the organic solvent at 60 degrees C, and trifluoroacetylation by on-line flash injection with MBTFA. GC analysis was performed by electron impact GC-MS in SIM mode. In this way satisfactory identification of 12 amphetamine derivatives could be obtained. Amphetamine, methamphetamine, MDA, MDMA and MDEA could be analyzed by using pentadeuterated analogs as internal standards. Low limits of detection 2.5-6.9 ng/mL could be reached. The assay was linear within the 5-100 ng/mL range with a regression coefficient greater than 0.999 for each compound. Our derivatization method is of low cost since only 1 microL of MBTFA is used for each flash trifluoroacetylation. 相似文献
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Amber R. Rose MSFS Monica Joshi PhD Marianne E. Staretz PhD Matthew Wood PhD Thomas A. Brettell PhD 《Journal of forensic sciences》2023,68(4):1148-1161
Aminoindanes are a class of novel psychoactive substances (NPSs) that have become more prevalent over the past decade. GC–MS is often utilized for identifying seized drugs and is well regarded for its ability to separate mixtures. However, certain aminoindanes have similar mass spectral data and require specific gas chromatographic stationary phases for separation. Derivatization is an alternative method that can be applied to GC–MS to enhance chromatographic results, providing more selective analysis in seized-drug identification. This study investigates derivatization techniques to provide options for forensic science laboratories in accurately identifying aminoindanes. Three derivatization reagents, N-methyl-bis(trifluoroacetamide) (MBTFA), heptafluorobutyric anhydride (HFBA), and ethyl chloroformate (ECF) were evaluated for the analysis of eight aminoindanes by GC–MS using two common gas chromatographic stationary phases, Rxi®-5Sil MS and Rxi®-1Sil MS. All three derivatization methods successfully isolated eight aminoindanes, including the isomers 4,5-methylenedioxy-2-aminoindane (4,5-MDAI), and 5,6-methylenedioxy-2-aminoindane (5,6-MDAI) that could not be differentiated prior to derivatization. Reduced peak tailing and increased abundance were observed after derivatization for all the compounds, and mass spectra of the derivatives contained individualizing fragment ions that allowed for further characterization of the aminoindanes. This excluded 4,5-MDAI and 5,6-MDAI as they shared the same characteristic ions and were only distinguishable by their retention times. All three derivatization techniques used in this study allow for successful characterization of the aminoindanes and give forensic science laboratories flexibility in their analysis approach when they encounter these compounds. 相似文献
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There have been reports on improved chromatographic parameters derived from the incorporation of sequential derivatization in preparing biological specimens for the analysis of opiates. This current study was designed to characterize the mass spectrometric data resulting from sequential derivatizations of commonly abused amphetamines (along with all commercially available deuterated analogs) containing two active sites, i.e., amphetamine, methylenedioxyamphetamine, phenylpropanolamine. The first derivatization groups included in this study were trifluoroacetyl, pentafluoropropionyl, and heptafluorobutyryl, while t-butyldimethylsilyl was used as the second derivatization group. Products resulting from the first step and the two-step derivatization processes were analyzed by GC-MS. Full-scan mass spectrometric data were used to select ions with potential for designating the analytes and their respective isotopically labeled analogs in quantitative analysis protocols. Selected ion monitoring data were then collected and assessed to determine the quality of these ions when one or two different derivatization groups were incorporated in the sample preparation processes. A total of 77 full-scan mass spectra and 8 ion intensity cross-contribution tables, representing various forms of derivatization and isotopic analogs of the three amphetamines, are systematically presented for reference. Evaluations of these data concluded that many, but not all, products derived from "double derivatization" (sequential derivatization with two derivatization groups), generate ions of higher quality than those derived from "single derivatization". 相似文献
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Vegetable oils have the ability to spontaneously heat under certain conditions, which may lead to spontaneous ignition. While the oils are not often encountered in forensic casework, they may be suspected in some fire cases. As these oils are not effectively analyzed using traditional fire debris analysis methods, a protocol must be established for extracting vegetable oils from fire debris. In this study, a protocol was developed for the extraction, derivatization, and analysis of vegetable oils from fire debris. Three derivatization methods were compared to establish an optimal derivatization procedure to convert the fatty acids found in vegetable oils to the fatty acid methyl esters (FAMEs) used in analysis. Three different gas chromatograph columns and programs were examined to determine which was best suited for the separation and analysis of FAMEs. The procedure was tested and refined using a variety of neat and burned vegetable oils, in addition to extractions from oils burned on commonly encountered fire debris materials. The findings of this research will serve as a starting point for further understanding and research of vegetable oils in fire debris. 相似文献
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基于五氟苄基溴(PFBBr)微波衍生化的气相色谱—质谱(GC-MS)鉴定N-乙酰邻氨基苯甲酸、邻氨基苯甲酸和苯乙酸三种酸类易制毒化学品,以苯甲酸为内标物。N-乙酰邻氨基苯甲酸衍生化产物特征碎片峰为119、181、317、359;邻氨基苯甲酸衍生化产物特征碎片峰为119、181、317;苯乙酸衍生化产物特征碎片峰为91、181、316。检测结果与直接测试比较,色谱峰型明显改善,检测灵敏度提高,检测限(S/N=3∶1)3~12ng。该方法可以用于N-乙酰邻氨基苯甲酸、邻氨基苯甲酸和苯乙酸的鉴定。 相似文献
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In this paper we have adapted a technique, previously used to determine the presence of urea in aqueous samples of wine and urine, to detect trace levels of urea nitrate explosives. The procedure involves the reaction of the uronium ion (protonated urea) with a fluorophore, xanthydrol. By modification of the procedure to utilize non-aqueous reagents, in neutral conditions, it can be made specific to the presence of the urea nitrate ion pair. The procedure includes selective detection of derivatization products by UV and fluorescence following separation by High-Performance Liquid Chromatography (HPLC). Analytical method development included optimization of HPLC conditions (solvent, gradient), UV and fluorescence wavelengths, and derivatization parameters (xanthydrol amount, reaction times, temperature). The extraction of urea nitrate from surfaces was also investigated and optimized. For best quantification, it was shown that an internal standard was required; this resulted in a quantification limit around 0.17mM (21mg/L). The entire procedure could be performed in less than 30min per sample and potential interferences such as ammonium, nitrate, and urea did not produce a response under standard conditions. 相似文献
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A derivatization/solid phase microextraction (SPME) method for the determination of benzoylecgonine in urine was developed. The derivatization is conducted directly in 1 mL of urine while sonicating for 3 min with 12 microL of hexyl chloroformate and 70 microL of a mixture containing acetonitrile:water:hexanol:2-dimethylaminopyridine (5:2:2:1 v/v), yielding benzoylecgonine hexyl ester (BHE) as the product. After the 3 min period, an aliquot of 250 microL is transferred to a vial for SPME. After the desired extraction time the 100 microns polydimethylsiloxane SPME fiber was transferred to the GC-MS for separation and analysis with a quadrupole ion trap mass spectrometer. The hexyl chloroformate derivatization and SPME procedures were optimized for compatibility and sensitivity. The method was found linear for 0.10 to 20.0 micrograms/mL (r2 = 0.999) of benzoylecgonine in urine using benzoylecgonine-d3 as an internal standard (1.5 micrograms/mL). Intra-day precisions were 8.8 and 6.8% RSD for 0.30 microgram/mL and 17 micrograms/mL benzoylecgonine standards in urine (n = 6), respectively. Inter-day precision (n = 3) were < or = 3.3% RSD, indicating good reproducibility. A detection limit of 0.03 microgram/mL (S/N = 3) was achieved, thus making the SPME method a simplified alternative to SPE for GC-MS confirmation after EMIT tests for benzoylecgonine which have a cutoff of 0.30 microgram/mL. Quantitative results by SPME and SPE of two clinical urine specimens known positive for cocaine by EMIT were in excellent agreement. Benzoylecgonine was detected by the derivatization/SPME method in 22 out of 22 other urine specimens known positive for cocaine. 相似文献
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Pharmacokinetic studies of psilocybin in humans have shown the rapid dephosphorylation of psilocybin to psilocin with further conversion to 4-hydroxy-tryptophole (4HT) and 4-hydroxyindole-3-acetic acid (4HIAA) in plasma. Our study shows that psilocin also undergoes conjugation and can be found in the urine as the psilocin-glucuronide conjugate. Recoveries after enzymatic hydrolysis of the urine with beta-glucuronidase (Helix Pomatia or E. Coli) when compared to non-hydrolyzed urine confirmed the presence of the glucuronide. Detection of psilocin from hydrolyzed and extracted samples was optimized for GC/MS by derivatization with MSTFA. The method developed allows for the detection of psilocin in urine with a limit of quantitation of 10 ng/mL, based on 5 mL of spiked urine. Using this method, our laboratory has confirmed the presence of psilocin in 6 out of 8 urine samples, with concentrations ranging from 10 ng/mL to greater than 200 ng/mL. Before implementation of the hydrolysis and derivatization steps, our limit of detection was 200 ng/mL, based on spiked urine standards. No case samples were positive without hydrolysis and derivatization. 相似文献