气质联用仪自动筛选常见毒物的应用研究

目的建立快速、灵敏的常见毒物的质谱自动筛选检测方法。方法建立常见毒物的质谱用户库，优化分离条件，优化质谱数据的自动分析参数，进行标样和样品分析。结果建立了含1306种常见毒物的质谱用户库；建立了自动筛选方法；得到了150种常见毒物的保留时间和检测限。结论建立的方法具有快速、灵敏、准确的优点，完全可替代繁杂的质谱检索手工操作。     

GC/MS/AMDIS在法医毒物分析中的应用

目的探索自动质谱去卷积定性系统(AMDIS)在法医毒物分析中的应用。方法利用自动质谱去卷积定性系统(AMDIS)、全扫描离子模式(FIM)和选择离子监测技术(SIM)对农药、毒品、安眠镇静类药等常见毒物进行检索分析,比较三种检索方式对不同质量浓度(40.0、4.0、0.4mg/L)毒物的检验结果。结果AMDIS与SIM具有相近的灵敏度,可以将GC/MS全扫描文件去卷积处理,解决杂质干扰问题,准确对目标化合物进行定性;AMDIS可以自动识别重叠的色谱峰并将其与目标谱库进行匹配,为重叠峰的定性提供了直观的鉴别依据。结论AMDIS检索自动快速,适用于GC/MS法快速鉴定毒物。     

液质联用仪自动筛选常见安眠镇静药的应用研究

目的建立快速、灵敏的常见安眠镇静药物的液质联用仪的定性筛选方法。方法采用ZORBAX sb-aq,150mm×2.1mm×3.5μm(带预柱)色谱柱;柱温:30℃;流动相:甲酸(0.1%)甲醇和甲酸(0.1%)水溶液梯度条件;流速:0.4mL/min;通过电喷雾电离,自动三级扫描质谱。结果通过软件自动处理数据,建立了57种常见安眠镇静药的质谱谱库和保留时间参数谱库。结论建立的常见安眠药谱库和分析方法具有快速、灵敏、准确的优点,不易造成漏检,并且用于实际案件检验。     

GC/MS/Xcalibur技术自动分析疑似固体中管制药物

目的建立疑似含毒检材中国家管制药品的自动筛选方法。方法以我国2007年公布的精神药品和麻醉药品的品种目录为检测目标物,建立质谱用户库;以此为基础,设置气质联用仪自动分析方法对疑拟检材进行常见管制药品的快速筛选。结果建立了库名含多种实用信息、包括230种管制药品的质谱用户库;建立管制药品的质谱自动分析方法,实现＂一针分析出结果＂。结论方法简单、快速、准确可靠,省时省力,能有效提高可疑检材中管制药品筛选分析的速度。     

41种抗生素LC/MS联合测定的谱图库建立

目的建立常见41种抗生素LC/MS联合测定谱图库。方法采用ZORBAX sb-aq,2.1mm×150mm×3.5μm（带预柱）;柱温：30℃;流动相：甲酸（0.1%）甲醇和甲酸（0.1%）水溶液梯度条件;流速：0.4mL/min;通过电喷雾电离（ESI）,自动三级质谱检测。结果应用液质联用仪通用检测方法,得到了含有41种常见抗生素的自用质谱谱库和保留时间参数谱图库。通过谱图解卷积和保留时间锁定软件方法实现数据自动处理。结论该方法具有不易漏检和减少假阳性的优点,完全可替代手工检索质谱,可用于实际案件检验。     

定量数据关联二级全扫描与选择反应监测在常见毒物检测中的应用

目的建立快速、准确,可同时进行定性定量的常见毒物的筛选检测方法。方法用Thermo TXQQuantum XLS气相色谱—三重四级杆质谱仪对57种常见毒物及内标惊醒检测。结果得到了57种常见毒物及内标的选择反应检测信息,并且农药鼠药检测限可达到0.1ng/μL水平,药品检测限达27pg/μL水平,毒品检测限达0.4ng/μL水平。结论该方法具有快速、灵敏、准确的优点,可在一次扫描中完成样品的定性定量分析检测。     

气-质联用法（EI．PCI．NCI）在系统毒物分析中的应用

本文应用电子轰击质谱(EI),正、负化学电离质谱(PCI.NCI)技术,建立了315种常见毒,药物的气一质联用系统分析方法。并建立了 EIMS、PCIMS、NCIMS 质谱图谱库。司法鉴定实践表明使用气相保留指数,特征碎片和 EI、PCI、NCI 图谱库检索等多指标的系统分析方法,是未知物鉴定的强有力的工具。     

液相色谱一高分辨质谱联用技术在毒物筛选分析中的应用

毒物种类的广泛性、目标化合物的不确定性以及检材的多样性、特殊性,使得毒物筛选技术一直受到法医毒物分析工作者的重视.液相色谱-高分辨质谱联用技术凭借液相色谱强大的分离功能及高分辨质谱超高的质量分辨率和精确分子质量测定功能,结合一级、二级谱库匹配以及同位素离子丰度比,在化合物的筛选定性方面表现出强大的优势.本文综述了液相色...     

固相萃取同时提取尿中的39种药毒物

目的建立固相萃取方法同时提取尿中的39种药毒物并用高效液相色谱法进行分析。方法以多沙普仑为内标,1ml尿样经Oasis小柱固相萃取,用HPLC进行分析。结果39种药毒物可同时从尿中提出,内源性物质不干扰测定。其绝对回收率除吗啡外均大于70％;天内及天间精密度均小于10％;检测限1-15ng／ml;线性相关系数在0.9977以上。结论本法快速、简便、重现性好,空白干扰小,可用于实际案例的药物毒物筛选。     

8种常见药（毒）物LC-MS/MS定性分析的保留时间和离子丰度比

目的探讨法医毒物分析中液相色谱-串联质谱(liquid chromatography-tandem mass spectrome-try,LC-MS/MS)法检测血液中毒品类(甲基苯丙胺、吗啡、氯胺酮)、苯二氮蓝卓类(艾司唑仑、咪达唑仑、地西泮、氯硝西泮)和巴比妥类(苯巴比妥)共3大类8种常见药(毒)物的保留时间和离子丰度比的最大允许偏差。方法在2根色谱柱、3种色谱条件下,经液液萃取后采用LC-MS/MS进行检测,分析质量浓度在检出限(limit of detection,LOD)、2倍检出限(2LOD)、定量限(limit of quantitation,LOQ)、1.5倍定量限(1.5LOQ)、2倍定量限(2LOQ)、4倍定量限(4LOQ)和6倍定量限(6LOQ)共7个较低质量浓度时保留时间和离子丰度比的偏差。结果血液添加样品中8种药(毒)物绝对保留时间的偏差在±0.05 min范围内的占98.11%,相对保留时间的偏差在±0.4%范围内的占96.21%。离子丰度比的最大偏差与质量浓度存在高度关联:药(毒)物质量浓度为LOQ及以上时,离子丰度比的绝对偏差和相对偏差都有95%以上分别在±25%和±40%范围内;质量浓度为LOQ以下时,范围可分别扩大至±35%和±50%。结论建议8种常见药(毒)物绝对保留时间的偏差判定范围为±0.1 min,相对保留时间的偏差判定范围为±1.0%。质量浓度在LOQ及以上时离子丰度比的绝对偏差判定范围为±25%,相对偏差为±40%,质量浓度在LOQ以下时偏差判定范围可分别扩大至±35%和±50%。     

Differentiation of side chain isomers of ring-substituted amphetamines using gas chromatography/infrared/mass spectrometry (GC/IR/MS).

Common analytical methods used for identifying samples obtained from clandestine laboratories were evaluated for their ability to differentiate between possible amphetamine isomers and homologs. A series of ring-substituted (4-methyl, 4-methoxy, and 3,4-methylenedioxy) amphetamine and N-methylphenethylamine isomers was analyzed using color tests, thin-layer chromatography, gas chromatography/mass spectrometry (GC/MS) and GC/infrared (GC/IR). The N-acetyl derivatives of the isomers were analyzed using GC/IR/MS. GC/IR/MS readily differentiated the 4-methylphenylalkylamine isomers. MS and IR spectra were also obtained for each pair of the 4-methoxyphenylalkylamine isomers and the 3,4-methylenedioxyphenylalkylamine isomers, but differentiation via GC/IR/MS was difficult. The N-acetyl derivatives of each pair of isomers could be readily differentiated using GC/IR/MS. Good library researchable spectra for N-acetylamphetamine could be obtained for IR identification with 10 ng (on-column) and MS identification with 2 ng. The spectrometrically independent IR and MS data obtained for the N-acetyl derivatives indicated that the combination of GC/IR/MS can add a significant level of confidence in the analysis of ring-substituted arylalkylamines.     

Identification of lorazepam and sildenafil as examples for the application of LC/ionspray-MS and MS-MS with mass spectra library searching in forensic toxicology

A mass spectra (MS) library using in-source collision induced dissociation (ESI-CID) as well as a tandem-mass spectra (MS-MS) library with product ion spectra of drugs has recently been developed with a triple-quadrupole ionspray mass spectrometer [1,2]. For the ESI-CID MS library, single-quadrupole mode and for the MS-MS library triple-quadrupole mode have been used. These mass spectra libraries were applied successfully for the general-unknown screening for drugs and metabolites in serum and urine with liquid-chromatography-mass spectrometry (LC-MS) using a PE/SCIEX API 365 with a turboionspray source. As examples, the identification of lorazepam and lorazepam-glucuronide in a serum extract and the identification of sildenafil and alkyloxidated sildenafil in urine are presented here.     

气/质联用法检测鱼藤中鱼藤酮

目的建立气相色谱/质谱联用法检测鱼藤中鱼藤酮的方法。方法将鱼藤根净化处理后使用三氯甲烷浸提,提取液浓缩后经FINNIGAN POLARIS Q型GC/MS气质联用仪检测。结果通过质谱库匹配检出鱼藤酮。结论本方法操作简便、结果准确,易于推广应用,适用于鱼藤酮的检测。     

Identification of selected psychopharmaceuticals and their metabolites in hair by LC/ESI-CID/MS and LC/MS/MS

Hair samples of patients of psychiatry and hair samples of suicide cases were analysed by liquid-chromatography/ionspray-mass spectrometry (LC/MS) for antidepressants and neuroleptics. Electrospray ionisation (ESI) with in-source collision induced dissociation (ESI/CID) and tandem-mass spectrometry (MS/MS) were used for drug and metabolite identification. Mass spectra library searching was performed using an ESI/CID mass spectra library and a MS/MS spectra library. Furthermore, extracted ion chromatograms were used for the detection of N-desmethyl-metabolites, which were also identified by their fragment-ion spectra. Three examples using these methods are shown: The tricyclic antidepressant maprotiline, the selective serotonin receptor inhibitor (SSRI) citalopram and their desmethylmetabolites as well as the neuroleptic pipamperone were detected and identified in hair extracts. For extraction powdered hair was treated by ultrasonication in methanol and solid-phase extraction was used for sample clean-up prior to LC/MS or MS/MS analysis. These examples demonstrate the power of LC/MS and LC/MS/MS for the detection and identification of drugs in hair extracts using full-scan mode and ESI/CID with library searching or using highly selective LC/MS/MS-analysis with library searching or in multiple reaction monitoring mode.     

GC/MS检验先锋必素方法

采取转相萃取法,脱去头孢哌酮钠中的钠,使其分子量降低,通过对样品的处理,使高分子化合物转变为适合GC/MS检测范围的低分子化合物,同样可以达到LC/MS检测的效果,适合基层实验室使用.     

GC/MS/MS时间编程在火灾现场助燃剂检测中的应用

运用Varian SATURN2000气质联用仪通过GC/MS、GC/MS/MS、时间编程 GC/MS/MS对汽油样品进行分析比对,发现利用时间编程GC/MS/MS,对检测火灾现场残留汽油效果很好,可彻底排除样品中基体的背景干扰,大大提高检测灵敏度;同时对混合助燃剂（汽油+煤油、汽油+柴油）进行了实验探索。