Determination of 7 Indictor Polychlorinated Biphenyls (PCBs) Residues in Porphyra by Ultrasonic Extraction and Gas Chromatography (GC)

A method was developed for determination of 7 indictors the polychlorinated biphenyls (PCBs) residues in porphyra by gas chromatography (GC) with electron capture detector (ECD). The PCBs were extracted with hexane/methylene chloride (1:1, v/v) by ultrasonic extraction and the samples were cleaned up by concentrated sulfuric acid and Alumina-N solid phase extraction cartridge. The analytes were quantified by an internal standard method. Under optimal experimental conditions, good linearity was observed in the range of 5 - 200 ng/mL and the correlation coefficients were 0.9994 - 0.9998. The limit of quantitation (LOQ) for target analytes ranged from 6.0 to 10.0 μg/kg. At the spiked levels of 10, 50, 100 μg/kg, the average recoveries ranged from 90.9% to 102% with the relative standard deviations 2.12% - 6.32%. The result showed that the proposed method was rapid, and could be used for the determination of the PCBs in porphyra.

Capillary gas chromatographic determination of dimethachlon residues in fresh tobacco leaves and cut-tobacco

Simple procedures for extraction and chromatographic determination of dimethachlon residues in fresh tobacco leaves and cut-tobacco are described.The determination was carried out by capillary gas chromatography(GC) with electron capture detection(ECD) and confirmed by GC-MS.The mean recoveries and relative standard deviation(RSD) were 93.2%～112.9% and 3.5%～6.7%,respectively at levels ranging from 0.01 to 0.1 mg/kg.The limit of determination was 0.001 mg/kg.Tobacco samples in routine check were successfully analyzed using the proposed method.

Analysis of residual crosslinking agent content in UV cross-linked poly(ethylene oxide) hydrogels for dermatological application by gas chromatography

Acrylates have been widely used in the synthesis of pharmaceutical polymers. The quantitation of residual acrylate monomers is vital as they are strong irritants and allergens, but after polymerization, are relatively inert, causing no irritation and allergies. Poly(ethylene oxide)(PEO) hydrogels were prepared using pentaerythritol tetra-acrylate(PETRA) as UV crosslinking agent. A simple, accurate, and robust quantitation method was developed based on gas chromatographic techniques(GC), which is suitable for routine analysis of residual PETRA monomers in these hydrogels. Unreacted PETRA was initially identified using gas chromatography–mass spectrometry(GC–MS). The quantitation of analyte was performed and validated using gas chromatography equipped with a flame ionization detector(GC–FID). A linear relationship was obtained over the range of 0.0002%–0.0450%(m/m) with a correlation coefficient(r2)greater than 0.99. The recovery( 4 90%), intra-day precision(%RSD o 0.67), inter-day precision(%RSD o2.5%), and robustness(%RSD o1.62%) of the method were within the acceptable values. The limit of detection(LOD) and limit of quantitation(LOQ) were 0.0001%(m/m) and 0.0002%(m/m), respectively.This assay provides a simple and quick way of screening for residual acrylate monomer in hydrogels.

Effective and inexpensive gas chromatography method for detection of trace level SO_2 in H_2 fuel

Gas chromatography （GC） analysis of sulfer dioxide is challenging because SO2 is a highly mobile and chemically active molecule. For the conventional GC method with flame photometric detector （FPD） and direct-injection, it is often ineffective particularly when the SO2 level is as low as on the trace level. In this paper, a modified GC system integrated with an adsorption-desorption device was developed to detect the trace SO2 impurity in H2 fuel. Adsorbent GDX-502 is used in the adsorber to adsorb/collect SO2 from the sample gas and desorb/release it in a concentrated flow so that the conventional GC at downstream could detect it with an acceptable accuracy.

基于GC×GC-TOF MS对太湖流域水体中有机物的非靶标识别

本研究基于全二维气相色谱-飞行时间质谱(GC×GC-TOF MS),采用非靶标筛选法分析太湖流域18个采样点的水样,通过特征离子峰、精确质量数、保留指数偏差和NIST谱库匹配,共识别出466种有机物,其中各采样点共有检出率超过80%的化合物有68种,主要是香精香料、工业化学品和多用途化合物,并识别出多种尚未纳入监管清单的化合物,如顺式-11-二十烯酰胺、地塞诺和γ-谷甾醇。对非靶标方法识别的化合物进行半定量计算,发现各类化合物的单体浓度在0.025~113.145μg/L之间波动,其中浓度较高的是顺式-11-二十烯酰胺、邻苯二甲酸二丁酯和地塞诺。通过聚类分析发现,新塘港和小梅口点位的水体污染较轻,主要受涂料行业排放的影响,其余采样点位污染较重,主要受工业和食品加工业的影响。此外,本研究还对检出的68种有机物的半定量浓度进行初步的生态风险评估,发现有22种污染物具有中等以上生态风险,其中的11种污染物具有高生态风险,这为评估水体有机物健康效应提供了参考。

自动固相微萃取(SPM E)GC-MS、GC-MS-MS法检测环境水中有机磷杀虫剂的研究

固相微萃取(solid-phase microextraction,SPME)是20世纪90年代发展起来的一种样品前处理技术,与传统的液-液提取、液-固提取相比,SPME更适用于提取、浓缩液态或气态的挥发性和半挥发性物质,SPME技术可将采样、萃取、浓缩和样本引入集中于一个步骤完成,尤其随着自动SPME与GC-MS等联用技术的日益完善,使SPME技术优点得到更充分的发挥.……

广防己挥发油的GC-MS指纹图谱研究

防己药材主要分粉防己和木防己两类,木防己包括广防己和汉中防己.广防己为马兜铃科植物广防己Aristolochia fangchi Y.C.WuexL.D.Chou.et S.M.Hwang的干燥根[1],习称"木防己"、"水防己",主产于广东、广西,具有祛风止痛、清热利水之功效[2].……

GC-MS Analysis of Essential oil and n-Hexane Extract from Moso Bamboo

[Objective] This study aimed to analyze the chemical composition and yield of essential oil and n-hexane extract from moso bamboo to find active compounds with potential value. [Method] Essential oil and n-hexane extract were respectively extracted from moso bamboo of four different ages by using hydrodistillation and ultrasonic-assisted extraction with n-hexane, and analyzed with gas chromatography/mass spectrometry （GC/MS）. [Result] The results show that cedrol （46.39%） is the first principal volatile component in essential oil of the middle stem of 7-year old moso bamboo; dibutyl phthalate （59.46%） is the first principal volatile component in n-hexane extract of the middle stem of 3-year old moso bamboo; yield of n-hexane extract is higher than that of essential oil from moso bamboo. [Conclusion] Cedrol is an active compound with potential value.

便携式快速GC程序升温中智能PID算法研究

针对快速气相色谱仪(GC)在程序升温时,由于色谱柱低热容,导致升温的线性度和超调难以控制,影响仪器的可重复性,产生峰重叠的问题,开发了一种基于智能比例-积分-微分(PID)算法的色谱柱温控系统。系统选用LTM柱,以该柱自带的铂测温丝作为温度传感器元件,设计了温度采集和控制电路。算法上,在增量式PID的基础上,将目标温度段划分为多个子区间段,引入温度补偿控制,补偿值的大小与升温速率呈线性关系。实验结果表明:补偿后,算法升温速率误差为2.58%,线性度达到99.92%,超调在3℃以内,满足系统需求。

A GC×GC-ToFMS Investigation of the Unresolved Complex Mixture and Associated Biomarkers in Biodegraded Petroleum

Heavy biodegraded crude oils have larger numbers of coeluting compounds than nonbiodegraded oils, and they are typically not resolved with conventional gas chromatography（GC）. This unresolved complex mixture（UCM） has been investigated using comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry（GC×GC-To FMS） within a set of biodegraded petroleums derived from distinct sedimentary basins, including northwestern Sichuan（Neoproterozoic, marine）, Tarim（Early Paleozoic, marine）, Bohai Bay（Eocene, saline/brackish） and Pearl River Mouth（Eocene, freshwater）. In general, the hydrocarbons that constitute the UCM in petroleum saturate fractions can be classified into three catalogues based on the distributions of resolved compounds on two dimensional chromatograms. Group 1 is composed mainly of normal and branched alkanes, isoprenoid alkanes and monocyclic alkanes; Group 2 comprises primarily terpanes ranging from two to five rings, and Group 3 is dominated by monoaromatic hydrocarbons such as tetralins and monoaromatic steranes. In addition, the UCM is source dependent and varies between oil populations. i.e., the UCM of petroleum derived from Precambrian and Early Paleozoic marine, Eocene saline/brackish and freshwater source rocks is specifically rich in higher homologues of A-norsteranes, series of 1,1,3-trimethyl-2-alkylcyclohexanes（carotenoid-derived alkanes）, and tetralin and indane compounds, respectively.

Determining organic compounds in coking wastewater by SPME-GC /MS

The solid-phase microextraction （SPME） combined with gas chromatography/mass spectrometry （GC/MS） was used to determine and analyze organic pollutants in coking wastewater. Based on the fact that the main compounds in the wastewater were organics, some key parameters of the SPME were optimized. The method has good linearity （ its correlation coefficients 〉 0.99） in the range determined,its relative standard deviations （RSD） are less than 15%, and its recovery is from 87.9% to 128.1% with the lowest quantification limit of 5 ~g/L. This method has been used to measure 15 organic pollutants in wastewater from a certain coking plant. The results show that compared with the conventional method,it can save an hour in pretreatment time. It is a fast, low-cost, accurate, simple and efficient analytical method indeed.

用快速高效液相色谱系统分离纯化Gc蛋白

报告Gc蛋白的一种分离方法，为免疫制备抗Gc血清制备抗原。硫酸该分级沉淀出含Gc的人血清组份，BlueSepharoseCL－6B亲和色谱除去含Gc硫酸铸分级沉淀的人血清组份中的白蛋白，快速高效液相色谱系统过Alkyl-SuperoseTMHR5／5疏水色谱柱和MonoQHR5／5离子交换柱。聚丙烯酸胺凝胶解离、非解离电泳证明，Gc蛋白得到了彻底纯化。免疫固定显示：纯化出的蛋白确实是Gc蛋白．为1-1型。快速高效液相色谱为蛋白质的纯化提供了新的技术及仪器手段。

Analysis on Volatile Components of Flowers and Leaves of Thymus mongolicus by SPME-GC/MS

[Objectives] To analyze volatile components of flowers and leaves of Thymus mongolicus. [Methods]Volatile components of collected T. mongolicus flower and leaves were separated by headspace solid-phase microextraction( SPME) and identified by gas chromatography/mass spectrometry( GC/MS) and normallized by peak area. [Results] A total of 24 and 14 compounds were identified from flowers and leaves of T. mongolicus in the total ion chromatogram,accounting for 99. 573% and 97. 187% of the total peak area,respectively. Main components of flowers and leaves of T. mongolicus include phenols and terpenes,and thymol accounts for 35. 38% and 49. 13% of flowers and leaves of T. mongolicus,respectively. [Conclusions] SPME-GC/MS can be applied in analyzing volatile components of flowers and leaves of T. mongolicus,to provide basis for further development and utilization of T. mongolicus.

快速响应的微型色谱柱及GC谱线拟合方案

采用激光刻蚀技术加工1 mm厚硅双面抛光片实现了蛇形沟道布局的微型色谱柱嵌刻基底,经涂覆固定相、封装后加工制作成新型嵌刻基底的微型色谱柱。该工艺具有加工周期短、成本低的优势。该新型色谱柱在甲醇与二氯甲烷的混合物的分离实验中能够快速响应,二氯甲烷和甲醇的保留时间分别为0.943 min和4.547 min。针对气相色谱(GC)谱线存在的色谱重叠峰问题,采用Nelder-Mead算法进行高斯曲线拟合,选择MATLAB函数通过迭代找到最优解,该算法结构简单,能够分离出清晰的高斯峰。该拟合方案对双高斯峰的重叠色谱图拟合度达到0.977,误差率为2.482%。

Using GC to determinate polychlorinated biphenyls in soil after pretreated with microwave-assisted alkaline degradation method

A new and simple microwave-assisted alkaline degradation （MAAD） method for the elimination of organoehlorine-pesticide interference on the determination of polychlorinated biphenyls （PCBs） in soil by GC is presented. Under the optimal conditions, the interference of α- HCH, β- HCH, γ -HCH,δ -HCH, o. p＇ - DDT, p. p＇ - DDD and p. p＇ - DDT could be eliminated completely, and p. p＇ - DDE, Aldrin and Dieldrin could be partially eliminated; however, Dieldrin could be completely eliminated by using concentrated sulphurie acid. The method was evaluated by analyzing the spiked-soil sample. The mean recovery obtained was 84. 1% and the Relative Standard Deviation （RSD） was 2. 7%. Experimental results also indicate that the degradation of the interference and the extraction of the target analytes, PCBs, could be carried out simuhaneously. Compared with the traditional methods, the MAAD method is a rapid, efficient and solvent-saving method,

Test on oxygen and benzene contents in gasoline by mid-infrared spectroscopy

This paper aims at testing oxygen and benzene contents in gasoline by mid-infrared spectroscopy.The experimental results prove that infrared spectroscopy(IR)is reliable.Compared with gas chromatography(GC)technology,this paper draws a conclusion that IR has several advantages,including rapid analysis,excellent repeatability and low analysis cost.

生物质快速裂解液体产物的分析

应用萃取及柱层析的分离方法将生物质快速裂解油分离成 4种组分 :烷烃、芳烃、极性组分和难挥发性组分 ;并应用气相色谱、气相色谱 -质谱、核磁共振等现代分析测试技术 ,对水相和油相中各分离组分分别分析和鉴定 。

阀切换技术在大气样品中六氟化硫快速分析中的应用

建立了双柱阀切换技术分析大气样品中的SF6含量的气相色谱-电子捕获检测器（GC-ECD）检测方法。采用规格为3.2mm×1m的5A分子筛（40-60目）柱为预柱,规格为3.2mm×0.5m的5A分子筛（60-80目）柱为分析柱。在所用实验条件下,平均峰高响应为1.08×10^-14mL/μV,SF6单位体积进样量的色谱峰高的相对标准偏差为2.2%,SF6的最低检测限为6.03×10^-13mL（3倍基线噪声）。采用该方法分析大气中SF6的含量,样品分析时间为1.2min,于12min内完成11个空气样品的分析,SF6含量的相对标准偏差2.1%。

QuEChERS-在线凝胶色谱-气相色谱-质谱法测定大米、黍子和小麦中34种农药残留

采用QuEChERS方法结合在线凝胶色谱-气相色谱-质谱（GPC-GC-MS）系统,建立了大米、黍子和小麦中34种中高毒农药的快速筛查方法。研究了称样量、萃取剂、净化吸附剂种类对大米样品提取净化效果的影响并考察了基质效应和分析保护剂的使用效果,采用选择离子监测（SIM）模式,外标法定量。结果表明,34种农药在大米、黍子和小麦中的检出限分别为0.028 1~5.30、0.028 2~4.82、0.027 3~5.13μg/kg;在0.05μg/g添加水平的平均回收率分别为94.5%~117.1%、83.1%~121.7%、93.1%~120.2%;相对标准偏差（RSD,n=6）分别为2.6%~14.5%、3.4%~15.1%、3.5%~15.2%。该方法消耗试剂少,分析成本低,符合绿色化学的理念,具有操作便捷、快速、通用性强等特点,适用于大米、黍子和小麦中34种农药残留的快速筛查与检测。