饲料及食品中玉米赤霉烯酮检测方法研究进展

玉米赤霉烯酮是一种由镰刀菌分泌,广泛污染谷物类粮食作物的真菌毒素,具有雌激素干扰和肝脏、免疫、遗传毒性.玉米赤霉烯酮污染不仅极大危害农牧业发展,更引发严重的食品安全问题.因此建立准确、灵敏的玉米赤霉烯酮检测方法对控制谷物及农副产品中毒素含量至关重要.就目前饲料及食品中常用的玉米赤霉烯酮检测方法进行综述,以供参考借鉴.     

Xylan and xylan derivatives – biopolymers with valuable properties, 1. Naturally occurring xylans structures,isolation procedures and properties

The availability of xylan‐type polysaccharides, representing an immense resource of biopolymers for practical application, is summarized. Xylans constitute 25–35% of the dry biomass of woody tissues of dicots and lignified tissues of monocots and occur up to 50% in some tissues of cereal grains. The most potential sources of xylans include many agricultural crops such as straw, sorghum, sugar cane, corn stalks and cobs, hulls and husks from starch production, as well as forest and pulping waste products from hardwoods, in particular. The structural diversity and complexity of xylans is illustrated and shown to depend on the botanic source. Various extraction procedures suitable for the isolation of xylans from different plant sources are described and compared. It is suggested that certain structural types of xylans like glucuronoxylan, arabinoglucuronoxylan, and arabinoxylan can be prepared from certain plant sources with similar chemical and physical properties. In contrast to structural analyses, the physicochemical properties, including solubility, molecular weight and molecular weight distribution, and rheological properties have been studied only for few xylan types. From the functional properties, the thermophysical and tensioactive properties are described. Finally, the physiological activities of xylans, which represent important dietary fibers as well as the immunological activities of some xylan types, are presented.     

Ultramicrodetermination of nitrogen in organic compounds: 8. Weighing of hygroscopic and volatile samples for the sealed-tube method

A new method for handling hygroscopic and volatile samples for decimilligram determination of organic nitrogen by the sealed-tube method was described. It involves the use of a copper-foil capsule in which hygroscopic and volatile samples can be dried to constant weight and weighed. Satisfactory results were obtained with this method.     

Eine Apparatur zur automatischen Bestimmung von Wasserdampf-Sorptions-Isothermen und -Isobaren

An apparatus for the automatic determination of water vapor sorption isotherm and isobares is described. Its main parts are a Cahn electrobalance and a gas circulating system. The gas can be held at constant dew points between – 85 and + 25 degree by an ultracryostal and an ultrathermostate and brings the sorbens to hygroscopic equilibrium.     

Oxidation of oleic acid and oleic acid/sodium chloride(aq) mixture droplets with ozone: changes of hygroscopicity and role of secondary reactions

The heterogeneous reactions of oleic acid (OL) and oleic-acid/sodium-chloride(aq) (OL/NaCl(aq)) mixture droplets with ozone are studied at two relative humidities (RH). The reactions were monitored concomitantly using attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FT-IR) for the organic species and UV-vis spectrometry for the ozone concentration in order to investigate reaction rate discrepancies reported in literature as well as the oxidation mechanism. The less volatile products were identified and resolved by a Fourier transform ion cyclotron resonance mass spectrometer (FT-ICR-MS). This led to identification of 13 organic molecules (up to 45 carbons). Identified products were predominantly composed by nananoic acid and azelaic acid. Our results suggest that the propagation reaction is possibly initiated by a secondary reaction such as the stabilized Criegee intermediates reacting with oleic acid. For hygroscopic properties, the ATR-IR spectra at high RH (87 +/- 5%) showed that the hydrophobic oleic acid droplets can take up water slightly when exposed to ozone. For internally mixed OL/NaCl(aq) droplets, the hygroscopic properties of the droplets upon ozone exposure were found to be complex; hygroscopic properties or the growth factors of the droplets are altered as the oxidation products of oleic acid exist concurrently with NaCl(aq). Furthermore, the concentration of ozone was monitored to examine the kinetics of the oxidation reaction. The integrated ozone profile recorded by UV-vis spectrometry showed the consumed ozone represents only 30 +/- 2% of total oleic acid and hence confirmed the existence of secondary reactions. A kinetic model was used to simulate an ozone temporal profile that could only be described if the secondary reactions were included. The discrepancy of ozone uptake coefficients according to the OL and ozone measurements as well as their atmospheric implications are herein discussed.     

Determination of Riboflavin in Cereal Grains by Capillary Electrophoresis with Laser-Induced Fluorescence Detection with On-Line Concentration

A very simple, sensitive, and reliable method for the routine determination of riboflavin in cereal grains by capillary electrophoresis with laser-induced fluorescence detection (CE-LIF) was established. Two on-line concentration techniques, namely, stacking in reverse migrating micelles (SRMM) and sweeping, were examined to enhance the detection signal. The optimum separation buffer consisted of 20 mM phosphoric acid and 140 mM sodium dodecyl sulfate (SDS), and a hydrodynamic injection of 30 s at 0.5 psi was confirmed for the introduction of a sample. In addition, it was found that salt in sample matrix influenced the performance of SRMM, showing the standard addition method was required for the quantitative analysis. The linearity of the method was good with a range of 0.5–500 ng/mL (r = 0.9990). The limit of detection (LOD) was 0.29 ng/mL at a signal-to-noise ratio of 3. This procedure presented was successfully applied to determine riboflavin in 18 samples of 9 types of cereal grains. The recovery rates varied from 94% to 98%, and the relative standard deviation (RSDs) was less than 4.1%.     

Abundance of 13C and 15N in emmer, spelt and naked barley grown on differently manured soils: towards a method for identifying past manuring practice

The shortage of plant-available nutrients probably constrained prehistoric cereal cropping but there is very little direct evidence relating to the history of ancient manuring. It has been shown that the long-term addition of animal manure elevates the δ(15)N value of soil and of modern crops grown on the soil. We have examined the δ(15)N and δ(13)C values of soil and of the grain and straw fractions of three ancient cereal types grown in unmanured, PK amended and cattle manured plots of the Askov long-term field experiment. Manure increased biomass yields and the δ(15)N values of soil and of grain and straw fractions of the ancient cereal types; differences in δ(15)N between unmanured and PK treatments were insignificant. The offset in straw and grain δ(15)N due to manure averaged 7.9 and 8.8 ‰, respectively, while the soil offset was 1.9 ‰. The soil and biomass δ(13)C values were not affected by nutrient amendments. Grain weights differed among cereal types but increased in the order: unmanured, PK, and animal manure. The grain and straw total-N concentration was generally not affected by manure addition. Our study suggests that long-term application of manure to permanently cultivated sites would have provided a substantial positive effect on cereals grown in early agriculture and will have left a significant N isotopic imprint on soil, grains and straw. We suggest that the use of animal manure can be identified by the (15)N abundance in remains of ancient cereals (e.g. charred grains) from archaeological sites and by growing test plants on freshly exposed palaeosols.     

吸湿发热型黏胶纤维的性能

通过盐酸肼交联羧甲基化黏胶纤维制得具有吸湿发热功能的黏胶纤维,讨论了纤维在吸湿发热量、断裂强度、热性能及微观结构等方面的特性.结果表明:当纤维中氮的质量分数为2%～4%,回潮率为25%～26%(相对湿度90%)时,纤维吸湿发热效果明显,发热量最高可达7.67J/g;交联使纤维的湿断裂强度明显提高,湿干强度比可提高16....     

Identification and characterization of new Fusarium masked mycotoxins,T2 and HT2 glycosyl derivatives,in naturally contaminated wheat and oats by liquid chromatography–high‐resolution mass spectrometry

The presence of glucoside derivatives of T‐2 and HT‐2 toxins (type A trichothecene mycotoxins) in naturally contaminated wheat and oats is reported for the first time. The use of advanced high‐resolution mass spectrometry based on Orbitrap technology allowed to obtain molecular structure details by measuring exact masses of main characteristic fragments, with mass accuracy lower than 2.8 ppm (absolute value). A monoglucoside derivative of T‐2 toxin and two monoglucoside derivatives of HT‐2 toxin were identified and characterized. The analysis of their fragmentation patterns provided evidence for glucosylation at C‐3 position for T‐2 toxin and at C‐3 or C‐4 position for HT‐2 toxin. A screening for the presence of these new masked forms of mycotoxins was carried out on a set of naturally contaminated wheat and oats samples. On the basis of peak area ratio between glucoside derivatives and free T‐2 and HT‐2 toxins, the presence of glucoside derivatives was more likely in wheat than in oats samples. The present work confirms the widespread occurrence of trichothecene glucosides in cereal grains naturally contaminated with the relevant unconjugated toxins, thus suggesting the importance of developing suitable analytical methods for their detection. Besides toxicity studies, tracking down these new masked forms of trichothecenes along the food/feed chain would enable to collect information on their relevance in human/animal exposure to mycotoxin risk. Copyright © 2012 John Wiley & Sons, Ltd.     

Binary Simple Sugar Profiling in Corn and Small Grain Flour Authentication Using GC/EI-qMS Approach

There is an increasing demand for mixed flour bakery products in the world market, considering the health benefits of various cereal grains. The aim of this work was to develop a rapid approach for corn and small grain flour authentication. Simple sugars present in flour samples were extracted with 96 % ethanol solution, derivatized into corresponding trimethylsilyl oximes (TMSO), and analyzed on a GC/EI-qMS device. The presence of a specific simple sugar at a specific retention time was confirmed using mass spectrometer, thus providing a semi-qualitative approach. Binary matrices were developed based on the presence/absence of detected simple sugar compounds in the investigated cereal species, to minimize the influence of variability between investigated cultivars of the same species. By performing exploratory data analysis: hierarchical cluster analysis (HCA), principal coordinate analysis (PCO), and principal component analysis (PCA), flour samples of corn species were strongly separated from every investigated species of small grains, using all three multivariate tools, thus enabling its authentication in a small grain/corn flour mixture.

     

Hydrophobization of coarse calico by wet treatment in aluminum chloride solutions

This paper describes the method of wet chemistry used for hydrophobization of coarse calico surface. It was found that hydrophobicity of coarse calico surface is achieved by the formation of aluminum oxide on the surface. An experimental plan was drawn up according to the Taguchi method. The effect of soap solution temperature, aluminum chloride solution concentration, sample treatment time in aluminum chloride solution and heat treatment temperature on water absorption, contact angle, capillary absorption and calico moisture content was studied. The dependencies of hygroscopic properties on the process parameters were obtained. Capillary absorption and water absorption of the test samples increased with increasing concentration of aluminum chloride solution. An increase in the processing time of coarse calico samples in an aluminum chloride solution leads to a decrease in the hydrophobicity of the samples. The characteristics of the dependencies of hygroscopic properties on the temperature of heat treatment and the temperature of the soap solution are similar.

     

Thermal analysis of transition metal salts of carboxylic acids

The thermal decomposition of salts (both normal and acid) of transition metals with carboxylic acids (maleic, ortho-phthalic and terephthalic) was studied in inert atmosphere. The residues after pyrolysis (up to 450°C) are composites including two structural components: an organic polymer matrix and spherical conglomerates from metal grains coated with polymer. Thermal decomposition of solid solutions of metal bimaleates (Co-Ni, Fe-Ni, Zn-Ni) was investigated. Thermogravimetric data (obtained at different rates of linear heating) were processed with 'Netzsch Thermokinetics' computer program. Kinetic parameters were calculated only for the first decomposition step, and the process is described by Prout-Tompkins equation of n ^th order with autocatalysis. Some properties of the resulting composites have been studied qualitatively. This revised version was published online in July 2006 with corrections to the Cover Date.     

Influence of chemical impurities in ammonium phosphate and ammonium sulfate on the properties of ABCE fire extinguishing dry powders

The influence of chemical impurities on hygroscopic properties, as well as on the grinding and modification efficiency of ammonium phosphate and ammonium sulfate was analyzed. It was shown that application of chemically pure ammonium sulfate and ammonium phosphate free of ammonium fluoride and magnesium phosphate impurities provides the best conditions for obtaining fire extinguishing dry powders with high fire suppression ability and properties that satisfy relevant specifications.     

Encapsulation and weighing of samples for analysis

Encapsulation and handling methods for hygroscopic, volatile, oily and other kinds of difficult samples for analysis are described. Hermetical encapsulation is achieved with an electrical spot welder.     

Injection molded hybrid composites based on corn fibers and poly(vinyl alcohol)

Ongoing research cooperation between USDA and the University of Pisa, Italy has yielded several composite blends of poly(vinyl alcohol) (PVA) and corn fibers (CF). The USA is the largest producer of ethanol from cereal grains. Composites based on natural fibers alone are extremely sensitive to water. Their mechanical properties deteriorated upon the absorption of water, thus suggesting a limited usefulness of such formulations in practical applications. In this study, corn-fibers produced during the wet milling process of corn for fuel ethanol were used to prepare composites. CF and PVA were processed in variable amounts in the presence of both dry/fluid plasticizers, such as glycerol and pentaerythritol. Composites prepared from CF in combination with PVA showed little change in their mechanical properties even after conditioning at variable relative humidities, as well as complete soaking in water. Composites tested after storage for one year under 50% relative humidity and 23°C exhibited mechanical properties similar to those of freshly prepared composites. Cornstarch was introduced in the formulation for the purpose of reducing the cost of the final product and to further increase the composition of natural components in the composites. Addition of starch moderately reduced the mechanical properties of the composites.     

Moisture uptake in nanocellulose: the effects of relative humidity,temperature and degree of crystallinity

Cellulose - Foams made from cellulose nanomaterials are highly porous and possess excellent mechanical and thermal insulation properties. However, the moisture uptake and hygroscopic properties of...     

Determination and survey of ochratoxin A in wheat, barley, and coffee--1997

Ochratoxin A (OA) is a nephrotoxic and nephrocarcinogenic mycotoxin produced by Aspergillus and Penicillium species. It has been found mainly in cereal grains and coffee beans. The purpose of this study was to investigate the occurrence of OA in cereal grains and in coffee imported to the United States. A modified liquid chromatographic (LC) method for determining OA in green coffee was applied to wheat, barley, green coffee, and roasted coffee. The test sample was extracted with methanol-1% NaHCO3 (7 + 3), and the extract was filtered. The filtrate was diluted with phosphate-buffered saline (PBS), filtered, and passed through an immunoaffinity column. After the column was washed with PBS and then with water, OA was eluted with methanol. The eluate was evaporated to dryness, and the residue was dissolved in acetonitrile-water (1 + 1). OA was separated on a reversed-phase C18 LC column with acetonitrile-water-acetic acid (55 + 45 + 1) as eluant and quantitated with a fluorescence detector. Recoveries of OA from the 4 commodities spiked over the range 1-4 ng/g were 71-96%. The limit of detection was about 0.03 ng/g. OA contamination at > 0.03 ng/g was found in 56 of 383 wheat samples, 11 of 103 barley samples, 9 of 19 green coffee samples, and 9 of 13 roasted coffee samples. None of the coffee samples contained OA at > 5 ng/g; only 4 samples of wheat and 1 sample of barley were contaminated above this level.     

Preprocessed barley,rye, and triticale as a feedstock for an integrated fuel ethanol-feedlot plant

Rye, triticale, and barley were evaluated as starch feedstock to replace wheat for ethanol production. Preprocessing of grain by abrasion on a Satake mill reduced fiber and increased starch concentrations in feedstock for fermentations. Higher concentrations of starch in flours from preprocessed cereal grains would increase plant throughput by 8–23% since more starch is processed in the same weight of feedstock. Increased concentrations of starch for fermentation resulted in higher concentrations of ethanol in beer. Energy requirements to produce one L of ethanol from preprocessed grains were reduced, the natural gas by 3.5–11.4%, whereas power consumption was reduced by 5.2–15.6%.     

Determination of Iodine in Cereal Grains and Standard Reference Materials by Neutron Activation Anaylsis

Abstract

Trace amounts of iodine in thirty-eight cereal grain samples cultivated at different locations in Austria were determined for the first time in this study by radiochemical neutron activation analysis. For the dissolution of cereal grain samples and standard reference materials, two different procedures, alkaline and acidic dissolution, were applied in the presence of an iodine carrier. Rapid and simple dissolution procedure with acidic solution was demonstrated in this study. The analytical values in the cereal grain as well as in the standard reference materials obtained by the different dissolution procedures were in good agreement within one standard deviation. The iodine in cereal grains and the standard reference materials ranged from 0.002 to 0.03 μg g^?-1 and 0.0015 to 0.30 μg g^?-1, respectively. The distribution of relative standard deviation (RSD) for iodine concentration below 0.01 μg g^?-1 were 21% and 24% of all data for the range 1–10% RSD and 11–20% RSD, respectively. The RSD for 0.1 μg g^?1 of iodine concentrations were around 10%