色谱分析法在生物科学研究中的应用

色谱分析法是兼具分离和检测能力的分析技术,已成为现代生物科学研究的重要实验手段。本文对近年来色谱分析技术在氨基酸和蛋白质的含量和组成检测方面的应用进行了介绍和总结。     

Analysis of potato sugars by gas chromatography

A procedure for determining sugars in potato tubers by gas chromatography is described and examples given of its application to stored and reconditioned potatoes. Juice from tubers is extracted, boiled, centrifuged, and the trimethylsilyl derivatives of the sugars prepared. Column choice and operating conditions are given. Results are fairly comparable to those from wet analysis, are more comprehensive, and more easily obtained.     

Effects of the nitrile group substitution on the gas separation properties of aromatic polyamide membranes

The effects of nitrile group substitution onto aromatic polyamide backbone on the gas permeability and permselectivity of the polymers are examined. The gas permeability of aromatic polyamides increase with increasing the content of nitrile group substitution, whereas the permselectivity decreases with increasing the nitrile group contents. The effects of chain linrearity on the permeability and permselectivity are also examined. The non-linearity of the polymers increases the permeability. These behaviors are interpreted in terms of chain packing and crystallinity of the aromatic polyamides.     

Studies of higher alcohol formation by yeasts through gas chromatography

Summary The methods of gas chromatography have made possible significant advances in understanding the pathways of formation of higher alcohols during alcoholic fermentation. The higher alcohols in wines of fermented media were quantitatively concentrated by close fractional distillation coupled with drying and extraction with diethyl ether. Gas-liquid chromatography was employed for determining the percentage of the individual alcohol components as well as for separation and collection of specific alcohols by condensation of the effluent gases in order to measure radioactive carbon-14 activities incorporated from C-14 intermediates and for degradation studies. The principal results of recent studies of the pathways of higher alcohol formation indicate that they are formed by reactions closely related to the synthesis of valine, leucine and isoleucine. However, the amounts of higher alcohols formed by the Ehrlich pathway of direct breakdown of endogenous amino acids are often negliglible or non-existent. Evidence was obtained to support the hypothesis that 2-ketobutyric acid is the intermediate from which bothn-propanol andn-butanol are found in fermentations by mutant strains of yeast.

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Zusammenfassung Die Methoden der Gaschromatographie haben bedeutende Fortschritte in der Kenntnis der Bildungweise der höheren Alkohole während der alkoholischen Gärung möglich gemacht. Die höheren Alkohole der Weine oder des Gärungsmilieus wurden zu diesem Zwecke quantitativ konzentriert, durch weitgehende fraktionierte Destillation, verbunden mit Trocknung und Extraktion mit Hilfe von Diäthyläther. Die Gas-Flüssigkeits-Chromatographie wurde zur Bestimmung des Prozentsatzes der an der Zusammensetzung beteiligten individuellen Alkohole benutzt, sowie auch zur Trennung der spezifischen Alkohole durch Kondensation der austretenden Gase, zum Zwecke der Messung der Radioaktivität des Kohlenstoff-14, der von mit Kohlenstoff-14 markierten Zwischen-produkten herrührte und zur Untersuchung des Abbaues. Die hauptsächlichsten Ergebnisse neuerer Untersuchungen über die Bildungsstufen der höheren Alkohole zeigen, daß sie durch Reaktionen gebildet werden, die denen der Synthese von Valin, Leucin und Isoleucin ähnlich sind. Dagegen sind die Mengen höherer Alkohole, die nach der Hypothese von Ehrlich, durch den direkten Abbau der endogenen Aminosäuren entstehen oft sehr gering oder sind nicht vorhanden. Es wurden Beweise zur Bestätigung der Hypothese gefunden, nach der die 2-Ketobuttersäure ein Zwischen-produkt ist, von dem aus sich gleichzeitig dern-Propanol und dern-Butanol gebildet haben im Laufe der Gärung mit von Mutationen stammende Hefekulturen.

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Résumé Les méthodes de la chromatographie en phase gazeuse ont rendu possible des progrès significatifs dans la connaissance du mode de formation d'alcools supérieurs pendant la fermentation alcoolique. Dans ce but les alcools supérieurs des vins ou des milieux fermentés ont été concentrés quantitativement par distillation fractionnée poussée, conjuguée avec une dessiccation et une extraction à l'éther diéthylique. La chromatographie en phase gaz/liquide fut utilisée pour la détermination des pourcentages des alcools individuels, entrant dans la composition, aussi bien que pour la séparation et le fractionnement des alcools spécifiques par la condensation des gaz effluents, afin de mesurer la radioactivité du carbone-14, incorporé à partir d'intermédiaires en C-14, et pour l'étude de la dégradation. Les principaux résultats des études récentes sur les voies de formation des alcools supérieurs, indiquent qu'ils sont formés par des réactions ressemblant beaucoup à celles de la synthèse de la valine, de la leucine, et de l'isoleucine. Cependant, les quantités d'alcools supérieurs formées selon l'hypothèse d'Ehrlich, par décomposition directe des aminoacides endogènes, sont souvent négligeables ou inexistantes. Des preuves furent trouvées pour confirmer l'hypothèse que l'acide 2-cétobutyrique est l'intermédiaire à partir duquel sont formés à la fois len-propanol et len-butanol au cours de la fermentation avec les souches de levures, issues de mutation.

     

非衍生化-气相色谱串级质谱（GC-MS-MS）法测定豆粉中的三聚氰胺

利用离子阱气相色谱质谱联用仪,建立了非衍生化处理-气相色谱串级质谱直接分析三聚氰胺的检测方法.利用三聚氰胺二级质谱进行定性,以二级质谱的特征离子峰m/z=85进行定量,分析效率大大提高.方法的线性范围为0.5～10 mg/L,线性相关系数为0.998 7,最小检测限为0.20 mg/kg,方法的精密度为5.9%,方法的回收率为82%～96%,满足现有三聚氰胺的检测,建立的方法可以直接应用于该类产品中三聚氰胺的检测.     

基于基质固相分散萃取的茶叶中拟除虫菊酯多农残气相色谱测定

建立了一种快速又简便的气相色谱电子捕获检测(GC-μECD)测定茶叶中8种拟除虫菊酯农药残留的方法,采用了新的样品前处理方法—基质固相分散(MSPD)对残留农药进行提取和净化。8种农药的回收率在80.4%～109.2%,相对标准偏差小于10%。实验表明这种方法适用于茶叶样品的拟除虫菊酯农药残留分析。     

基质固相分散—气相色谱法测定植物油中多种拟除虫菊酯类及有机磷类农药残留

通过对基质固相分散吸附剂、淋洗剂、样品填料比等处理条件的优化研究,建立了植物油中22种农药残留分析方法——基质固相分散—气相色谱法,实现对植物油中8种拟除虫菊酯类和14种有机磷类农药残留的同时测定。加标实验结果表明,22种农药回收率均在80.6%～110.3%之间,相对标准偏差均小于4.9%;8种拟除虫菊酯类农药检出限为0.0005 ㎎/㎏～0.015 ㎎/㎏,14种有机磷类农药检出限达到0.01㎎/㎏～0.05㎎/㎏。本方法操作简便,成本低,回收率高,精密度好。     

基质固相分散—气相色谱法测定油菜籽中多种有机磷农药残留

采用基质固相分散法从油菜籽中提取、净化油菜生产中常用的5种有机磷农药，用配有火焰光度检测器的气相色谱定性和定量分析。通过对基质固相分散吸附剂、洗脱剂、净化材料与方式的优化，建立了油菜籽中5种常用有机磷农药残留分析的前处理方法。利用所建立的方法进行3个水平（0.1 mg/kg，0.25 mg/kg，0.5 mg/kg）加标回收实验，结果表明，平均回收率80.3.%-104.4%，相对标准偏差＜10%，方法的回收率和相对标准差满足农药残留检测中准确度和精密度的要求。在此基础上对收集到的150份油菜籽样品进行5种有机磷农药残留检测，检出率为2%。     

An internal standard for rapid analysis of potato sugars by gas chromatography

Summary This paper reports on the use of stearic acid as an internal standard in the analysis of silylated sugars in potatoes by gas chromatography. A Center cooperatively operated by the North Central Region, Agricultural Research Service, United States Department of Agriculture; the Minnesota Agricultural Experiment Station; the North Dakota Agricultural Experiment Station; and the Red River Valley Potato Growers' Association.     

新疆冬、春小麦品种磨粉品质与面粉及新疆拉面品质的关系

为给新疆冬小麦品种新疆拉面加工品质改良提供理论依据,本文选用30个新疆冬麦品种为试验材料,研究新疆冬小麦品种磨粉品质与面粉（团）品质性状、新疆拉面加工品质的关系。结果表明：冬小麦磨粉品质对新疆拉面加工品质具有显著影响作用,其中,出粉率与色泽、适口性、光滑性间呈显著正相关（r=0.396,0.466,0.475）,灰分与适口性、食味呈显著或极显著负相关（r=-0.364,-0.524）,破损淀粉与适口性呈极显著正相关（r=0.485）,a*值与食味呈显著负相关（r=-0.565）,而b*值与食味呈显著正相关（r=0.402）。研究结果还表明,新疆冬小麦品种磨粉品质性状间关系密切,各性状之间相互联系、相互作用;磨粉品质对主要品质性状具有显著影响,其通过影响面粉（团）品质性状进而影响新疆拉面加工品质,如出粉率、灰分、破损淀粉通过对面团吸水率、形成时间、延展性等品质性状的影响对新疆拉面表观、适口性、光滑性等产生间接影响。总之,新疆冬小麦品种磨粉品质与新疆拉面加工品质关系密切,在冬小麦品种新疆拉面加工品质改良中应该重视磨粉品质的改良,要注重提高出粉率、降低灰分和破损淀粉,同时还应改良面粉色泽。对冬小麦优质新疆拉面品种的磨粉品质性状研究后认为优质新疆拉面的磨粉品质指标为：出粉率≥66.04%,灰分(14%MB)≤0.62%,破损淀粉率≤3.69%,面粉颗粒度≤104.28%,L*≥90.78,a*≥-0.81,b*≤8.54。     

Rapid determination of glucose,fructose and sucrose in potato tubers by capillary gas chromatography

Summary A method has been developed for the rapid quantification of glucose, fructose and sucrose in potato tubers by capillary gas chromatography. Baseline separation of trimethylsilyl derivatives of β-D(−) fructose, α-D(+) glucose β-D(+) glucose, myoinositol (internal standard) and sucrose was achieved in under 10 min with a detection range of 10 ng to 3 μg per component. Use of an on-column injector resulted in the retention of a proportion of injected sucrose by the column, despite an oven starting temperature of 140°C. This did not occur with a splitless injection system (inlet temperature 220°C).     

Investigation of surface properties of physico-chemically modified natural fibres using inverse gas chromatography

Inverse gas chromatography (IGC) is a suitable method to determine surface energy of natural fibres when compared to wetting techniques. In the present study, the surface properties of raw and modified lignocellulosic fibres have been investigated by IGC. The fibres chosen for the study were flax, hemp, kenaf, agave, agave hybrid, sisal and pineapple. The treatments used were 4% NaOH and 2% zein. The uniqueness of zein treatment is that it is bio-based and therefore maintains the biodegradable character of the natural fibres. Fourier transform infrared spectroscopy (FTIR) and environmental scanning electron microscope (ESEM) were also performed to characterize the surface changes in fibres. The surface properties of fibres are influenced by the chemical composition, crystallinity and morphology of the fibres. Bast fibres exhibited higher surface dispersive energy than leaf fibres. The raw fibres have a predominant basic character, whereas the alkaline treatment makes the fibres more acidic. Both alkaline and zein treatments decrease the dispersive surface energy and the specific free energy of adsorption.     

Amino acid composition of some Swedish cultivars of Brassica species determined by gas liquid chromatography

The analysis of bulk seed samples of some selected Swedish cultivars showed thatBrassica campestris cultivars contain higher amounts of alanine, valine and aspartic acid than those ofB. napus, whereasB. sinapis cultivars contain higher amounts of glycine and aspartic acid and slightly more threonine and phenylalanine. The amino acid analysis was carried out by gas chromatography.

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Zusammenfassung Die Analyse von Samenproben einiger selektierter Sorten zeigte, dasz Sorten vonBrassica campestris höhere Gehalte an Alanin, Valin, Asparaginsäure besitzen als Sorten vonB. napus. Dagegen verfügen Sorten vonB. sinapis über höhere Gehalte an Glycin und Asparaginsäure und etwas mehr an Threonin und Phenylalanin. Die Aminosäurenbestimmungen erfolgten gaschromatographisch.

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Résumé Lés analyses d'échantillons massifs de graines de certains cultivars selectionnes en Suéde ont montré que les cultivars deBrassica campestris contiennent des taux plus élevés d'alanine, valine, acide aspartique, que ceux deB. napus, tandisque les cultivars deB. sinapis contiennent des taux plus élevés de glycocolle et d'acide aspartique, et un peu plus de thréonine et de phénylalanine. Les analyses d'aminoacides ont été faites par chromatographie en phase gazeuse.

     

Amino acid composition of single seeds and cotyledons of some brassica species by gas liquid chromatography

There are considerable differences in amino acid pattern between the seed coat and the embryo (separated after 5 h of imbibition in water) but only minor differences between the various embryonic parts, the hypocotyl, the inner and outer cotyledons. Thus, the seed coat is high in proline and hydroxyproline and relatively low in glutamic acid. No change in amino acid pattern was observed in the cotyledons after an additional 19 h of imbibition. This is of pratical significanse since a separation of the seed parts — of value in genetic studies — is greatly simplified if performed with swollen seeds as compared with dry seeds.The variation in the amino acid composition among single seeds of heterozygousB. campestris was higher than the variation among single seeds of homozygousB. tournfortii.

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Zusammenfassung Es bestehen bedeutende Unterschiede im Aminosäuremuster der Samenschale und des Embryos (getrennt nach 5 Stunden Inhibition in Wasser) aber nur geringere zwischen den verschiedenen Teilen des Embryos, dem Hypocotyl und den inneren und äusseren Cotyledonen. So sind die Gehalte der Samenschale hoch an Prolin und Hydroxyprolin sowie relativ niedrig an Glutaminsäure. Keine Anderung trat im Aminosäuren-Muster der Cotyledonen ein, wenn sie einer weiteren 19 Stunden-Inhibition unterworfen wurden. Dies ist von praktischer Bedeutung, da eine Trennung der Samenbestandteilewichtig für genetische Studien-im inhibierten Zustand sstärker vereinfacht wird als im normalen trockenen Zustand.Die Variation des Aminosäuren-Spektrums zwischen einzelnen Samen vonBrassica campestris-Heterozygoten war gröszer als die der Heterozygoten vonBrassica tournefortii.

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Résumé Il y a des différences considérables dans la composition en aminoacides entre le tégument séminal et l'embryon (séparé après 5h d'imbibition dans l'eau); par contre il y a peu de différences entre les diverses parties de l'embryon, l'hypocotyle, l'intérieur des cotylectons. Ainsi le tégument séminal est riche en proline et hydroxyproline, et relativement pauvre en acideglutamique. Aucun changement dans les taux d'amincides n'a été observé lors d'une imbibition supplémentaire de 19 heures.Ce fait a une importance pratique, car la séparation de la graine en ses diverses parties — importante dans les recherches génétiques — est grandement simplifiée si elle est pratiquée sur des graines gonflées et non sur des graines sèches. La variation du taux d'aminoacides entre graines isollées deB. campestris hétérozygote était plus grande que chez les graines homozygotes deB. tournefortii.

     

微波炉萃取鲜、粗、细茶叶中的农残及气相色谱检测

本文主要介绍用普通家用的变频微波炉萃取鲜茶叶、粗茶叶、细茶叶中的各种有机氯农药残留，采用氟罗里硅土柱层析净化方法，以AN-5毛细管柱、GC—ECD的气相色谱法进行检测分析。此种方法萃取效果快而好，溶剂使用量少、操作简便快速，一个样品在2—2．5h内就可完成，可满足茶叶中多种农药残留检测的需要。其中对“鲜茶叶的农残检测”进行初步实验。是“茶叶的农残从源头控制。快速检测鲜茶叶农残”的难题的一个尝试。     

施氮对宁杂1号油菜各枝序角果性状的调控

通过不同施N量处理,研究了N素营养对油菜各枝序角果质量的影响,结果表明：(1)油菜各枝序的角果数以主序和中上部分枝较多,并随施N量的增加而明显增加,过多地施用N肥会造成结角层角果过多而严重影响其它产量因素。(2)每角粒数以主序和中上部分枝较多,下部分枝较少。各枝序的千粒重和单位角果皮面积生产力(PPA)以主序最高,上部分枝较高,下部分枝较低。(3)适量施N可使上部8个分枝的每角粒数、千粒重和PPA都维持较高的水平。     

Effects of wheat bran with different colors on the qualities of dry noodles

White, blue, black and purple red wheat bran powders were prepared by ultrafine grinding to the particle size distribution of 0.5–100 μm. The effects of wheat bran addition on the qualities of dry Chinese noodles were investigated. Rapid Visco Analyzer results suggested that peak viscosity, hot paste viscosity, cool paste viscosity, breakdown viscosity and setback viscosity of the blends decreased with the increasing bran levels from 2.0% to 6.0% (P < 0.05). Color of dough sheet (L*) decreased with the addition of wheat bran, while a* and b* values increased distinctly. Water absorption and firmness of the cooked noodles showed up trends with increasing addition of bran, while cooking loss showed a downtrend. Tensile strength and elongation rate decreased when bran addition was 2.0%, but increased when bran addition reached 4.0%–6.0%. Storage modulus (E′) and loss modulus (E″) showed decreasing trends with increases in bran addition at frequencies of 0.1–10 Hz. SEM revealed that bran presence could slightly decrease surface connectivity between starch granules and gluten. It is possible to produce fiber-rich noodles by using 2.0%–6.0% ultrafine-ground bran in wheat flour.     

Florisil固相萃取法联用气相色谱测定油脂中sn-2位脂肪酸

为探寻与气相色谱分析相配套的高效前处理方法,以测定不同物种来源的油脂中sn-2位(β位)脂肪酸组成及含量,考察了Florisil固相萃取柱对经sn-1,3专一性脂肪酶水解后的油脂各产物的分离富集能力,并对萃取条件进行了优化。结果表明,Florisil固相萃取柱能有效地将sn-2单甘脂从油脂水解产物中分离;同时发现Florisil固相萃取可以实现油脂水解产物中甘油三酯、甘油二酯、单甘脂及游离脂肪酸的依次分离。5种不同来源的油脂(植物油、藻油、微生物油脂、鱼油和海豹油脂),水解后经Florisil固相萃取柱萃取,联用气相色谱测定sn-2位脂肪酸组成及含量,结果表明,植物油、藻油和海豹油中sn-2位主要为中长链不饱和脂肪酸(植物油sn-2位中C18∶1,C18∶2和C18∶3约占95%;藻油sn-2位中C16∶1,C18∶1和C18∶2约占50%;海豹油sn-2位中C16∶1,C18∶1和C18∶2约占67%),菌油和鱼油中sn-2位多为长链多不饱和脂肪酸(菌油sn-2位中C20∶4约占37%;鱼油sn-2位中C20∶5,C22∶5和C22∶6约占40%)。     

Improved model for studying hydrological process in the field-to-field irrigation system

Paddy and Water Environment - One of the common irrigation systems in the paddy fields is field-to-field irrigation. The management of these irrigation systems is difficult and essential because of...     

The use of frequency estimates in studying sward structure

Estimates of the frequency of absence of rooted perennial ryegrass tiller bases from concentric sampling quadrats of different sizes are recommended for characterizing the open space structure of perennial ryegrass swards. It is proposed that these estimates are useful for evaluating the persistence of grass species and cultivars in swards. Data on this aspect of sward structure could provide criteria for the productivity of a sward and thus for the need to reseed grassland.