Gamma irradiation influence on wheat flour gelatinisation

Differences were detected by DSC between gelatinisation and amylose-lipid complex transition occurring in suspensions of control and irradiated with 30 kGy wheat flour characterised by a dry matter to water ratio equal to ca. 1:1 and the dependence of the results on the heating rate. Two steps viscosity was discovered using of Brabender viscograph for the wheat flour irradiated with 1-30 kGy dose (apart to an essential decrease in maximum viscosity) while a one step process occurs in the case of the control one. It was compared to one step viscosity jump observed in the case of rye flour, both control and irradiated. The results are discussed in terms of radiation induced changes in starch granules. Storage of the suspensions at -20°C led to an additional exothermic effect, preceding well-recognised gelatinisation effect. This revised version was published online in August 2006 with corrections to the Cover Date.     

Morphology of polytetrafluoroethylene before and after irradiation

Supramolecular structure and morphology of as-polymerized, sintered, and gamma-irradiated suspension PTFE were studied with scanning electron microscopy. Irradiation was performed both below and above melting point of crystal phase. Fibrillar supramolecular structure of as-polymerized PTFE is preserved after its sintering. In contrast to as-polymerized PTFE, in the sintered polymer some segments of fibrils form lamellae of thickness 100-300 nm and length up to several microns, with fibrils arranged perpendicularly to a lamella. Irradiation below the melting point (20 and 200 °C) does not change quantitatively PTFE morphology. In both cases and also in the case of pristine PTFE, dense and loose (porous) regions are present in its morphology. Dense regions are packages of irregular shape and consist of densely packaged fibrils. Loose regions consist of individual ribbons and fibrillar lamellae. Irradiation at 200 °C increases greatly the width of lamellae. PTFE structure rearrranges drastically under irradiation above the melting point. New morphology units, spherulites of size about 50 μm, are formed, the spherulites consisting of radially extending fibrils, and porosity decreases substantially. Formation of spherulites is ascribed to radiation-induced chain scission and decrease in molecular mass and viscosity of polymer.     

高效液相色谱-二极管阵列检测法测定小麦粉及面粉改良剂中福美双

福美双是重要的二硫代氨基甲酸酯(DTC)杀菌剂,在小麦中使用限量以1 mg/kg二硫化碳(CS2)计.目前我国相关检测方法是针对二硫代氨基甲酸酯一类的化合物,二硫代氨基甲酸酯通过与酸反应生成CS2,采用光谱法或色谱法测定CS2,间接实现二硫代氨基甲酸酯测定.该方法无法特异性实现对福美双的检测,因此开展小麦粉中福美双检测...     

Experience with wheat and wheat flour CRMs

The Chemical Section of OHM [1–2] embarked on the preparation of a wheat sample series as CRMs in 1992. The certification process has been carried out according to the recommendations of ISO. Since then a series of wheat flour samples has been developed as well. The investigations of the long-term stability and the application of wheat and flour CRMs are presented. Received: 23 May 1997 / Revised 8 September 1997 / Accepted: 16 September 1997     

Determination of deoxynivalenol in whole wheat flour and wheat bran

A liquid chromatographic (LC) method was developed for determining deoxynivalenol (DON) in whole wheat flour and wheat bran. A 15 g test sample was extracted with acetonitrile-water (84 + 16, v/v) and applied to a Romer MycoSep cleanup column. The eluate was dried and then reconstituted in a 0.1 M phosphate buffer, pH 7.0, and applied to a Vicam DONtest-LC cleanup column. The methanol eluate was chromatographed with a methanol-water (17 + 83, v/v) mobile phase on a C18 column with UV detection at 220 nm. Five replicates at each of 5 fortification levels (0.25, 0.50, 1.0, 2.0, and 4.0 ppm), plus 5 controls, were determined for both whole wheat flour and wheat bran. For flour, the average recoveries were 72.2-91.5% with relative standard deviations (RSDs) of 4.9-18.4%. The intra-assay flour recovery was 82.4% with 9.8% RSD. A 5 replicate sample of naturally incurred wheat had an average of 1.1 ppm DON with 6.7% RSD. For bran, average recoveries of fortified samples were 69.5-99.7% with RSDs of 1.7-18.8%. The intra-assay bran recovery was 81.5% with 8.9% RSD. The limit of detection (about 3x noise) for the method is 0.05 ppm; the correlation coefficient (linearity) was >0.9995. The DON peak was clearly identified and easily integrated in the chromatograms.     

Experience with wheat flour reference material

The Chemical Section of the National Office of Measures, Hungary (OMH) [1] embarked on the preparation of a wheat sample series as a Certified Reference Material [2] (CRM) in 1992. The practical implementation of the wheat sample series has shown that test- ing laboratories are in great need of easy-to-use flour reference samples to objectively and independently qualify wheat. To fill this need, we have developed a three-term flour reference sample series. The certification process was car-ried out according to ISO recommendations. Investigations of the long-term stability [3] and the application of wheat and flour CRMs are continuing. Wheat is one of the most widely grown crops in Hun- gary and it is one of the major determinative factors in the economy. Its uniform and objective qualification is of outstanding importance. There are well-equipped laborato-ries with sufficient experience to assess wheat flour quality, howev- er, proficiency testing has shown that certified samples need to be used to achieve exact and uniform measuring results. Received: 12 November 1999 Accepted: 16 August 2000     

An electron spin resonance study of dry vegetables before and after irradiation

The ESR signals were successfully observed for the first time in dry vegetables (DVs) that are prominently used in oriental cuisines. We analyzed ESR signals of DV before and after irradiation. Before irradiation, the ESR signal of DV consisted of the three components: a singlet at g=2.0030, the sextet signals from Mn(2+) ion, and a singlet from Fe(3+). The first originated from a carbon centered organic free radical. The second is attributable to the sextet signal with hyperfine interactions of Mn(2+) ion centered at g=2.0020. The third is a singlet at g=4.0030 due to Fe(3+). After the gamma-ray irradiation, a new pair of signals, or twin peaks, appeared in the ESR spectrum of DV. The intensity of the organic free radical at g=2.0030 of the irradiated DV increased lineally with radiation doses. Progressive saturation behavior of the DV indicates a unique saturation and the signals obeyed various relaxation processes.     

Shear stress relaxation of wheat flour dough and gluten

Measurements of shear stress relaxation of wheat flour dough and its corresponding gluten in cone-plate geometry are reported. The range of shear strains used is 0.1–1.0. It is found that the relaxation function is separable into a function of strain and a function of time for shear strains up to 0.4 for dough and 1.0 for gluten. The strain function is non-linear for both dough and gluten. Typically the observed half relaxation time is 1.5 seconds for both dough and gluten. The data suggest the existence of two separate flow processes. The observed time-dependence of the relaxation function has been analysed in terms of a theory of flow as a cooperative phenomenon. In this analysis the process which occurs at short times (0.1–10 s), is characterized by a four-fold coordination of flow units. This process is similar in dough and gluten. The second process, occurring at longer times (10–10⁴ s), is different for dough and gluten and the coordination numbers found are two and one, respectively. This second flow process has to our knowledge not been reported previously.     

ESR investigation of sucrose radicals produced by particle irradiation

We investigated sucrose radicals produced by heavy-ion irradiation with various linear energy transfer (LETs) and the possibility for a sucrose electron spin resonance (ESR) dosimeter. The impact of heavy ions on sucrose produced sucrose radicals, which were measured by ESR. The obtained spectral pattern was the same as that for helium (He) ions, carbon (C) ions, neon (Ne) ions, iron (Fe) ions, and gamma-ray irradiation. Identical spectra were measured after 1 year, but the initial intensities decreased by a few percent when the samples were kept in ESR tubes with the caps at ambient temperature. The total spin concentration obtained by heavy-ion irradiation had a linear relation with the absorbed dose, and correlated logarithmically with the LET. Qualitative ESR analyses showed that the production of sucrose radicals depended on both the particle identity and the LET at the same dose. The production of spin concentration by He ions was the most sensitive to LET. Empirical relations between the LET and the spin yield for various particles imply that the LET at a certain dose can be estimated by the spin concentration. Therefore, the present ESR results imply that sucrose can be used to monitor the absorbed dose and the LET of particle irradiation.     

Gamma radiation influence on technological characteristics of wheat flour

This study aimed at determining the influence of gamma radiation on technological characteristics of wheat (Triticum sativum) flour and physical properties of pan breads made with this flour. The bread formulation included wheat flour, water, milk, salt, sugar, yeast and butter. The α-amylase activity of wheat flour irradiated with 1, 3 and 9 kGy in a Gammacell 220 (AECL), one day, five days and one month after irradiation was evaluated. Deformation force, height and weight of breads prepared with the irradiated flour were also determined. The enzymatic activity increased—reduction of falling number time—as radiation dose increased, their values being 397 s (0 kGy), 388 s (1 kGy), 343 s (3 kGy) and 293 s (9 kGy) respectively, remaining almost constant over the period of one month. Pan breads prepared with irradiated wheat flour showed increased weight. Texture analysis showed that bread made of irradiated flour presented an increase in maximum deformation force. The results indicate that wheat flour ionizing radiation processing may confer increased enzymatic activity on bread making and depending on the irradiation dose, an increase in weight, height and deformation force parameters of pan breads made of it.     

Calorimetric and rheological properties of wheat flour suspensions and doughs: Effects of wheat types and milling procedure

Three types of wheat were submitted to two different milling procedures, giving rise to six flours which differed by some physico-chemical characteristics such as particle size, level of damaged starch and protein content. Differential scanning calorimetry was used for monitoring heat-induced structural changes in flour aqueous dispersions 80% water and in doughs 45% water. Differences between the thermal behaviour of the flour dispersions and doughs were explained mainly by differences in protein content. This result was confirmed after partial substitution of flour by gluten. Dynamic mechanical analysis performed at 20°C on the flour doughs indicated, as expected, a linear increase in the elastic modulus with increasing protein content. The results did not bring any evidence that, under these experimental conditions, starch damage might affect gluten hydration.This revised version was published online in November 2005 with corrections to the Cover Date.     

Matrix-isolation infrared spectra of 2-, 3- and 4-pyridinecarboxaldehyde before and after UV irradiation

Three structural isomers of pyridinecarboxaldehydes (2-, 3- and 4-pyridinecarboxaldehyde) have been investigated in detail with matrix-isolation infrared spectroscopy in the 3000–600 cm⁻¹ region, combined with the UV photo-excitation and density-functional theory (DFT) calculations. Two rotamers (anti and syn) for 2- and 3-pyridinecarboxaldehyde (2- and 3-PCA, respectively) and one rotamer for 4-pyridinecarboxaldehyde (4-PCA) were identified upon photo-excitation. Most of the observed bands of each rotamer have been assigned. Both the infrared data and the results of the DFT calculations agree that the syn rotamer is a less stable isomer for 2- and 3-PCA. Formation of an intramolecular CH⋯N hydrogen bond in the anti rotamer of 2-PCA results in a shortening of the aldehyde CH bond length. The CO bond length is shortened in the syn rotamer due to the repulsion between the N and aldehyde O atoms. With 2-PCA, both photoinduced rotational isomerism and photolysis were observed upon UV irradiation.     

小麦粉中甲醛(吊白块)的测定方法研究

对小麦粉中甲醛提取方法、甲醛与2,4-二硝基苯肼的衍生化反应条件以及甲醛衍生物的提取净化方法进行了研究, 建立了一种小麦粉中甲醛(吊白块)的高压液相色谱测定方法.该方法在甲醛浓度为0.026～0.832 μg/mL范围内与其衍生物的色谱峰面积呈显著线性相关, 相关系数r=0.9986. 小麦粉中甲醛不同添加量的平均回收率＞99%;吊白块不同添加量的平均回收率＞94%(以甲醛量计). 重复测定相对标准偏差平均为4.5%, 甲醛的检出限为9.6 μg/L, 相当于小麦粉中甲醛的最小检出量为0.24 mg/kg.     

Development and certification of a reference material for Fusarium mycotoxins in wheat flour

Deoxynivalenol (DON), nivalenol (NIV) and zearalenone (ZEN) are toxic secondary metabolites produced by several species of Fusarium fungi. These mycotoxins are often found together in a large variety of cereal-based foods, which are regulated by maximum content levels of DON and ZEN. To date, suitable certified reference materials (CRM) intended for quality control purposes are lacking for these Fusarium mycotoxins. In order to overcome this lack, the first CRM for the determination of DON, NIV and ZEN in naturally contaminated wheat flour (ERM®-BC600) was developed in the framework of a European Reference Materials (ERM®) project. This article describes and discusses the whole process of ERM®-BC600 development, including material preparation, homogeneity and stability studies, and an interlaboratory comparison study for certification. A total of 21 selected expert laboratories from different European countries with documented expertise in the field of mycotoxin analysis took part in the certification study using various gas and liquid chromatographic methods. The certified values and their corresponding expanded uncertainties (k?=?2) were assigned in full compliance with the requirements of ISO Guide 35 and are as follows: 102?±?11 μg?kg^?1 for DON, 1000?±?130 μg?kg^?1 for NIV and 90?±?8 μg?kg^?1 for ZEN.     

基于真菌毒素污染差异的液相色谱-串联质谱法鉴别板栗粉中掺假小麦粉

建立了分散固相萃取-超快速液相色谱-串联质谱法同时测定板栗粉和小麦粉中43种真菌毒素的方法,对48份板栗粉和80份小麦粉样品的污染状况进行调查,筛选出5种专属于小麦粉的标志性真菌毒素.样品采用84％(v/v)乙腈水溶液提取,提取液采用C18结合增强型脂质去除净化剂(EMR-Lipid)净化,采用响应曲面-中心组合设计优...     

偶合反应化学发光法测定过氧化苯甲酰

基于过氧化苯甲酰可以氧化K4Fe(CN)6生成K3Fe(CN)6,生成的K3Fe(CN)6在碱性溶液氧化鲁米诺可产生强的化学发光的特性,建立了测定过氧化苯甲酰的偶合反应化学发光新方法.该方法测定过氧化苯甲酰的线性范围为1.0×10-8～4.0×10-6 g/mL, 检出限为5×10-9 g/mL,相对标准偏差为3.0% (1.0×10-7 g/mL过氧化苯甲酰溶液,n=11).该方法已用于市售面粉中过氧化苯甲酰的测定.     

Distribution of deoxynivalenol in wheat,wheat flour,bran, and gluten,and variability associated with the test procedure

Analytical data obtained on deoxynivalenol (DON) concentration in naturally contaminated wheat during processing in an industrial mill were statistically analyzed, and the distribution functions of DON concentration in lots of wheat, bran, wheat flour, and gluten were estimated. The analytical method had acceptable precision (HORRAT 0.25-0.32) for each test sample. The total variance combined sampling, sample preparation, and analytical variances were 0.188, 0.033, 0.42, and 0.0014 ppm2 for wheat, 1.93; flour, 0.99; bran, 4.68; and gluten, 0.29, respectively. The distribution function of DON contamination presented an asymmetric tail for high values of concentration in wheat grains and wheat flour; in bran it seemed to be bimodal with 2 separated peaks of different concentrations; in gluten the normal distribution function gave a reasonably good fit to empirical data. The function eta(c) = -In(-Inp), where p (c) is the cumulative distribution function was linear with c in the so-called extreme-value type I distribution and could be fitted by a cubic polynomial in c in the distributions determined for all the products. This variability and distributional information contributes to the design of better sampling plans in order to reduce the total variability and to estimate errors in the evaluation of DON concentration in lots of wheat and wheat products.     

Simultaneous and rapid determination of deoxynivalenol and its acetylate derivatives in wheat flour and rice by ultra high performance liquid chromatography with photo diode array detection

A simple and reliable method of ultra high performance liquid chromatography coupled with photo‐diode array detection has been proposed for the simultaneous determination of deoxynivalenol and its acetylated derivatives in wheat flour and rice, especially focusing on the optimization of sample extraction, cleanup, and chromatographic separation conditions. Sample pretreatment consisted of a first step using a quick, easy, cheap, effective, rugged, and safe based extraction procedure and a subsequent cleanup step based on solid‐phase extraction. The method was extensively validated in wheat flour and rice, obtaining satisfactory analytical performance with good linearity (R² ≥ 0.999), acceptable recoveries (80.0–104.4%), and repeatability (RSDs 1.3–10.7%). The limits of detection (21.7–57.4 μg/kg) and quantitation (72.3–191.4 μg/kg) for deoxynivalenols were lower than those usually permitted by various countries’ legislation in these food matrices. The method was applied to 34 wheat and rice samples. The results were further compared with results of ultra high performance liquid chromatography with electrospray ionization tandem mass spectrometry.