Photocatalytic oxidation of aqueous trichloroethylene using dye sensitized buoyant photocatalyst monitored via micro-headspace solid-phase microextration gas chromatography/electron capture detection and mass spectrometry

Trichloroethylene (TCE), a useful industrial agent which unfortunately exhibits carcinogenic properties, has become an extremely prevalent environmental contaminant. As such, new rapid, sensitive, and cost effective detection methods are needed for the identification of potential point sources of contamination. A new analytic micro-headspace method is described, utilizing solid phase micro-extraction (SPME) fibers and routine gas chromatography/electron capture detection (GC/ECD) for the detection of TCE to the 3.89 ppb level in aqueous samples. The polydimethylsiloxane (PDMS) fiber was shown to have the greatest analytical promise, with excellent sensitivity and minimal carry over. This method was employed in the monitoring of the photo-oxidation of TCE using buoyant TiO₂ coated microspheres, which were sensitized using natural anthocyanin dyes obtained from fruits. Solar mediated photo-oxidation was shown to be a successful method for the removal of aqueous organic contaminants. The dye sensitized system yielded excellent remediation with 93% of the TCE removed from the system within 12 h. As irradiation was executed, overall TCE concentrations were reduced, while the expected mineralization product of hydrochloric acid was produced. The micro-headspace SPME procedure described here, offers considerably improved sensitivity, with orders of magnitude improvement in method detection limits, over previously published micro-headspace methods.     

调味品中氯丙醇的GC/ECD和GC/MS/MS衍生化检测方法研究及应用

报道了调味品中氯丙醇的衍生化气相色谱(GC／ECD)和衍生化气相色谱双串联质谱法(GC／MS／MS)测定。GC／ECD测定酱油中3—氯—1，2—丙二醇(3—MCPD)的检出限达到0．01mg／kg，回收率为91％～104％，变异系数为2．27％～7．96％；GC／MS／MS同时测定酱油中1，3—二氯—2—丙醇、2，3—二氯—1—丙醇和3—氯—1，2—丙二醇，1，3—二氯—2—丙醇、2，3—二氯—1—丙醇的检出限为0．02mg／kg，3—氯—1，2—丙二醇的检出限为0．01mg／kg，回收率在92％～106％，变异系数为3．51％～13．33％。     

Identification of arsenolipids with GC/MS

Arsenic-containing hydrocarbons have recently been reported as natural constituents of fish oil. We report a simple method for determining these compounds by GC/MS. Application of the methodology will delineate the distribution of these novel arsenic compounds in foods, and facilitate an assessment of the toxicological implications.     

硒芳香杂环化合物的GC/MS分析

本文对合成的7种含硒芳香杂环化合物进行了GC／MS分析研究。结果表明：BS、MB、BBS和DBBS等4个化合物在色谱柱内的保留时间与它们的相对分子质量呈线性关系。所有化合物均可获得特征质谱,表现出含单个硒原子的分子离子或碎片离子特征峰簇,硒的两种主要同位素在峰簇中表现为主要峰M与（M-2）的相对丰度比约为2：1,可为鉴定含硒分子离子或碎片离子提供重要信息。新化合物1,2,5-硒二唑并[3,4-d]嘧啶-5,7-（4H,6H）二酮（SPDO）在色谱柱内出现11．83min和7．96min两个具有相同的质谱的色谱峰,被认为是互变异构体的峰。     

微波辅助萃取-GC/MS联用分析竹子中氨基酸

建立了微波辅助萃取-GC/MS联用测定竹子中谷氨酸、天冬氨酸和苯丙氨酸等10种氨基酸的分析方法, 优化了微波辅助萃取条件, 方法的线性范围在0.100～100 μg/mL之间, 检出限在0.0098～0.36 μg/mL之间, RSD为4.1%～9.7%, 回收率在84.3%～118%之间. 分析了4种不同产地、竹龄竹子的竹叶、竹枝和竹沥中氨基酸含量. 结果表明, 不同竹种、产地及竹龄的竹子中氨基酸总量有较大差异;相同竹种其竹沥中氨基酸含量显著高于竹叶及竹枝中氨基酸含量.     

Simultaneous profiling of multiple neurochemical pathways from a single cerebrospinal fluid sample using GC/MS/MS with electron capture detection

Biogenic amines and amino acids are widely characterized in the pathways representing neurotransmission. Although several analytical methodologies have been used to detect specific target molecules in relevant fluids such as cerebrospinal fluid (CSF), multiple assays must be used to survey the primary pathways involved. This article describes the development of a GC/MS/MS method capable of analyzing up to 43 analytes (representing 20 amino acids and more than seven neurochemical pathways) from a single 50 microl CSF sample. In this procedure, a CSF sample is first treated with acetonitrile to precipitate proteins. The dried sample is then derivatized with a mixture of 2,2,3,3,3-pentafluoro-1-propanol and pentafluoropropionic acetic anhydride to replace all active hydrogen atoms with fluorine-containing groups. Due to the concentration difference between amino acids and neurotransmitters, these two compound classes are analyzed in separate injections of the same derivatized extract. The total run time for each injection is approximately 15-20 min. An essential feature of the method is the use of argon as a reagent gas for electron capture chemical ionization (ECCI), as the use of the more traditional gas (methane) lacked sufficient durability to be considered for use with the present instrumentation. This article describes the development of this method including a detailed investigation of the chemical ionization conditions used. The resultant conditions allow for the profiling of biogenic amines (e.g. serotonin, norepinephrine, and dopamine) in the low picogram per milliliter range.     

GC/MS和ESI/MS/MS同位素内标法检测甲基丙二酸血症

以甲基丙二酸血症为对象,分别用GC/MS和ESI/MS/MS方法对该疾病进行了定性和定量检测.通过对样品前处理和分离条件的改善,对疾病的标识化合物之一甲基丙二酸进行了定量测定,其稳定性、精密度和回收率结果很好.同时比较了GC/MS和ESI/MS/MS两种方法的特点,发现两种方法的结合不仅可满足新生儿代谢疾病筛查的要求,同时还可对高危人群进行诊断.     

GC/MS测定锅巴中丙烯酰胺含量

建立了一种测定市售锅巴中的丙烯酰胺含量的方法.该法样品前处理不必经过溴化衍生,样品脱脂后用水提取丙烯酰胺,提取液过活性炭柱,再用乙酸乙酯将活性炭柱中吸附的丙烯酰胺洗脱.洗脱液浓缩后经气相色谱-质谱(GC-MS)定量分析,检测限为0.06 mg/kg,适合测定市售锅巴中的丙烯酰胺的含量.还考察了丙烯酰胺在水的固液两相中的分配比.     

生物样品中苯丙胺类毒品的小体积液相萃取及GC/MS分析

小体积液相萃取;苯丙胺毒品;唾液;毛发;GC/MS     

乙酰乙酸乙酯烯醇式与酮式GC/MS和GC/IR分析

采用ＧＣ／ＭＳ对乙酸乙酯烯醇式在不同离子源温度,接口温度,进样器温度,柱温等条件下的气相色谱行为进行了研究,用重氢交换法和高分辨质谱法对烯醇式和酮式的质谱进行了解析,并通过ＧＣ／ＩＲ研究了烯醇式和酮式的红外光谱。     

有机硅烷KH—550的气相色谱／质谱分析

对硅-550交联剂的组分进行了研究报道。通过GC对样品进行了研究分析,得到了七个分离很好的色谱峰以及样品中各组分的含量,再利用GC/MS联用技术和质谱裂解规律鉴定出样品各组分的分子结构。     

固相微萃取/气相色谱/质谱联用技术在农药残留物分析中的应用

综述了固相微萃取／气相色谱／质谱（SPME／GC／MS）在各种环境水、土壤等样品中农药残留分析中的应用和发展。SPME／GC／MS联用技术具有快速、简便、准确等优点。     

GC/MS方法分析豇豆中水胺硫磷等37种农药残留

建立了GC/MS法同时测定豇豆中水胺硫磷等37种农药残留的方法.农药经过乙腈提取,NH2/CARBON复合固相萃取小柱净化,HP-5MS(30 m×0.25 mm×0.25 μm)弹性石英毛细管柱分离后,用GC/MS选择离子模式进行测定.农药在0.020～0.500 mg/L时与峰面积有良好的线性关系(r2>0.990...     

Analysis of anabolic steroids in hair by GC/MS/MS

A simple and sensitive gas chromatography/tandem mass spectrometry (GC/MS/MS) method is described for the detection of anabolic steroids, usually found in keratin matrix at very low concentrations. Hair samples from seven athletes who spontaneously reported their abuse of anabolic steroids, and in a single case cocaine, were analyzed for methyltestosterone, nandrolone, boldenone, fluoxymesterolone, cocaine and its metabolite benzoylecgonine. Anabolic steroids were determinate by digestion of hair samples in 1 m NaOH for 15 min at 95 degrees C. After cooling, samples were purificated by solid-phase and liquid-liquid extraction, then anabolic steroids were converted to their trimethylsilyl derivative and finally analyzed by GC/MS/MS. For detection of cocaine and benzoylecgonine, hair samples were extracted with methanol in an ultrasonic bath for 2 h at 56 degrees C then overnight in a thermostatic bath at the same temperature. After the incubation, methanol was evaporated to dryness, and benzoylecgonine was converted to its trimethylsilyl derivative prior of GC/MS/MS analysis. Results obtained are in agreement with the athletes' reports, confirming that hair is a valid biological matrix to establish long-term intake of drugs.     

固相微萃取-气相色谱/质谱联用分析室内空气中的苯系物

自制了一种固相微萃取采样装置,建立了固相微萃取-气相色谱/质谱(SPME-GC/MS)联用测定室内空气中苯系物的分析方法。方法的线性范围为1~300μg/m3,检出限为0.1~0.3μg/m3,RSD(n=6)3.2%~15%。采用该方法研究了广州市内20户新装修民居中苯、甲苯、乙苯、对二甲苯和1,3,5-三甲苯的含量及分布,并探讨了苯系物的来源。     

GC/MS Analysis of Polymethoxyflavones in Citrus Oils

The cold pressed peel oils of three species of citrus fruit, viz. sweet orange, tangerine, and grapefruit, have been examined for polymethoxyflavones by GC and GC-MS. Four GC column stationary phases were compared and separation of the six predominant orange oil polymethoxyflavones was obtained isothermally at 310°C in under ten minutes, including the resolution of the polymethoxyflavones from β-sitosterol. The nature of the stationary phase and the analysis temperature exercise dramatic effects on the resolution and elution order of the components, DB-35ms providing the best overall separation. A temperature programmed separation is also presented and the polymethoxyflavone composition of all three oils, as determined by GC-MS, is described. This is the first reported GC-MS study of the PMFs of these citrus species. While tangerine oil is as rich in polymethoxyflavones as orange oil, they are less abundant and occur at lower concentrations in grapefruit oil. Hydroxy-polymethoxyflavones were identified by GC-MS in tangerine oil. One hydroxy-pentamethoxyflavone, M⁺ = 388, identified in tangerine was also present at low levels in both orange and grapefruit oils. These results are compared with previous studies utilizing HPLC and GC.     

采用配备GPC纯化装置的GC/MS进行农产品中农药残留的快速分析

本文采用GPC-GC／MS在线连接系统和固相萃取的方法快速测定农产品中的农药残留。该方法首先用液-液分配法从均化的食物样品中提取农药,然后用PSA结合相进行固相萃取,最后进行GPC-GC／MS分析。GPC-GC／MS系统包括一套GPC净化装置,可以简化样品前处理步骤。把浓度为0．1 μg／g的97种农药添加到马铃薯、甘蓝和胡萝卜中,得到了比较好的回收率。整个分析过程大约需要50 min。     

红景天挥发油的GC／MS／DS和GC／IR／DS研究

红景天挥发油的ＧＣ／ＭＳ／ＤＳ和ＧＣ／ＩＲ／ＤＳ研究阎吉昌，张宏徐少敏卫永弟，阎雪（东北师范大学测试中心，长春，１３００２４）（吉林省石油化工研究院，白求恩医科大学）关键词红景天，色谱／质谱，色谱／红外，复杂有机混合物应用色谱／质谱／计算机（ＧＣ／Ｍ...