GC-MS/MS法对临床样本中甲基苯丙胺的确证分析

目的建立准确可靠的甲基苯丙胺(即冰毒,MA)初筛阳性样本的确证分析方法,排除由于服用药物而产生的假阳性结果。方法在样品前处理中选用环己烷萃取临床样本中的MA,采用七氟丁酸酐对萃取出的MA进行衍生化,结合串联四级杆气相色谱质谱联用法(GC-MS/MS)开发的多反应检测(MRM)方法对样本进行确证分析。结果在MA确证分析中前处理采用衍生化处理后的检测结果不论在峰型、峰高、检测限、灵敏度、定量线性范围方面均优于未进行衍生化处理的结果,不同的衍生化试剂中选用七氟丁酸酐衍生的结果最好。结论本研究建立的GC-MS/MS分析方法对于毒品确证十分准确、有效,可推广应用于其他毒品初筛为阳性的样本进行进一步的确证。     

气相色谱质谱联用快速确证氯美扎酮中毒

[目的]研究建立气相色谱-质谱联用（GC／MS）检测确证氯美扎酮中毒的分析方法。[方法]采用多阶程序升温的色谱分离方法。分别对血样、尿样、呕吐物、洗胃液等中毒样品中氯美扎酮的提取、富集、净化、分离、检测等进行了实验研究。并采用建立的GC／MS方法进行中毒样品实际测定和加标样品回收率测定。[结果]标准系列在0．1000ng范围内线性良好，在100μg/kg加标水平样品回收率范围70．3％～90．2％之间，同一样品平行测定7次相对标准偏差7．6％，选择离子检测方式最低检测量（S／N=10）为42．50ng。[结论]该方法定性、定量准确，能适应于氢美扎酮快速中毒检测的要求。     

毒鼠强的3种检测方法对比分析

目的 对毒鼠强的3种检测方法进行对比分析，为各级检测机构根据设备情况对毒鼠强开展检测工作提供选择依据。方法 对同一样品分别采用化学法、气相色谱法和气相色谱，质谱联用法（GC/MS）进行对比研究。结果 化学法和气相色谱法符合率为80％。气相色谱法和气相色谱，质谱联用法符合率为100％。结论 3种方法快速、灵敏、准确，各项技术指标均能满足各层次检测机构的检测要求。化学法适用于基层单位中毒样品的初筛。气相色谱法简便、准确，气相色谱，质谱联用法（GC/MS）则体现在“快速定性”上，为最后的确证性实验提供有力证据。     

孕激素的UFLC/DAD/ESI/MS/MS定性确证体系研究

目的:建立牛奶中21а-羟基孕酮、17а-羟基孕酮、炔孕酮、甲羟孕酮、醋酸甲地孕酮、醋酸氯地孕酮、醋酸甲羟孕酮和孕酮等8种孕激素的快速液相色谱/二极管阵列/电喷雾电离串联质谱(UFLC/DAD/ESI/MS/MS)定性鉴别体系。方法:牛奶样品经甲醇提取、Oasis HLB固相萃取小柱净化和快速液相色谱分离后,利用DAD检测器在线检测,采用标准紫外光谱和三维光谱图对照方式进行初筛;按照三离子定性原则,利用电喷雾电离串联质谱(ESI-MS/MS)进行确证。结果:DAD在线扫描光谱信息丰富,超快速液相色谱分离良好,电喷雾电离准分子离子强而稳定,二级质谱裂解碎片离子稳定可靠,初筛和确证的定性依据充分。结论:本方法建立的超快速液相色谱、紫外光谱及串联质谱的联合定性方法适用于孕激素残留的筛选和确证检测。     

G/CMS同时检测人尿中N,N-二甲基乙酰胺及其代谢产物N-甲基乙酰胺

目的:探讨利用气相色谱-质谱(GC/MS)建立一种准确可靠的尿样中的N,N-二甲基乙酰胺(DMAC)及其代谢产物N-甲基乙酰胺(NMAC)的测定方法。方法:尿样经乙酸乙酯萃取、浓缩后,用GC/MS全扫描模式(scan)进行定性分析,确定组分出峰时间和特征质量离子,DMAC选择15、44、87m/z,NMAC选择30、43、73m/z,进行选择离子扫描(SIM),作定量分析。结果:DMAC和NMAC的线性范围分别为0.1 mg/L~10.0 mg/L和0.5 mg/L~10.0 mg/L;相关系数分别为0.9993和0.9991;最低检出限分别为0.02 mg/L和0.10 mg/L;相对标准偏差分别为3.26%和7.22%;样品加标回收率分别为91%~99%和88%~102%。结论:方法准确性好、灵敏度高、干扰少,是检测尿样中DMAC和NMAC的较好方法。     

气相色谱联用质谱法同时检测人体尿液中草甘膦及氨甲基膦酸含量

目的建立一种同时检测人尿样中草甘膦(PMG)和氨甲基膦酸(AMPA)含量的气相色谱联用质谱(GC/MS)分析方法。方法采用GC/MS法,EI检测器,色谱柱为DB-5MS毛细管色谱柱。进样前尿样经三氟乙酸酐(TFAA)和七氟丁醇(HFB)衍生化后用氮气吹干,0.2%柠檬醛乙酸乙酯溶液溶解混匀后供GC/MS分析。结果 PMG和AMPA在10~400 ng/ml范围内呈线性关系,最低检测限分别为4.66 ng/ml和1.77 ng/ml,最小检测浓度(LOQ)分别为15.52 ng/ml、5.91 ng/ml,回收率分别为85.2%~97.5%、89.2%~99.1%,精密度均小于10%。结论本实验可同时检测尿液中草甘膦及其代谢产物氨甲基膦酸,且最低检测限较单个检测方法灵敏。     

尿样中三甲基氯化锡测定方法的研究

目的建立尿样中三甲基氯化锡的测定方法。方法尿样中三甲基氯化锡经乙酸乙酯萃取后用毛细管气相色谱分离-质谱定性定量(GC/MS)检测。结果尿样中三甲基氯化锡浓度在0.776～19.400mg/L范围内呈线性关系,相关系数为0.9999,最低检出浓度为0.01mg/L(取尿样10ml)。相对标准偏差(RSD)为4.4%～8.6%,回收率为99.4%～110.0%,样品在-20℃冰箱中至少可保存半年。结论方法适用于尿样中三甲基氯化锡的检测。     

饮水中57种农药的GC/MS确证检验方法

目的:建立饮水中57种农药的GC/MS确证检验方法。方法:采用液-液萃取(LLE)技术,对水样中57种有机磷类、有机氯类、氨基甲酸酯类、菊酯类农药进行提取、净化、浓缩前处理。采用气相色谱/质谱(GC/MS)联用法进行定性测定。结果:本法回收率为89.1%～112.2%,测定精密度为2.4%～14.5%,SCAN检测模式的检出限为0.3μg/L～4μg/L,SIM检测模式的检出限为0.07μg/L～8μg/L。结论:本法简便、快速、灵敏、定性准确,适合于水样中农药的快速鉴定。     

GC/MS法鉴定饮用水中的灭多威

目的：建立以气相色谱-质谱联用技术对多份水样进行灭多威成分鉴定的方法。方法：采用气相色谱-质谱联用法（GC／MS）对饮用水中灭多威进行定性分析，并比较样品处理中3种溶剂的提取效果。结果：灭多威在本次实验设置的色谱条件和质谱条件下能与其他有机物良好分离，在质谱图上可通过灭多威的105、58、88等几个特征离子峰进行准确定性；经比较发现二氯甲烷的提取效果较好。结论：GC／MS法鉴定未知有机毒物简单、灵敏、快速、准确，适合于公共卫生突发事件的应急处理。     

饮水中多种农药残留的气相色谱-质谱检验方法

目的 建立饮水中45种农药的气相色谱-质谱( GC/MS)检验方法.方法 采用液-液萃取方法,对水样中有机磷类、有机氯类、氨基甲酸酯类、菊酯类等45种农药进行提取.优化了气相色谱-质谱(GC/MS)仪器工作参数.结果 本法回收率在88.0％ ～ 116.0％之间,测定精密度RSD在2.4％ ～ 12.5％之间,检出限在0.000 2 ～0.032 mg/L之间.结论 本法灵敏、快速、可靠.     

GC/MS法定性研究硫磺化学成分

目的:介绍硫磺的GC/MS定性分析方法。方法:将硫磺及含硫磺的检材用有机溶剂提取后经GC/MS分析。结果:GC/MS总离子流中得到清晰的S8特征离子峰。结论:运用GC/MS法可以对硫磺进行快速、准确的定性分析。     

调味品中氯丙醇衍生化检测方法研究及应用

本文概述了调味品中氯丙醇形成机理及毒性，报告调味品中氯丙醇的检测技术的研究过程，把其中最主要且成熟的三种气相色谱和质谱检测方法详细论述。（1）衍生化气相色谱／电子捕获检地测定酱油3－氯－1，2－丙二醇（3－MCPD）；（2）衍生化气相色谱／质谱法测定酱油中3－氯－1，2－丙二醇（3MCPD）；（3）衍生化气相色谱／双串联质谱法同时测定酱油中1，2－二氯－2－丙醇、2，3－二氯－1－丙醇和3－氯－1，2－丙醇。应用以上完善的检验技术完成大量样品检测，全面对酱油企业进行管理，解决了输欧酱油遭禁问题，为酱油顺利出口做了大量工作。应用三种气相色谱和质谱方法检测调味品中氯丙醇含量，结果可靠，符合国家调味品最高残留量（MRL）标准。     

血清中16种有机磷农药GC/MS/MS检测方法的研究

目的应用GC/MS/MS建立测定血清中敌敌畏、氧化乐果等16种有机磷农药的分析方法。方法首先做GC/MS全扫描分析,确定16种化合物的母离子,然后比较不同碰撞诱导裂解(CID)电压时二级质谱中特征离子的峰面积大小以及信噪比,对CID电压进行优化,从而确定各化合物的色谱质谱条件。样品用Oasis HLB小柱进行固相萃取后,用乙酸乙酯洗脱,浓缩后再用乙酸乙酯定容后上机测定。结果在0～1000ng/ml范围内,16种化合物的线性相关系数均大于0.995,加标回收率在75%～129%之间,RSD<10%;日内和日间相对标准偏差小于15%(n=6)。除敌敌畏的检测限为55ng/ml外,其余待测物均检出限均小于2ng/ml。结论该方法灵敏度高、准确性好,适合于血清中有机磷农药的分析测定。     

Analytical techniques and method validation for the measurement of selected semivolatile and nonvolatile organofluorochemicals in air

The widespread use of semi- and nonvolatile organofluorochemicals in industrial facilities, concern about their persistence, and relatively recent advancements in liquid chromatography/mass spectrometry (LC/MS) technology have led to the development of new analytical methods to assess potential worker exposure to airborne organofluorochemicals. Techniques were evaluated for the determination of 19 organofluorochemicals and for total fluorine in ambient air samples. Due to the potential biphasic nature of most of these fluorochemicals when airborne, Occupational Safety and Health Administration (OSHA) versatile sampler (OVS) tubes were used to simultaneously trap fluorochemical particulates and vapors from workplace air. Analytical methods were developed for OVS air samples to quantitatively analyze for total fluorine using oxygen bomb combustion/ion selective electrode and for 17 organofluorochemicals using LC/MS and gas chromatography/mass spectrometry (GC/MS). The experimental design for this validation was based on the National Institute of Occupational Safety and Health (NIOSH) Guidelines for Air Sampling and Analytical Method Development and Evaluation, with some revisions of the experimental design. The study design incorporated experiments to determine analytical recovery and stability, sampler capacity, the effect of some environmental parameters on recoveries, storage stability, limits of detection, precision, and accuracy. Fluorochemical mixtures were spiked onto each OVS tube over a range of 0.06-6 microg for each of 12 compounds analyzed by LC/MS and 0.3-30 microg for 5 compounds analyzed by GC/MS. These ranges allowed reliable quantitation at 0.001-0.1 mg/m3 in general for LC/MS analytes and 0.005-0.5 mg/m3 for GC/MS analytes when 60 L of air are sampled. The organofluorochemical exposure guideline (EG) is currently 0.1 mg/m3 for many analytes, with one exception being ammonium perfluorooctanoate (EG is 0.01 mg/m3). Total fluorine results may be used to determine if the individual compounds quantified provide a suitable mass balance of total airborne organofluorochemicals based on known fluorine content. Improvements in precision and/or recovery as well as some additional testing would be needed to meet all NIOSH validation criteria. This study provided valuable information about the accuracy of this method for organofluorochemical exposure assessment.     

水中14种挥发性有机污染物的吹扫捕集气相色谱质谱联用测定法

目的建立吹扫捕集气相色谱质谱联用法测定水中14种挥发性有机物的方法。方法采用吹扫捕集方法对样品进行吹脱,吸附,烘烤,吹扫后,用气相色谱质谱联用仪进行定性定量测定。结果利用吹扫捕集气相色谱质谱联用法测定水中14中挥发性有机物,最低检出限0.002～0.01μg/L,回收率97.9%～106.3%,相关系数均大于0.998,相对标准偏差2.26%～9.09%。结论该方法能同时分离水中14中挥发性有机物,线性良好,具有操作简便,快捷,灵敏度高等优点。     

Traditional sampling with laboratory analysis and solid phase microextraction sampling with field gas chromatography/mass spectrometry by military industrial hygienists

The opinions or assertions contained herein are the private ones of the authors and are not to be construed as official or reflecting the views of the United States Department of Defense or the Uniformed Services University of the Health Sciences. Rapid on-site detection and identification of environmental contaminants to which personnel may be exposed is often needed during military deployment situations. The availability of military industrial hygienists with capabilities for "complete" on-site exposure assessment of chemical species should allow detection and identification of a number of important stressors almost immediately following sample collection. Portable gas chromatography/mass spectrometry (GC/MS) provides a rapid and efficient separation of volatile and semivolatile organic analytes, accompanied by sensitive electron impact ionization-mass spectrometry (EI-MS) detection. The use of GC/MS in the field is limited, however, by equipment cost, complexity of the equipment, and the analytical process. Additionally, a skilled operator is needed to obtain useful separations and to interpret mass spectral data. To demonstrate benefits and limitations of "complete" exposure assessment capabilities, a previously unidentified complex mixture, produced by thermal dispersion of riot control agents, was examined. Established active sampling methods were used with laboratory analyses. Solid phase microextraction, a passive sampling method that simplifies preparation for GC/MS analysis, also was used with a field-portable GC/MS system. Both sampling/analysis methods were used to detect CS riot control agent-derived air contaminants dispersed from riot control type canisters through oxidizer-supported combustion of a chemical fuel.     

Determination of mercapturic acid in urine samples for the monitoring of occupational exposure to xenobiotics

The determination of mercapturic acids in urine samples of employees exposed to carcinogenic substances requires highly sensitive and specific methods such as GC/MS or HPLC/Fluorimetry. We applied GC/MS to the analysis of thiodiglycolic acid, which is an indicator metabolite of vinyl chloride exposure and of S-phenylmercapturic acid which can be used to control benzene exposure. S-cyanoethylmercapturic acid appears as a degradation product during acrylonitrile metabolism. This metabolite can be determined by HPLC combined with a sulfur specific fluorimetric detector. This procedure which is of general use offers the possibility to improve the biological monitoring in case of exposures to carcinogenic substances.     

Long Chain Perfluorinated Alkyl Acids Derivatisation and Identification in Biota and Abiota Matrices Using Gas Chromatography

An analytical method involving derivatisation of perfluorocarboxylic acids for their analysis in abiotic and biotic matrices is presented. Derivatisation of the acid group to form a suitable alkyl ester provided a suitable compound for mass spectrometric detection in gas chromatography/mass spectroscopy (GC/MS) instrumental analysis. The acid is esterified by an alkyl halide i.e. benzyl bromide as the alkylating agent for perfluorocarboxylic acids quantification in fish and water by GC/MS. The gas chromatography method can be applied in the analysis perfluoro alkyl acids in water and biological matrices, especially where high levels of these compounds are expected. Typical values for precision obtained were 0.1%–10.0% with concentrations ranging from 0.2 to 1 μg/mL). Results demonstrate that GC/MS can supplement liquid chromatographic/mass spectroscopy method for quantification of fluorocarboxylic acid surfactants. The result indicates that there is need for more research on method analysis of perfluorinated acids in environmental matrices.     

In-solution derivatization and detection of glyoxal and methylglyoxal in alcoholic beverages and fermented foods by headspace solid-phase microextraction and gas chromatography–mass spectrometry

A simple and sensitive method for the simultaneous determination of glyoxal and methylglyoxal in alcoholic beverages and fermented foods was developed. This method involved simultaneous derivatization in solution with 2,2,2-trifluoroethyl hydrazine (TFEH) and headspace solid phase microextraction, followed by detection via gas chromatography-mass spectrometry (GC–MS). The method established herein can be summarized as follows. The sample was adjusted to pH 6.0 in a headspace vial, saturated with sodium chloride, and allowed to react with TFEH at 85 °C for 20 min. The formed derivatives were vaporized and adsorbed on divinylbenzene/carboxy/polydimethylsiloxane fibers. The TFEH derivatives were subsequently desorbed and analyzed by GC–MS, where the spectrum showed a single sharp peak. Under the established conditions, the quantification limits of glyoxal and methylglyoxal were 3.6 and 2.1 μg kg⁻¹, respectively, and the relative standard deviations were under 8% at concentrations of 20, 100 and 2000 μg kg⁻¹. All samples were detectable at typical glyoxal (62–4116 μg kg⁻¹) and methylglyoxal (11–2342 μg kg⁻¹) concentrations in beverages and foods.     

测定室内空气中挥发性有机污染物的SUMMA罐采样-GC—MS联用方法研究

[目的]建立并完善适用于日常检测工作的SUMMA罐采样．气相色谱-质谱（GC—MS）联用技术检测空气中多种挥发性有机物的方法。[方法]用预先抽真空的SUMMA采样罐采样,气体样品经由Enteeh 7100预浓缩系统富集浓缩后,再注入GC分离后利用MS进行定性及定量分析,可分析62种挥发性有机物。[结果]测定空气中的挥发性有机物方法的检测限为体积分数2×10^-10（0．2ppbv）,方法报告限为体积分数1×10^-9（1ppbv）。各化合物标准曲线线性R^2均≥0．995,回收率均在±30％范围,大多数目标化合物的回收率均在±15％,方法稳定性、重现性良好。[结论]SUMMA罐采样-GC—MS联用技术在保存样品稳定性、保证方法检测限及提高分析化合物的种类等方面均有较大优势,适用于对室内空气中低浓度挥发性有机物的监测。