一种水体中有机污染物快速筛查与半定量的方法及其应用

采用液液萃取法富集水体中的有机污染物,以气相色谱-质谱和Compound composer软件进行筛查和半定量计算,同时以气相色谱-质谱法在选择离子模式下对Compound composer软件的半定量结果进行验证,结果表明除3-氨基苯酚、豆甾醇和β-谷甾醇外,其它物质的回收率在74％～102％之间,保留时间偏差为-0.158 ～0.049 min,对添加量为1.0μg目标物的水样半定量,结果偏差在-0.48～0.62 μg之间.在无标准样品的条件下,利用Compound composer软件及其自带含近千种化合物标准曲线的数据库,对江苏省南通、苏州和无锡三市的地表水环境样品进行监测,筛查其中主要的有机污染物,并进行半定量计算.三市地表水样中共检出47种有机污染物.2,6-二叔丁基-4-甲基苯酚为检出浓度最高的化合物,其浓度达140 μg·L-1,酞酸酯类和多环芳烃类物质普遍存在,其单体浓度范围分别为1.7～48μg·L-1和0.13 ～9.6 μg· L-1.依照GB3838-2002《地表水环境质量标准》,三市地表水体中酞酸酯类严重超标,水体中总有机物污染状况应引起关注.     

Determination of 48 fragrance allergens in toys using GC with ion trap MS/MS

This paper presents a method for the simultaneous determination of 48 fragrance allergens in four types of toys (plastic toys, play clays, plush toys, and paper toys) based on GC with ion trap MS/MS. Compared with single‐stage MS, MS/MS is superior in terms of the qualification and quantification of a large range of compounds in complicated matrices. Procedures for extraction and purification were optimized for each toy type. The method proved to be linear over a wide range of concentrations for all analytes with correlation coefficients between 0.9768 and 0.9999. Validation parameters, namely, LODs and LOQs, ranged from 0.005–5.0 and from 0.02–20 mg/kg, respectively. Average recoveries of target compounds (spiked at three concentration levels) were in the range of 79.5–109.1%. Intraday and interday repeatabilities of the proposed method varied from 0.7–10.5% and from 3.1–13.4%, respectively. The proposed method was used to monitor fragrance allergens in commercial toy products. Our findings indicate that this method is an accurate and effective technique for analyzing fragrance allergens in materials composed of complex components.     

土壤中64种痕量半挥发性有机污染物的分析方法研究

利用超声提取技术将土壤中的半挥发性有机污染物(SVOC)提取出来, 经旋转蒸发浓缩至一定体积后, 用ODSC18柱净化, 再用氮吹浓缩后, 取1.0 μL注入气相色谱中, 用DB-5 ms柱分离, 用气相色谱质谱仪(GC-MS)进行定性定量分析. 本方法研究土壤中64种半挥发性有机污染物, 其中包括苯系物、苯酚类、苯胺类、硝基芳香烃类、氯代芳烃类、多环芳烃类和酞酸酯类等物质的提取、净化方法以及回收率、精密度和检测限的测定. 该方法回收率为52.5%～105%.     

Strategies for compound identification and quantification using fused silica capillary column GC/MS

A test mixture containing 28 compounds plus their stable isotopically labeled analogs was analyzed on a daily basis for one month during a series of routine fused silica capillary column GC/MS analyses in order to establish the precision with which retention times and responses were produced. These long-term precision data were evaluated to determine how to best predict retention times and how to best reproduce quantification. Results clearly indicate that relative retention times should be calculated using the reference compound eluted most closely to the target compound and that quantification should be based on relative response using a chemically “similar” compound.     

气相色谱/质谱/质谱法分析石油基引燃物

应用Ｖａｒｉａｎ ３８００ ＧＣ／Ｓａｔｕｒｎ ２０００ ＭＳ 气相色谱／质谱联用分析仪（简称ＧＣ／ＭＳ／ＭＳ）对以汽油、煤渍和紫油为引燃物，燃烧聚丙稀化纤地毯和土壤时的模拟现场物品进行了引燃物的检出。发现采用ＧＣ／ＭＳ／ＭＳ方法比用ＧＣ／ＭＳ方法可以较彻底地排队由于柱注失、地毯燃物分解产物、土壤背景产物和地毯增塑剂等引起的干扰，而且可以提高检测灵敏度。详细考察了以不同质荷比的离子作母离子时对ＧＣ     

微波萃取-GC/MS联用法测定橡胶及其制品中多环芳烃

建立了微波萃取-GC/MS联用法测定橡胶及其制品中16种多环芳烃(PAHs)的方法,通过实验优化了萃取溶剂、萃取时间、萃取温度等微波萃取条件和16种PAHs的分离和测定条件。用加标回收方法试验确定方法的准确度。结果表明:16种PAHs检出限(S/N=5)为0.002~0.01 mg/L,平均回收率为63.58%~100.5%,RSD为1.9%~9.9%。该方法可以满足橡胶及其制品中多环芳烃的检测要求。     

纤维素酶前处理没药挥发油成分的GC/MS分析

采用水蒸汽蒸馏法分别从未处理和纤维素酶前处理的没药中提取挥发油,利用气相色谱-质谱(GC/MS)联用技术对其挥发油成分进行分析。从中分别鉴定出38种和34种化学成分,用峰面积归一法通过数据处理系统得出各化学成分在挥发油中的质量分数,占挥发油总成分的67.95%和70.05%。     

Determination of acetone in seawater using derivatization solid-phase microextraction

Acetone plays an important role in the chemistry of both the atmosphere and the ocean, due to its potential effect on the tropospheric HO_x (= HO + HO₂) budget, as well as its environmental and health effects. We discuss the development of a mobile, sensitive, selective, economical and facile method for the determination of acetone in seawater. The method consists of derivatizing acetone to its pentafluorobenzyl oxime using 1,2,3,4,5-pentafluorobenzylhydroxylamine (PFBHA), followed by solid-phase microextraction (SPME) and analysis by gas chromatography/mass spectrometry (GC/MS). A detection limit of 3.0 nM was achieved. The buffering capacity of seawater imposes challenges in using the method’s optimum pH (3.7) on seawater samples, requiring calibration standards to be made in buffered salt water and the acidification of seawater samples and standards prior to extraction. We employed the technique for analysis of selected surface seawater samples taken on the Nordic seas during the ARK-XX/1 cruise (R.V. Polarstern). An upper limit of 5.5–9.6 nM was observed for acetone in these waters, the first acetone measurements reported for far North Atlantic and Arctic waters. Simplified schematic of transformations of organic compounds at the atmosphere–ocean interface     

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.