气相色谱/质谱法分析孔石莼中的脂肪酸

建立了孔石莼脂肪酸的气相色谱/质谱(GC/MS)测定方法。使用Folch法提取了孔石莼中的总脂,经过2 mol/L HCl-甲醇溶液的甲酯化处理后,采用GC/MS法对其脂肪酸组成进行了分离分析,同时结合有机质谱学规律,分别对饱和脂肪酸甲酯、单不饱和脂肪酸甲酯和多不饱和脂肪酸甲酯的裂解规律和质谱特征进行了分析归纳。通过质谱数据库检索和标准品对照,鉴定出孔石莼中的24种脂肪酸,其中9,12,15-十八碳三烯酸、4,7,10,13-十六碳四烯酸和6,9,2,15-十八碳四烯酸3种主要多不饱和脂肪酸占总脂肪酸含量的45.14%。通过对孔石莼中脂肪酸的分析,表明特征离子在脂肪酸甲酯尤其是多不饱和脂肪酸甲酯的定性方面具有很好的应用价值。     

裂解气相色谱/质谱法检验复印墨粉

复印墨粉检验分析在经济案件侦查以及墨粉配方研究方面具有十分重要的意义。采用裂解气相色谱技术,对收集到的复印墨粉进行分离分析,并用裂解气相色谱/质谱联用技术,对所得裂解峰进行归属。分析结果的重复性与稳定性良好,复印件上墨粉与原墨粉分析结果一致。对不同厂家与牌号的墨粉进行区分与归类,为墨粉鉴别提供了依据。     

气相色谱-质谱法鉴定二氯丁烷异构体

利用气相色谱-质谱联用仪测试样品得到质谱图，按各峰强度及基峰质荷比等信息对化合物图谱进行解析，确定醚-三氯化铝体系中二氯丁烷异构体的结构。该法综合利用大型分析仪器分析同分异构体，较之利用标准品的传统方法更加省时、省力。     

气相色谱/质谱法测定空气中痕量偏二甲肼

建立了气相色谱/质谱法测定空气中痕量偏二甲肼的分析方法。以2-硝基苯甲醛为衍生化试剂,以含有衍生化试剂的甲醇溶液为吸收液,气体发生装置发生的偏二甲肼气样用吸收液直接吸收后,与衍生化试剂在甲醇中发生反应,对气体采样和衍生化反应条件进行了优化,考察了气相色谱/质谱法测定空气中痕量偏二甲肼的加标回收率为75%～92%;检出限(S/N=3)为0.019mg/L。采样2L时,最低检测浓度为9.5ng/m3。当采样流量为0.2L/min时,平均采样效率为99%。本方法灵敏快速,简便易行,可实现对空气中痕量偏二甲肼的检测。     

凝胶渗透色谱-气相色谱/质谱法同时测定食用油中22种邻苯二甲酸酯

建立了凝胶渗透色谱-气相色谱/质谱法同时测定食用油中22种邻苯二甲酸酯的方法。方法具有良好线性,相关系数R均大于0.999,检测限在0.09～11.83 mg/kg之间,平均回收率在81.45%～113.90%范围内,相对标准偏差为1.55%～9.41%。采用该方法对国内食用油中邻苯二甲酸酯增塑剂进行检测,实际样品中检出邻苯二甲酸二异丁酯、邻苯二甲酸二丁酯和邻苯二甲酸二(2-乙基)己酯,可满足目前食用油中邻苯二甲酸酯的检测要求。     

烟草制品中紫苏葶的气相色谱/质谱法分析

以二氯甲烷为溶剂,丙酸苯乙酯为内标,将烟草制品进行萃取,经固相萃取柱纯化,采用气相色谱／质谱法定量分析了烟草制品中的紫苏葶．方法的定性检测限为0．11μ/g,定量检测限为0．36μ/g,平均回收率为95．53％,相对标准偏差（RSD）为1．89％．     

气相色谱质谱法测定功能性饮料中的肌醇

研究建立了功能性饮料中肌醇的气相色谱/质谱(GC/MS)测定方法.样品经浓缩、硅烷化后以正己烷提取,用气相色谱/质谱仪外标法测定其含量.此方法回收率范围为90.0%～105%;变异系数为2.0%～5.0%.方法适合于功能性饮料中肌醇的分析测定.     

松香产品中重质松节油成分的气相色谱/质谱法分析

利用水汽蒸馏提取法富集了松香产品中残留的重质松节油,经气相色谱／质谱联机分析,发现其主要由１９种单萜和倍半萜化合物组成,全部为香味物质（未知物除外）。为提高松香产品的品质和开发利用松香重质松节油提供了依据。     

气相色谱-质谱法测定白酒中邻苯二甲酸酯

建立了白酒中15种邻苯二甲酸酯类化合物(PAEs)残留量的气相色谱-电子轰击离子源质谱(GC-EI/MS)测定方法。样品通过旋转蒸发除乙醇,正己烷超声提取,LC-Si SPE小柱净化,氮吹浓缩后进行气相色谱-质谱法分析。结果表明:该方法具有良好的线性关系,相关系数(r2)大于0.998,平均加标回收率为85.3%~103.1%,相对标准偏差为3.8%~8.8%,15种邻苯二甲酸酯(PAEs)的方法检出限(MDL)为0.011~0.041mg/L。该方法具有简单、快速、灵敏度高和定性定量准确等优点,满足各类白酒样品的分析要求。     

猪油挥发油成分的气相色谱/质谱法分析

1　引　　言油脂是人类的主要食品之一 ,其主要成分是脂肪酸甘油三酯 ,它参与人体正常生理代谢。油脂香气成分是其微量成分 ,含量一般在油脂总量的 1%以下 ,却构成其各自特征香气。奶油、玉米油、牛油等均有较详细的报道。本文以ＧＣ ＭＳ分析猪油香气成分 ,70种成分被确定。2　实验部分2 .1　主要仪器　ＨＰ5 973气质联用仪 (ＧＣ ＭＳ) ,ＨＰＩＮＮＯＷＡＸ 30ｍ× 0 .2 5ｍｍ× 0 .2 5 μｍ毛细管柱 ,ＮＩＳＴ98谱库。2 .2　ＧＣ ＭＳ条件　进样口温度 2 5 0℃ ,检测器温度 2 80℃ ,柱温 6 0℃ (2ｍｉｎ) 2℃ ｍｉｎ12 0℃ (1ｍｉｎ) 10…     

有机硅混合环硅氧烷色谱－质谱联用定性分析

通过色谱－质谱联用定性地分析了二甲基硅氧烷和甲基乙烯基硅氧烷混合环体的色谱、质谱特征。讨论了甲基乙烯基环四硅氧烷质谱的离子分裂方式,测定了各种有机环硅氧烷的色谱保留时间（ｔＲ）,建立了有机硅混合环体色谱－质谱的定性分析方法。     

山楂挥发性化合物的气相色谱-质谱分析

采用蒸馏－萃取法收集山楂果的挥发性化合物,通过气相色谱及气相色谱／质谱分析,鉴定了３２种化合物,占总峰面积的６１％～６８％。其中主要的１０种化合物是顺－３－己烯醇、顺－３－乙酸己烯酯、α－萜品醇、糠醛、己醇、乙酸己酯、壬醛、柠檬醛、３－戊烯－２－酮,反－２－癸烯醛等。     

Analysis of turkish lignite tar by coupled LC/GC,GC/MS,and capillary SFC

This work describes the analysis of a pyrolysis product of a lignite sample obtained from the Turkish Goynuk reserve. The aliphatic, aromatic and polar compounds present in the tar are separated and identified by various chromatographic techniques: Capillary gas chromatography/mass spectrometry (GC/MS), on-line high performance microbore liquid chromatography/capillary gas chromatography (LC/GC) and capillary supercritical fluid chromatography (SFC). The suitability of each technique for this particular application is discussed, and semi-quantitative results are presented for the major components detected.     

Interlaboratory GC/MS response factor precision

A quality control procedure for Fused Silica Capillary Column Gas Chromatography/Mass Spectroscopy (FSCC GC/MS) was tested and shown to produce similar response factors at five Spectroscopy (FSCC GC/MS) was tested and shown to produce similar response factors at five laboratories. The average relative standard deviation (RSD) of interlaboratory response factors for fifty three compounds of environmental interest determined at each laboratory at nominal injected weights of 20, 100, and 200 ng was found to be 18.9% for four of the five laboratories which participated in this work. These data demonstrate that similar response factors can be attained in routine GC/MS measurements when adequate quality control is maintained.     

食品中胆固醇色谱／质谱／质谱的测定

确立了用色谱／质谱／质谱测定食品中胆固醇的一种新方法，试样经乙酸乙酯提取后，ＧＣ／ＭＳ／ＭＳ测定分析，以胆固醇分子离子为母离了，以其子离子为定量分析的碎片离子。线性好，回收率高，方法可靠。     

Py-GC/MS, GC/MS and FTIR investigations on LATE Roman-Egyptian adhesives from opus sectile: New insights into ancient recipes and technologies

An analytical protocol based on optical microscopy, Fourier transforms infrared spectroscopy (FTIR), analytical pyrolysis in the presence of hexamethyldisilazane followed by gas chromatographic/mass spectrometric analysis (Py-GC/MS) and gas chromatography/mass spectrometry after alkaline hydrolysis, solvent extraction and trimethylsilylation (GC/MS) was used in the chemical characterisation of the original adhesives used to fix monochrome and mosaic glass and stone plaques coming from the Late Roman archaeological site of Antinoopolis (Egypt).FTIR analysis demonstrated the presence of calcite fragments, and Py-GC/MS and GC/MS analyses provided detailed molecular compositions, highlighting the presence of a wide range of compound classes including diterpenoid acids, tricyclic abietanes with a high degree of aromatisation, mid- and long-chain monocarboxylic fatty acids, mono- and di-hydroxy acids, α,ω-dicaboxylic fatty acids, n-alkanols, and n-alkanes. Characteristic biomarkers and their distribution patterns indicated the presence of pine pitch in all the adhesives, which in some cases was admixed with beeswax and brassicaceae seed oil.The results provided new insights into the complex recipes used by artisans in ancient Egypt in the production of adhesives and in the sophisticated manufacture of opus sectile decorations.     

Development and validation of GC/MS method for determination of pramipexole in rat plasma

A simple, rapid and sensitive method has been developed and validated for the determination of pramipexole in rat plasma by using gas chromatography mass spectrometry. The lower limit of quantification (LLOQ) is superior to the other reported LC‐MS/MS methods. After being made alkaline with NaOH, plasma samples (0.1 mL) were subjected to liquid–liquid exteraction using methyl‐t‐butyl ether. Analytes were determined using electron impact ionization in a single quadrupole mass spectrometer. GC/MS was performed in the selected ion monitoring mode using target ions at m/z 211, 212 and 152 for pramipexole and m/z 194 and 165 for caffeine as internal standard. A linear calibration curve was plotted over the range of 20–1000 pg/mL for pramipexole (r² > 0.996). The LLOQ was 20.0 pg/mL, respectively, which offered high sensitivity and selectivity enough for bioanalytical investigation. Inter‐ and intraday precisions ranged from 0.3 to 8.8% and from 0.9 to 11.33%, respectively. The recovery of pramipexole from plasma ranged from 82.4 ± 7.1 to 87.8 ± 5.7%. The method fulfills all standards required for bioanalytical methods and can be successfully applied to a pharmacokinetic study of pramipexole in rats. Copyright © 2010 John Wiley & Sons, Ltd.     

Application of gas chromatography–tandem mass spectrometry (GC/MS/MS) for the analysis of deuterium enrichment of water

Incorporation of deuterium from deuterium oxide (²H₂O) into biological components is a commonly used approach in metabolic studies. Determining the dilution of deuterium in the body water (BW) pool can be used to estimate body composition. We describe three sensitive GC/MS/MS methods to measure water enrichment in BW. Samples were reacted with NaOH and U‐¹³C₃‐acetone in an autosampler vial to promote deuterium exchange with U‐¹³C₃‐acetone hydrogens. Headspace injections were made of U‐¹³C₃‐acetone‐saturated air onto a 30‐m DB‐1MS column in electron impact‐mode. Subjects ingested 30 ml ²H₂O, and plasma samples were collected. BW was determined by standard equation. Dual‐energy X‐ray absorptiometry scans were performed to calculate body mass, body volume and bone mineral content. A four‐compartmental model was used to estimate body composition (fat and fat free mass). Full‐scan experiments generated an m/z 45 peak and to a lesser extent an m/z 61 peak. Product fragment ions further monitored included 45 and 46 using selected ion monitoring (Method1), the 61 > 45 and 62 > 46 transition using multiple reaction monitoring (MRM; Method2) and the neutral loss, 62 > 45, transition (Method3). MRM methods were optimized for collision energy (CE) and collision‐induced dissociation (CID) argon gas pressure with 6 eV CE and 1.5 mTorr CID gas being optimal. Method2 was used for final determination of ²H₂O enrichment of subjects because of lower natural background. We have developed a sensitive method to determine ²H₂O enrichment in BW to enable measurement of FM and FFM. Copyright © 2015 John Wiley & Sons, Ltd.