手性药物气相、液相色谱拆分法及其在体内药分中的应用

“手性”系一种化学特征,它引起分子的不对称性。不能与镜象体重合的称为手性分子,即对映异构体,有光学活性。药物的构型与药理作用的关系很密切,然而人工合成品往往是外消旋体。虽然人们力图运用不对称合成直接制备光活性化合物,但目前大多数情况下,还不可能只获得某种单旋体。药物的消旋体引入人体后,其对映体分子均由体内具手性的蛋白质、酶和受体,以两个完全不同的分子处理。因而,药物对映体在体内可具有不同的代谢途径和药理作用。

PTT纤维与PET纤维鉴别方法的研究

在已知PTT和PET纤维基本结构与性能的基础上,用密度法、熔点法、差热分析法和气相色谱分析法对PTT和PET纤维进行了试验、观察与比较,有效地鉴别出了2种纤维。证明4种方法都可用于PTT和PET纤维的定性鉴别,并分析比较了各方法的优缺点。

Classification of Chinese Traditional Drug-"Beimu" (Bulbus Fritillariae) by Pyrolysis High Resolution Gas Chromatography-Pattern Recognition

The combination of pyrolysis high resolution gas chromatography and pat- tern recognition techniques is a powerful tool for the classification of traditional Chinese drug.A study has been completed on 55 Beimu samples of five different geographic origins: Eastern China.Central China.South-western China,North-western China and North-eastern China.Principal component analysis and SIMCA are applied to effectively classifying the samples according to the origin of the plants.The chemical information contained in the high resolution gas chromatographic data is sufficient to characterize the geographic origin of sam- pies.

Analysis of Active Components of Hexane Extractives of Morus alba Leaves

[Objective]The aim was to explore the active compound of Morus alba leaves with the analysis of active components of hexane extractives of M.alba leaves.[Method]Antibacterial assays of hexane extractives of M.alba leaves were done and the volatile components of hexane extractives of M.alba leaves with the strongest antibacterial activity were analyzed by gas chromatography-mass spectrometry（GC-MS）.[Result]The results of inhibitory effect of hexane extractives of M.alba leaves on Staphylococcus aureus and Escherichia coli showed that hexane extractives of M.alba leaves collected in June,July and August had antibacterial activity against S.aureus and had no antibacterial effect against E.coli.Furthermore,hexane extractives of M.alba leaves collected in June had the strongest antibacterial activity against S.aureus（inhibition diameter 10.95 mm）.The hexane extractives of M.alba leaves collected in June was analyzed by GC-MS,the main volatile components were tetradecane（16.76%）,dodecane（13.20%）,diisobutyl phthalate（10.26%）,decane（9.10%）,hexadecane（8.71%）,linolenyl alcohol（7.25%）,octadecane（5.88%）,eicosane（3.26%）,dibutyl phthalate（2.59%）.[Conclusion]Linolenyl alcohol was the potential antibacterial compound.

Determination of constituents of essential oil from Angelica sinensis by gas chromatographymass spectrometry

Gas chromatographymass spectrometry (GC-MS) coupled with chemometric resolution upon two- dimensional data was employed to analyze the constituents of essential oils of Angelica sinensis. Constituents in essential oils of Angelica sinensis root were identified by GC-MS with the help of subwindow factor analysis (SFA) method resolving two-dimensional original data into mass spectra and chromatograms. 76 of 97 separated constituents in essential oil of Angelica sinensis root were identified and quantified, and they account for about 91.36% of the total content. The results show that ligustilide, butylene phthalide, 2-methoxy-4-vinylphenol, carvacrol, allo-ocimene,2,6,6-trimethylbicyclo-[3,1,1]hept-2-ene are the main constituents in essential oil of Angelica sinensis root.

Measurement of Infinite Diluted Activity Coefficient of Solvents in Polymer by Inverse Gas Chromatography Method

The infinite diluted activity coefficients of solvents in polyisopropyl methylacrylate was measured using inverse gas chromatography. The solvents used were benzene, toluene, ethyl benzene, methyl acetate, ethyl acetate, propyl acetate, butyl acetate, methanol, ethanol isopropyl alcohol, butyl alcohol, 1,2-dichloroethane, and chloroform. It was observed that the infinite diluted activity coefficient of alcohols are well above those of the other solvents investigated.

Chemical Composition of Essential Oil from Chimonanthus praecox Flower

Objective] To analyze the aroma constituents of essential oils from Chi-monanthus praecox. [Method] Extracted by microwave-assisted hydrodistil ation （MAHD）, aroma constituents of essential oils of Chimonanthus praecox flowers were analyzed by gas chromatography-mass spectrometry （GC-MS）. Normalization method was used to determine the constituents quantitatively. [Result] Total y 27 compounds were identified, accounting for 98.85% of total amounts. The main aroma con-stituents are terpenes, aldehydes, esters, alcohols and hydrocarbons. Main compo-nents with relative percentage over 5% are germacrene D （25.62%）, bornyl acetate （16.71%）, caryophyl ene （10.51%）, cis-α-ocimene （5.18%）, γ-elemene （8.05%）, β-linalool （5.01%）, 1-ethenyl-1-methyl-2,4-bis （1-methylethenyl）-cyclohexane （7.18%） and 2,3,4,4α,5,6-hexahydro-1,4αdimethyl-7-（1-methylethyl）-naphthalene （5.20%）. [Conclu-sion] The study provided a theoretical reference for the development and utilization of Chimonanthus praecox resources.

Diethylstilbestrol in Fish Tissue Determined Through Subcritical Fluid Extraction and with GC-MS

As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol(DES) in fish tissue using subcritical 1,1,1,2-tetrafluoroethane(R134a) extraction in combination with gas chromatography-mass spectrometry(GC-MS). After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C_(18) and NH_2 solid phase extraction(SPE). Finally, the analyte was derived by heptafluorobutyric anhydride(HFBA), followed by GC-MS analysis. Response surface methodology(RSM) was employed to optimizing the extraction condition, and the optimized was as follows: extraction pressure, 4.3 MPa; extraction temperature, 26℃; amount of co-solvent volume, 4.7 m L. Under this condition, at a spiked level of 1, 5, 10 μg kg^(-1), the mean recovery of DES was more than 90% with relative standard deviations(RSDs) less than 10%. Finally, the developed method has been successfully used to analyzing the real samples.

Determination of the gas compositions for direct coal liquefaction by gas chromatography

Via multi-dimensional gas chromatography, configured with parallel dual-channel, double detectors, valves switching and back flushing, rapid analysis of the gas compositions consisting of C1-C5 hydrocarbons and permanent gases, such as CO2, H2S, H2, and CO, for direct coal liquefaction has been realized. With four packed chromatographic columns, which are Hayesep-Q pre-column, Hayesep-Q column, molecular sieve 5A column and one PLOT A1203 S capillary column, the gas compositions for direct coal liquefaction are analyzed qualitatively and quantitatively by the external standard method. The determination method has such advantages as excellent separation, simple operation, rapid analysis and accurate results.

Comparative analysis of volatile constituents between herbal pair flos lonicerae-caulis lonicerae and its single herbs

Gas chromatography-mass spectrometry(GC-MS) and the chemometric resolution method(alternative moving window factor analysis,AMWFA) were used for comparative analysis of volatile constituents in herbal pair(HP) flos lonicerae-caulis lonicerae(FL-CL) and its single herbs.The temperature-programmed retention index(PTRI) was also employed for the identification of compounds.In total,44,39,and 50 volatile chemical components in volatile oil of FL,CL and HP FL-CL were separately determined qualitatively and quantitatively,accounting for 87.22%,94.54% and 90.08% total contents of volatile oil of FL,CL and HP FL-CL,respectively.The results show that there are 32 common volatile constituents between HP FL-CL and single herb FL,33 common volatile constituents between HP FL-CL and single herb CL,and 10 new constituents in the volatile oil of HP FL-CL.

Principal Component Analysis （PCA） on Multivariate Data of Lard Analysis in Cooking Oil

Discrimination of fatty acids （FAs） of lard in used cooking oil is important in halal determination. The aim of this study was to find the information related to the changes FAs of lard when frying in cooking oil. Quantitative analysis of FAs composition extracted from a series of experiments which involving frying cooking oil spiked with lard at three different parameters; concentration of spiked lard, heating temperatures and period of frying. The samples were analyzed using Gas Chromatography （GC） and Principal Components Analysis （PCA） technique. Multivariate data from chromatograms of FAs were standardized and computed using Unscrambler X10 into covariance matrix and eigenvectors correspond to Principal Components （PCs）. Results have shown that the first and second PCs contribute to the FAs mapping which can be visualized by scores and loading plots to discriminate FAs of lard in used cooking oil

Carbothermic reduction of alumina with carbon in vacuum

Carbothermic reduction alumina in vacuum was conducted, and the products were analysed by means of XRD and gas chromatography. Thermodynamic analysis shows that in vacuum the initial carbothermic reduction reaction temperature reduces compared with that under normal pressure, and the preferential order of products is Al404C, Al4C3, Al2OC, Al20 and A1. Experiment results show that the carbothermic reduction products of alumina are A1404C and A14C3, and neither A12OC, Al20 or Al was found. During the carbothermic reduction process, the reaction rate of Al203 and carbon decreases gradually with increasing time. Meanwhile, lower system pressure or higher temperature is beneficial to the carbothermic reduction of alumina process. A1404C is firstly formed in the carbothermic reaction, and then A14C3 is formed in lower system pressure or at higher temperature.

Identification of Volatile Compounds in Codfish(Gadus) by a Combination of Two Extraction Methods Coupled with GC-MS Analysis

Codfish is a kind of abyssal fish species with a great value in food industry. However, the flavor of codfish, especially the unpleasant odor, has caused serious problems in its processing. To accurately identify the volatile compounds in codfish, a combination of solid phase micro-extraction(SPME) method and simultaneous distillation extraction(SDE) method was used to extract the volatiles. Gas chromatography-mass spectrometry(GC-MS) along with Kovats indices(KI) and authentic standard compounds were used to identify the volatiles. The results showed that a total of 86 volatile compounds were identified in codfish, of them 24 were extracted by SDE, 69 compounds by SPME, and 10 compounds by both SDE and SPME. Seventy volatile compounds were found to have specific odors, of them 7 typical compounds contributed significantly to the flavor of codfish. Alcohols(i.e.,(E)-2-penten-1-ol and 2-octanol), esters(i.e., ethyl butyrate and methyl geranate), aldehydes(i.e., 2-dodecenal and pentadecanal) contributed the most to fresh flavor while nitrogen compounds, sulphur compounds, furans, as well as some ketones(i.e., 2-hydroxy-3-pentanone) brought unpleasant odor, such as fishy and earthy odor. It was indicated that the combination of multiple extraction methods and GC-MS analysis can enhance the accuracy of identification, and provide a reference for the further study on flavor of aquatic products.

Separation of arenols from a high-temperature coal tar

A high-temperature coal tar collected from Xuzhou Coking Plant, Saint-Gobain Pipelines （Xuzhou） Co., Ltd. was exhaustively extracted with petroleum ether （PE）. The extract was sequentially eluted through silica gel with PE and PE/ethyl acetate （EA） mixed solvents （volume ratio 2：1 ） to afford two eluted frac- tions. The extract and eluted fractions were analyzed with gas chromatography/mass spectrometry. In total, 14 arenols were detected, including phenol, cresols, xylenols, fluorenols, phenanthren-3-ol and pyren-l-ol.

Determination of Water Content of Water-soluble Paints by Gas Chromatography

This paper describes the determination of water content of water-soluble paints by gas chromatography. The water in paints is extracted by dimethyl formamide (DMF) as a solvent.Isopropanol is used as an internal standard. The mixture is separated by low-speed centrifugation.Then a 1-uL sample of the supernatant from the prepared solution is injected into the gas chromatograph. The water content is determined by internal standard calibration curve. The rate of recovery of added standard of this method is more than 98%. Relative mean deviation is less than 3‰.The linearity of calibration curve is good and relativity coefficient is higher than 0.998.

Study on the basic nitrogen compounds from coal-derived oil

The distillation range analysis and elemental analysis of fractioned direct liquefied oil were conducted. Each fraction of liquefied oil contains some nitrogen compounds. Using the acid extraction method and gas chromatography/mass spectrometry （GC-MS）, the basic nitrogen compounds have been separated and identified. Compared with the nitrogen content of the liquefied oil before and after separation, the basic nitrogen compounds account for more than half of all nitrogen compounds. The basic nitrogen compounds in the light liquefied oil are easily separated, and contain more types of basic nitrogen compounds. The results also show that there are many basic nitrogen compounds in liquefied oil, such as pyrrole, aniline, pyridine, quinoline and so on. However, there are fewer other types of basic nitrogen compounds.

Natural Attenuation and Biostimulation of Biodiesel Contaminated Soils from Southern Brazil with Different Particle Sizes

Biodiesel bioremediation in soils may occur by natural attenuation or by engineered techniques, such as biostimulation and bioaugmentation. The present study evaluated the degradation of biodiesel in two soils with different particle size characteristics by the bioremediation processes of natural attenuation and biostimulation. The experiment was carried out ex situ, with the factors temperature, moisture content, and pH being controlled for the experimental period of 110 days. The study aimed at evaluating the biodegradation of a clayey soil （A） and a sandy soil （B）, both contaminated with pure biodiesel, by using the analytical methods of respirometry and gas chromatography. Biostimulation treatments using nitrogen, phosphorus, and potassium solutions （NPK） promoted higher microbiological activity in both soils. At the end of the experiment, it was observed that biostimulation was more efficient when compared to natural attenuation, showing higher biodiesel degradation for both soils A （59.76%） and B （90.41%）.

Assessing the kinetic model of hydro-distillation and chemical composition ofAquilaria malaccensis leaves essential oil

This study aimed to model the kinetic of hydro-distillation of Aquilaria malaccensis leaves oil in order to understand and optimize the extraction process. In addition, this study, for the first time, aimed to identify the chemical compositions of the A. rnalaccensis leave-oil. By assessing both first-order kinetic model and the model of simultaneous washing and diffusion, the result indicated that the model of simultaneous washing and diffusion better describes the hydro-distillation mechanism of the essential oil from A. rnalaccensis leaves. The optimum time, solid to liquid ratio, and the heating power for extracting the highest amount of essential oil were found to be around 3 h, 1：10 （g. ml-1）, and 300 W respectively. Yellow essential oil with a strong smell and a yield of 0.05 v/w was extracted by hydro-distillation Clevenger apparatus. Chemical compounds of the essential oil were analyzed using gas chromatography-mass spectroscopy （GC/MS）, which resulted in identification of 42 compounds that constitute 93% of essential oil. Among the identified components, Pentadecanal （32.082%）, 9-Octadecenal, （Z） （15.894%）, and Tetradecanal （6.927%） were the major compounds. Considering the fact that all the identified major components possess pesticidal properties, A. malaccensis leaves can be regarded as a promising natural source for producing pesticides.

Pyrolysis of Polytrimethylene Terephthalate(PTT) Fiber by Pyrolysis Gas Chromatography-Mass Spectroscopy

Pyrolysis of polytrimethylene terephthalate(PTT) fiber has been investigated by pyrolysis gas chromatography-mass spectroscopy in the temperature range from 400℃ to 750℃ in order to observe the possible effect of the temperature on its composition of pyrolysates.At 400℃,pyrolysis of molecular chain could occur,only 13 pyrolysates could be identified.The trimethylene moieties bound to the macromolecular core by ester bonds are cleaved at around 400℃.At 550℃-750℃,pyrolysis of molecular chain could completely take place,46 pyrolysates could be found.As the temperature increases,the compositions of pyrolysate are distinctly increased.Several compounds,especially benzoic acid,monopropenyl-p-phthalate,2-propenyl benzoate,di-2-propenyl ester,1,4-benzenedicarboxylic acid,benzene,1,5-hexadiene,biphenyl and 1,3-propanediol dibenzoate could be formed.The thermal degradation mechanism,which is determined by structure and amount of the thermal decomposition products,are described.During pyrolysis of polytrimethylene terephthalate,polymeric chain scissions take place a peeling reaction as a successive removal of the dimer units from the polymeric chain.The chain scissions are followed by the elimination reaction,linkage action and secondary reactions,which bring about a variety fragment.

Utilization of Hydrocarbons Obtained by Waste Plastic Pyrolysis： Energetic Utilization （Part Ⅰ）

The pyrolysis of different waste polymers （polyethylene, polypropylene and polystyrene） was investigated in a tube reactor at 550 ℃ in the absence of oxygen. Additionally the energetic utilization of products have also been followed both in refining and petrochemical industry. Pyrolysis products were separated into fractions of gases, naphtha, middle distillates and heavy oil. Raw materials have been collected both from industrial and household sources： polyethylene from agriculture, polyethylene from packaging and polystyrene from packaging and electronic equipments. Yields and properties of volatile products have changed by the raw materials. Products have been analyzed by gas chromatography. Fourier transformed infrared spectroscopy, size exclusion chromatography and other standardized methods. Naphtha had high octane numbers （80 〈 RON）, while high cetane numbers （〉 75） in case of middle distillates. Moreover fractions contained approximately half of unsaturated hydrocarbons, mainly α-olefins, but the percentage was depending on the raw materials. These properties are advantageous for fuel-like applications.