裂解气相色谱-质谱联用法分析卷烟燃吸产物

应用带有吸附阱的CDS 5200型热裂解仪,在不同的裂解温度条件下对卷烟样品进行裂解处理,所得裂解产物直接引入仪器进行气相色谱-质谱分析,检测其中的特征组分、烟碱、新植二烯及有害物质,所测得结果与按标准GB/T 19609-2004方法测得的结果作比较。结果表明:①有害物质的裂解释出量随裂解温度降低而明显下降;②半挥发性烟碱的裂解释出量与常态卷烟吸燃温度相近的裂解温度下不存在相关性;③非挥发性的新植二烯的裂解释出量随裂解温度升高而降低;④在常态卷烟吸燃温度下,所测得的烟碱及新植二烯的释出量基本相同;⑤主流烟气中烟碱主要通过蒸馏而并非通过裂解释出;⑥卷烟吸燃温度的降低有利于减少有害物质的释出;⑦所提出的裂解处理方法作为卷烟燃吸产物的模拟分析是可行的。     

裂解气相色谱-质谱联用法对香叶醇的热裂解产物分析

采用裂解气相色谱-质谱法(Py-GC-MS)研究了香叶醇热裂解性质。以氦气为载气,将香叶醇样品分别在不同温度(300,400,500,600,650,700,800℃)下进行热裂解,将热解产物直接引入气相色谱-质谱仪进行定性和半定量分析。结果表明:在700℃时香叶醇完全裂解,裂解产物可达87种。根据主要的裂解产物和其相对含量的变化对香叶醇裂解机理进行初步探讨,为香叶醇在卷烟中的作用评价提供重要的理论依据。     

气相色谱-质谱联用法测定黄兰中挥发油化学成分

采用水蒸气蒸馏法、超临界萃取法、微波辅助提取法与超声波辅助萃取法等4种提取方法提取黄兰挥发油,运用毛细管气相色谱-质谱联用法结合计算机检索对其挥发油化学成分作了鉴定和测定.结果显示从水蒸气蒸馏法、超临界萃取法、微波辅助提取法与超声波辅助萃取法所得挥发油中分别鉴定出了36,35,25和26种化合物.用面积归一法测定了4种挥发油中各种化学成分的相对百分含量,各占总峰面积的92.62%,91.46%,93.18%和95.53%.虽然不同提取方法所得的4种挥发油化学成分有所不同,但其中有20种化合物包括β-荜澄茄烯、大根香叶烯D、丁香烯氧化物、丁香烯等为4种挥发油提取物所共有.     

气相色谱-质谱联用法测定纺织品中1,2-二氯乙烷

建立了气相色谱-质谱联用(GC-MS)测定纺织品中1,2-二氯乙烷的方法。样品经甲醇超声提取后,以TG-624(30 m×0.32 mm×1.8μm)为色谱柱,采用气相色谱-质谱联用全扫描和选择离子扫描进行定性定量分析、外标法定量。结果表明:在0.05~30 mg/L范围内,1,2-二氯乙烷的线性关系良好,相关系数为0.999 3;方法检出限为0.50 mg/kg。在0.5、1.0、5.0 mg/kg 3个加标水平下,粘纤、聚酯、羊毛、锦纶、桑蚕丝、腈纶、棉7种纺织品基底的加标回收率为85.2%~101.4%,相对标准偏差(RSD)为4.0%~7.4%。该方法简便、准确,灵敏度和精密度高,适用于纺织品中1,2-二氯乙烷的分析检测。     

硅烷化衍生-气相色谱-质谱联用法测定烟酸

烟酸片样品用吡啶超声提取、分离后,所得上清液中的烟酸与六甲基二硅氨烷和三甲基氯硅烷进行衍生化反应,产物用正庚烷萃取。萃取液加入苯甲酸乙酯作为内标,供气相色谱-质谱分析。在气相色谱分离中用HP-5MS毛细管柱(30m×250μm,0.1μm)为固定相,在质谱测定中采用全扫描模式。烟酸标准与内标峰面积的比值与烟酸的质量浓度在1.000 g.L-1范围以内呈线性关系,检出限(3s)为4.54 mg.L-1。方法用于烟酸片剂中烟酸的测定,相对标准偏差(n=6)为1.65%~2.89%,回收率在90.1%~93.2%之间。     

气相色谱-质谱联用法测定槐花中挥发性化学成分

槐花样品经蒸气蒸馏及乙醚萃取处理所得挥发油,用气相色谱-质谱联用法进行分析,按峰面积归一化法求出挥发性化学成分的相对含量.分离出42个峰,已鉴定了26个化合物,占其挥发油总相对含量的87.76%.已鉴定的有酸、酯、烯烃、醇、烷烃等10类化合物.其中酸类化合物占总色谱流出峰面积的30.53%,酯类占19.26%,烯烃类占18.01%,醇类占8.64%,烷烃类占5.52%.其主要组分有n-十六酸(26.43%)、17-三十五(烷)烯(14.84%)、喇叭茶萜醇(8.00%)、十六酸甲酯(4.18%)、肉豆蔻酸(4.10%)、8,11-十八碳二烯酸甲酯(3.79%)、月桂酸酐(3.60%)、9-十八(碳)炔酸甲酯(3.26%)、1,2-邻苯二甲酸丁基环己基酯(3.03%)、c-榄香烯(2.66%).     

气相色谱-质谱联用法测定烟火药剂中的苦味酸

建立了气相色谱-质谱联用测定烟火药剂中的苦味酸含量的分析方法。根据烟火药剂的组成特点,在前处理技术方面做出了优化,改进了对氯化衍生产物-氯化苦的萃取方法,将正交实验应用于碳粉中脱附苦味酸的处理步骤,对升温、冲洗、超声波和置换等4个脱附条件做了考查。结果表明:苦味酸的质量浓度在1.0~50.0μg/mL时与色谱峰面积之间线性关系良好(相关系数r=0.9998);仪器检出限(S/N=3)为0.043 mg/kg;方法检出限(3.143δ)为0.543 mg/kg。对3类烟火药剂样品进行5,20,50μg/g 3个不同浓度水平的添加回收,回收率为83.0%~90.0%。     

裂解气相色谱-质谱联用法分析聚醚酰亚胺的裂解产物

应用裂解气相色谱及质谱联用法研究了3种聚醚酰亚胺(PEIM′s)的裂解行为,并根据裂解产物的结构及其相对产率推断了裂解的机理。取3种PEIM样品置于石英裂解管中,分别在550℃,650℃,750℃条件下裂解,所得产物用气相色谱-质谱联用法分析。分析中采用DB-5毛细管色谱柱,电子轰击离子源(200℃,70eV)及在m/z 29～500范围内全扫描方式,并用NIST谱库进行检索和用归一化法计算峰面积进行定量。由试验结果可知:选择在750℃进行裂解较好,在此条件下获得主要裂解产物存在的更明显的信息,有利于对产物进行详细分析和鉴定。     

茚虫威残留的气相色谱-质谱联用法测定

研究了用固相萃取(SPE)-选择离子(SIM) -气相色谱(GC) -质谱(MS)联用法测定蔬菜、水果中茚虫威残留的分析方法.样品采用乙腈超声波均质提取,固相萃取柱净化,丙酮定容.添加量为0.05 μg ～ 1.00μg时,回收率为86.5％ ～ 107.2％,相对标准偏差(RSD)＜5.0％,定量检出限为:0.001...     

气相色谱-质谱联用法测定紫菜中扑草净的残留量

建立了固相萃取净化与气相色谱-质谱联用技术测定紫菜中扑草净除草剂残留量的检测方法。样品由乙腈溶剂提取浓缩后,活性炭和氨基柱双柱串联固相萃取净化,由气相色谱-质谱联用技术测定。方法定量限为2μg/kg,满足国外最低10μg/kg的限量要求;方法在10,40和100μg/kg 3个添加水平和不同人员操作条件下,回收率均稳定在90%~120%之间,RSD%≤7.1%。     

A Study of Oxidative Degradation of Plastics by GC and GC-MS

Abstract

The behaviour of plastics, namely, polyethylene, polypropylene, polystyrene, polyvinyl chloride, polyamide and some copolymers, was studied in a combustion chamber in which the conditions of large-scale fires were simulated. Volatile combustion products were frozen-out or analyzed directly on two columns, one packed with Porapak Q and the other capillary column coated with squalane or CP Sil 5 CB. Carbonyl compounds were determined as the 2,4-dinitro-phenyl hydrazones on an OV-101 stationary phase. Thermal conductivity and flame ionization detectors were used. The decomposition products were identified either on the basis of retention data (retention indices) or by combined capillary GC-MS. The data obtained are used for the cataloguing of plastics from the point of view of their product toxicity during fires.     

Study of spontaneous combustion coals by GC and GC-MS

Organic geochemical characteristics of 3 Chinese spontaneous combustion coals have been carried out by means of GC and GC-MS analysis. It has been observed that more compounds with low to medium carbon number, such as terpenoids and others can be found in spontaneous combustion coals than in normal samples.     

Study of spontaneous combustion coals by GC and GC-MS

Organic geochemical characteristics of 3 Chinese spontaneous combustion coals have been carried out by means of GC and GC-MS analysis. It has been observed that more compounds with low to medium carbon number, such as terpenoids and others can be found in spontaneous combustion coals than in normal samples.     

羰基合成碳酸二乙酯反应产物的气相色谱-质谱分析

碳酸二乙酯(DEC)是重要的有机合成中间体,具有很高的工业应用价值^[1,2]。目前非光气合成DEC的主要方法有酯交换法和氧化羰基合成法。后者是一条很有发展前途的工艺路线^[3]。本文采用气相色谱-质谱联用及保留时间对比的方法分析了乙醇气相氧化羰基合成DEC的反应产物。     

Capillary GC and GC-MS of porphyrins and metalloporphyrins

Summary Despite their inherent low volatility, a wide range of alkyl porphyrins and their various metallo-derivatives have been successfully analysed by gas chromatography on wall coated open tubular (WCOT) capillary columns. As a result of their superior peak shape (comparable ton-alkanes of similar retention times) and relatively low Kovat's retention indices (3300–3900), the bis(trialkylsiloxy)Si(IV) derivatives offer the greatest potential for the GC analysis of geological mixtures of alkyl porphyrins. Similar derivatives of porphyrins of biomedical importance, possessing polar side chains, are also amenable to GC and GC-MS analysis.Presented at the 14th International Symposium on Chromatography London, September, 1982     

Analysis of essential oils from Scutellaria orientalis ssp. alpina and S. utriculata by GC and GC-MS

The chemical composition of the essential oils obtained from aerial parts of Scutellaria orientalis L. ssp. alpina (Boiss.) O. Schwarz and S. utriculata Labill. growing wild in Lebanon, were analyzed by GC and GC-MS. In S. orientalis ssp. alpina, strongly characterized by sesquiterpenes (41.2%) and particularly sesquiterpene hydrocarbons (31.7%), hexahydrofarnesylacetone (11.7%) was recognized as the main constituent, together with hexadecanoic acid (7.6%), caryophyllene (7.4%), caryophyllene oxide (6.8%), 4-vinylguaiacol (5.4%) and germacrene D (5.4%). S. utriculata oil was instead constituted above all by monoterpenes (42.2%), particularly oxygen containing monoterpenes (39.9%), and in this oil the main compounds were linalool (20.1%), 4-vinyl guaiacol (15.5%), alpha-terpineol (8.9%), (E)-nerolidol (8.9%) and geraniol (8.2%).     

Trace-level determination of 1,4-dioxane in water by isotopic dilution GC and GC-MS

The volatile and polar solvent 1,4-dioxane has recently been reported as a contaminant of ground and surface waters, establishing the need to determine this substance in drinking water. This investigation established that 1,4-dioxane can be determined in water by various techniques including direct aqueous injection (DAI) gas chromatography (GC) and purge and trap GC-mass spectrometry (MS). Purge and trap GC-MS is limited by 1,4-dioxane's poor purge efficiency, resulting in detection limits up to 100 times greater than the efficiently purged volatile organic compounds. To attain the sensitivity required for drinking water monitoring, a method based on continuous liquid-liquid extraction with dichloromethane was developed. Isotope dilution was more accurate and reproducible than quantification with external standards, and the improvement in precision led to a lower method detection limit, 0.2 microgram L-1, using a quadrupole ion trap instrument in the electron ionization mode. Isotope dilution accuracy approached 100% in ppb determinations. Isotopic dilution quantification was also possible using a non-selective GC detector owing to the high efficiency of capillary GC columns that resolve the deuterium-labeled solvent from the natural isotopes.     

The importance of GC and GC-MS in perfume analysis

Gas chromatography (GC) and mass spectrometry (MS) are by far the most important analytical techniques in the perfume industry. Both perfume houses (the suppliers) and the home and personal-care companies (the clients) rely primarily on GC and GC-MS for unraveling the composition of perfumes (i.e. perfume formulation), quality control, competitor analysis and trace analysis on substrates and in the headspace. State-of-the-art perfume formulation is based on perfume-specific Kovats Index (KI) and MS databases. By applying FID (flame-ionization detector) response-correction factors, the accuracy of the perfume-formulation process can be further improved. Because of the complexity of perfumes, use is made of GC columns and conditions that offer maximum resolution rather than minimum analysis time. Mass-spectral deconvolution tools can be very useful in identifying perfume ingredients from GC-MS data in cases of co-elution or strong matrix interference. By applying the MS detector in the selected ion monitoring (SIM) mode, GC-MS is very suitable for trace analysis of perfume ingredients, thus enabling the study of perfume efficacy during use of home and personal-care products. Recent developments in the field of comprehensive GC (i.e. GC×GC) also seem very promising for perfume analysis.     

Identification and determination of (+)-sesamin in Semen Cuscutae by capillary GC and GC-MS

(+)-Sesamin has been found to have pharmacological effect which can improve activity, prevent aging and has the effect of antihypertension 1-2. Figure 1 shows its chemical structure. (+)-Sesamin has been known to be abundant in sesame originally, but our previous study shows that (+)-sesamin also presents in a Chinese herbal medicine Semen Cuscutae3-4. Gas chromatography (GC) and gas chromatography - mass spectrometry (GC-MS) have been applied for the determination and identification of (+…     

GC与GC-MS联用技术进展及其在环境中的应用

气相色谱是物质分离分析的重要手段,在环境、生命科学、药物、化工产品分析等领域的应用日益广泛,几乎在所有的领域都涉及到色谱法及其相关技术的应用.本文对气相色谱、气质联用技术的发展及在环境中的应用作一些介绍.