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1.
毛细管色谱直接进样法测定白酒中高碳脂肪酸乙酯的研究   总被引:2,自引:0,他引:2  
介绍了采用FFAP键合毛细管柱直接进样测定白酒中5种高碳脂肪酸乙酯的方法,操作简捷,定量准确,检测限低达04mg/L。用该法测定了各种香型近90个白酒样品。改变色谱条件后,在一次直接进样分析中除能测定高碳脂肪酸乙酯外,而且还能对白酒中醇、酯、醛、酮以及有机酸等52种香味组分进行定量测定,结果重现性良好。  相似文献   

2.
快速气相色谱法分析白酒中的香味组分   总被引:7,自引:0,他引:7  
张超  胡可萍  端裕树  曹磊  武杰 《色谱》2007,25(4):586-589
中国的传统白酒里含有多种香味组分,包括醇类、醛类、酸类和酯类,它们的比率决定着白酒的香型和品质。这些组分可以使用气相色谱仪进行很好的分析并定性和定量。为了缩短分析时间,建立了一种快速检测白酒中香味组分的气相色谱法。采用该方法,用20 m×0.1 mm×0.1 μm的熔融石英毛细管柱在12 min之内完成了对白酒中香味组分的分析,分析时间只是传统色谱方法的三分之一。该方法的重现性良好。  相似文献   

3.
专用型国产气相仪及DNP填充柱测定白酒中的主要香味组分   总被引:4,自引:0,他引:4  
张晓磊  胡国栋 《色谱》2002,20(5):471-473
 采用微机控制的国产气相仪和自制的DNP填充柱测定了白酒中的主要香味组分。通过对各种操作参数的优化 ,确立了等温及程序升温时合适的条件。该方法除可测定十余种主要醇、酯、醛组分外 ,还将分析对象扩大至丙酮、异戊醛、2 戊酮、2 戊醇、3 羟基 2 丁酮等组分 ,从而使采用这一技术可准确测定的组分增至 1 8种。在选定的条件下 ,仪器具有良好的稳定性 ,各香味组分定量结果的重复性好。并对科技部组织研制的这一专用气相仪的适用性作了研讨。  相似文献   

4.
卷烟烟气中挥发性组分的毛细管气相色谱分析   总被引:11,自引:1,他引:10  
采用毛细管气相色谱(CGC)和色谱-质谱联用(GC-MS)技术对国内外部分名牌卷烟烟气中的挥发性和半挥发性化学成分进行了定性定量分析,质谱鉴定出107种化合物;对其中重要的32种化合物进行了定量比较,结果发现烤烟型卷烟、混合型卷烟和英式烤烟在烟气的香味组分中存在一些差异和规律,烤烟型烟气组分总含量最高,烤烟烟气中碳氢化合物裂解产物和低级酸类组分含量较高,混合型卷烟烟气中茄酮和异戊酸较高,英式烤烟的烟气组分更接近于混合型卷烟。  相似文献   

5.
毛细管多维气相色谱法分析炼厂气   总被引:12,自引:0,他引:12  
刘嘉敏  赵盛伟  于世建  王福江  田忠 《分析化学》2000,28(10):1263-1266
用HP6890气相色谱仪,使用多孔层空心毛细管柱(PLOT),选用HP-PLOT/Porapack Q色谱柱测定CO2;HP-PLOT 5A分子筛柱测定O2,N2,CH4;HP-PLOT/Al2O3柱测定有机烃类。采用3阀4柱色谱运行系统,用FID及TCD分别检测烃类及无机气体组分。用色谱工作站控制气动切换阀切换气样走向及两种检测器数据的转换校正和归一化定量计算,用已知物对照法定性,测定了炼厂气中  相似文献   

6.
邻硝基氯苯异构体成分的GC/MS分析   总被引:1,自引:0,他引:1  
本文采用GC/MS分析邻硝基氯苯异构体成分,对样品前处理、溶剂及色谱条件、质谱条件、组分定量作了探讨,分析结果满意。该法无需标样,具有准确、简便、快速的特点。  相似文献   

7.
利用气相色谱/质谱(GC/MS)确定三氯新经多相催化加氢后所得的氯代邻羟基二苯醚类化合物的分子组成和结构;以正二十烷为内标物利用气相色谱/原子发射光谱(GC/AED)碳元素(496nm)检测通道,直接得到氯代邻羟基二苯醚类化合物中碳元素的质量,再根据分子式对组分定量。同时选择氯(479nm)和氧(171nm)通道,以三氯新为内标物定量组分中的氯和氧元素的质量。不同检测通道和不同内标物对同一组分所得定量结果基本一致。因而,对难以全部获得标准样品的复杂体系(如含有多种杂原子、同分异构体以及化学反应过程产物),GC/MS和GC/AED联用能够得到准确、可靠的定性和定量结果。  相似文献   

8.
建立了气相色谱–红外光谱联用法测定白酒中乙醛、戊醛、异戊醛3种醛类挥发性香料成分的方法。白酒样品直接进样分析,在10~10000 mg/L范围内,3种醛类的色谱峰面积与质量浓度线性相关,相关系数大于0.998,方法的检出限为10 mg/L,加标回收率大于90%。利用各个组分的特征红外谱图,提高了分析定性和定量的准确性,特别是提高了对同分异构体的区分能力。  相似文献   

9.
采用石墨化炭黑(GCB)预涂覆技术对白酒分析专用色谱柱(LZP-930)的制备方法进行了优化,详细考察了所制备的色谱柱(LZP-930G)的性能参数,并对LZP-930G色谱柱的保留行为进行了评价,探讨了GCB对LZP-930G色谱柱性能的影响。研究发现,LZP-930G色谱柱的柱效、惰性、稳定性和极性均得到了明显提高,从而改善了酸类和醇类组分的分离选择性和色谱峰峰形,实现了白酒中53种易挥发和半挥发性微量组分的同时分离,且各组分的保留时间和峰面积的相对标准偏差分别小于0.63%和4.51%(n=5)。表明GCB预涂覆技术能够用于高性能白酒分析色谱柱的制备方法。  相似文献   

10.
名优白酒质量指纹专家鉴别系统   总被引:16,自引:0,他引:16  
利用气相色谱法分析了中国名白酒(茅台、泸州老窖、五粮液、汾酒、董酒等)中的34种主要挥发性香味化学物质,根据这些香味化学物质之间的量比关系提出了中国名白酒的“质量指纹”是决定名白酒香型及质量特征的观点。建立了一套完整的名白酒质量指纹库。一次色谱分析可定量检测白酒中多种酯、醇、醛、酸并确定出它们之间的量比关系,通过计算机专家鉴别系统的自动分析,不仅能鉴别白酒的真伪,还能确定白酒的优劣。  相似文献   

11.
A new capillary electrochromatography (CEC) column for the simultaneous analysis of cationic, neutral, and anionic compounds using CEC-ESI-MS is described. Three different silica monolith columns were prepared by changing the poly(ethylene glycol) (PEG) contents for comparison of the separation property of these columns. Different separation programs were used for the simultaneous separation of different charged compounds under the same conditions. The column prepared with 80 mg of PEG separated typical compounds within 15 min using 1 M formic acid as the electrolyte. The analytes migrated in the order of cationic, neutral, and anionic compounds, which means that the migration order was mainly determined by the electrophoresis. The hydrodynamic flow by pressure from the inlet side was significant for a stable analysis to be achieved. The effect of the composition of the sheath liquid was also examined. All analytes (14 amino acids, thiourea, urea, citric acid, and ATP) were detectable when 1% acetic acid in 50% (v/v) methanol was used as the sheath liquid.  相似文献   

12.
《Analytical letters》2012,45(16):2721-2731
In the present work a novel strategy for improving and/or tuning the selectivity of gas chromatographic (GC) separation by combining three different stationary phases (SPs) without premixing was introduced. A fused silica fiber coated with polydimethylsiloxane (SE30) and another coated with cyanopropylphenylmethylpolysiloxane (OV1701) were serially inserted into an 8-m polyethylene glycol 20 M (PEG20M) capillary column to form a GC annular column with ternary SP, abbreviating as SE30-OV1701-CF/PEG20M-CC. The separation capability of this ternary SP annular column was compared with a SE30-coated fiber-in-PEG20M-coated capillary annular column and a PEG20M-coated open tubular column by a test mixture of 19 organic compounds. Among these three columns, SE30-OV1701-CF/PEG20M-CC produced the best separation when the SE30-coated fiber and OV1701-coated fiber was 3 and 5 m, respectively. Selectivity can be easily tuned by changing the length of the SP-coated fibers in the ternary SP annular column. The proposed ternary SP annular column shows additional tunability, thus making it a promising tool for separation of organic solvents that are often used in the manufacturing process of pharmaceutical formulations and lacquer thinners.  相似文献   

13.
The successful separation of 2- and 3-methyl-substituted positional isomers of butanol, butyl acetate, and butanoic acid and its ethyl ester, is reported. These compounds are of interest in the study of wine flavour, however the separation of the 2- and 3-methyl isomers may present problems, and more so in the presence of the wine matrix components, when single capillary column gas chromatography (GC) is used. The strategy to achieve separation was based on the use of shape-selective cyclodextrin derivative (CDD) capillary columns (commonly referred to as chiral columns). These columns provide simultaneous resolution of the enantiomeric pairs of the 2-methyl isomers, and at the same time the ability to separate the 3-methyl isomer from the 2-methyl is achieved in all but the case of the ( S)-2- and 3-methylbutanol. The advantages of using shape-selective columns to perform this study is demonstrated, with coupling of two CDD columns giving improved separations of these compounds. Although these compounds are relatively volatile, cryogenic modulated comprehensive two-dimensional GC was shown to provide good pulsed peak profiles with chiral separation in the first dimension when a thicker film trapping column segment was employed. The components of interest were well separated from other wine matrix components.  相似文献   

14.
测定了61个不同类型化合物在6根PEG20M石英毛细管柱上的保留指数(RI),结果表明各柱间RI存在相当大的差异,给RI数据库的应用带来了困难,结合文献数据,从固定液本身、相界面吸附、热力学函数及柱极性的表征等方面探讨其原因,认为以烷烃为主的相界面吸附是影响RI可比性的重要因素,同时柱制备过程带来的影响也不容忽视。  相似文献   

15.
Complex organic mixtures, such as coal liquefaction and oil shale products and by-products, are comprised of hundreds or thousands of individual components. State-of-the-art high resolution gas chromatography does not always provide sufficient resolution to allow accurate quantitation or identification of many compounds of interest. The concept of dual capillary column chromatography combines the different resolving characteristics of two capillary columns coated with different stationary phases into a single chromatographic run. In this approach, both columns are connected to the same injection port. Analysis of complex mixtures in this fashion can confirm the identification and quantitation of components on two columns of different polarity with little increased analysis time, can provide a means of obtaining quantitative data for individual components which are known to coelute on any one column, and can alert one to unknown coelution problems that would be undetected by gas chromatographic analysis on a single capillary column. Simultaneous dual column analysis was applied to three samples, the neutral polycyclic aromatic hydrocarbon (PAH) fraction of a Solvent Refined Coal-II (SRC-II) heavy distillate, the nitrogen-containing polycyclic aromatic compound (N-PAC) fraction of an SRC-II heavy distillate, and the basic fraction from a shale oil process water. Fused silica capillary columns coated with SE-54 and Durawax 3 were used for the analyses of the heavy distillate, while SE-54 an Carbowax 20M capillary columns were used for the analysis of the process water.  相似文献   

16.
Summary The gas chromatography of all chlorinated methyl acetates, methyl propanoates and methyl mono- and dichlorobutanoates has been studied on Carbowax 20M and SE-30 glass capillary columns under various running conditions. The order of elution on a non-polar column was largely determined by the boiling point of esters, whereas on a polar column it was much influenced by the structure of compounds. Complete separation of the combined mixture of all 27 compounds could not be achieved, however, methyl 3,3-dichlorobutanoate was the only ester overlapped on both columns in spite of the various column temperatures used. The best separation of the mixture was on Carbowax 20M with a temperature program from 50°C at 8°C/min, isothermal running conditions leading either to poor separation of volatile components or long analysis time and broad peaks of higher chlorinated esters. The relative retention times for compounds at the various column temperatures are given and the retention order on a polar and on a non-polar column discussed.  相似文献   

17.
Official methods for the determination of 2-furaldehyde in spirits involve for a spectrophotometric evaluation, which is characterized by poor specificity. Gas chromatographic evaluations have also been proposed, which offer a much higher sensitivity, particularly when capillary columns are used. In this paper a high-performance liquid chromatographic (HPLC) method based on the formation of the 2,4-dinitrophenylhydrazones of carbonyl compounds and subsequent reversed-phase separation of these derivatives is described. Derivatization is carried out by utilizing an acidic solution of 2,4-dinitrophenylhydrazine in acetonitrile. Precipitation of the derivatives is avoided, and direct injection of the sample into the HPLC system is allowed. The determination ofrers a high specificity and a detection limit of the order of 10−8 mol/1. Accuracy and reproducibility data are presented.  相似文献   

18.
快速毛细管气相色谱分析白酒中的香味成分   总被引:1,自引:0,他引:1  
本文建立了快速毛细管气相色谱法,在10 min内分离了白酒中的香味成分,并对其中的醇、醛、酸、酯进行定性分析,对主要呈味成分己酸乙酯进行定量分析,方法重复性好,回收率较高。与常规毛细管色谱法相比,快速毛细管气相色谱法有效地缩短了分析时间,提高了白酒的分析效率。  相似文献   

19.
田怀香  王璋  许时婴 《色谱》2006,24(2):177-180
采用顶空固相微萃取法(HS-SPME)制备样品,利用气相色谱-质谱法(GC-MS)分离鉴定了金华火腿的挥发性风味物质。实验中筛选了固相微萃取纤维头,优化了固相微萃取的操作条件。用75 μm碳分子筛/聚二甲基硅氧烷(CAR-PDMS)纤维头,于60 ℃下对金华火腿样品顶空吸附40 min,于250 ℃下解吸2 min,采用GC-MS对解吸物进行分离鉴定。金华火腿样品的分析结果表明,其挥发性风味物质中含量较高的是醛、酸和酮类化合物,还有一些含硫或杂环化合物。  相似文献   

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