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1.
Fat acidity values were determined on 8 commercially available flours by the American Association of Cereal Chemists method (AACC-02-01A) and by the International Organization for Standardization method (ISO-7305). Comparisons of means obtained by these 2 methods indicated that the ISO method produced results that were 1.4-2.5 times greater (P less than 0.001) than those for the AACC method. These data are consistent with a previous report which indicated that acidic materials (phosphates and amino acids) other than fatty acids are extracted by 95% alcohol (ISO method), whereas fatty acids alone are extracted by petroleum ether (AACC method). Fat acidity values obtained by AACC methodology employing Soxhlet and continuous extraction were also compared. No difference in fat acidity means existed with respect to extraction technique except for an aged whole wheat flour sample which produced a higher value (P = 0.05) by continuous extraction.  相似文献   

2.
土壤样品中痕量丁草胺的分析方法   总被引:2,自引:0,他引:2  
本研究完善了土壤中除草剂丁草胺残留的分析测试方法。在实验室条件下,利用超声提取、弗罗里硅土柱(湿法填柱和干法填柱)进行净化和分离、毛细管气相色谱分析测试,进一步优化了弗罗里硅土柱净化分离丁草胺的条件。土壤中丁草胺的平均回收率为97.46%,检出限为0.002mgkg-1,变异系数小于10%。本方法灵敏度高、重复性好、可排除有机污染物对微量丁草胺残留物测定的干扰,同时减少了有机试剂的用量,适用于土壤样品中痕量丁草胺的分析测试。  相似文献   

3.
The recently developed Eastern Regional Research Center ( ERRC ) dry column chromatographic procedure for determining N-nitrosopyrrolidine (NPYR) in fried cure-pumped bacon was evaluated for its applicability to fried dry-cured bacon. The method was then compared with 2 established procedures for volatile nitrosamine analysis in cured meat products: the multidetection thermal energy analyzer (MD) method and the mineral oil distillation (MOD) screening procedure. No significant difference (P less than 0.05) in NPYR values was found between the ERRC and MD procedures, but significant differences were found between the ERRC and MOD procedures and between the MOD and MD procedures. No artifactual nitrosamine formation was found in the ERRC procedure, but significant amounts were found in samples analyzed by the MOD procedure. The ERRC method was demonstrated to be rugged and very rapid. It is proposed that the ERRC method replace the MOD method as the official screening procedure for NPYR in fried bacon.  相似文献   

4.
The dry weight accumulation per male and female flower as well as the concentration per gram of dry weight and the accumulation of nitrogen (N), phosphorus (P), potassium (K), calcium (Ca), magnesium (Mg), iron (Fe), manganese (Mn), zinc (Zn), and copper (Cu) were determined in walnut tree (Juglans regia L.) catkins and female flowers at the stage of flower bud and during the flower development. Catkin emergence was accompanied by a very fast hydration of the tissues. After the catkin matured, the fresh and dry weights were reduced. The female flower development period was accompanied by the dry and fresh weight increase. Total N, P, K, Fe, Mn, Cu and Zn concentrations in catkin buds were detected at lower levels, Mg in equal levels, and Ca at higher levels as compared to the nutrient concentrations in young growing leaves. The estimated values of the ratio NCmfb/NCygl were: total N = 0.54, P = 0.83, K = 0.56, Ca = 1.5, Mg = 1.0, Fe = 0.46, Mn = 0.71, Cu = 0.85, and Zn = 0.60. Nutrient concentration in female flower buds was detected in almost equal levels with the exception of total N and Fe. The estimated values of the ratio: NCffb/NCygl were: total N = 0.57, P = 1.1, K = 1.17, Ca = 1.06, Mg = 0.9, Fe = 0.47, Mn = 1.0, Cu = 0.92, and Zn = 0.85. Total N, P, Mn, Cu, and Zn accumulations in the catkin were increased during the fast growing phase and decreased after catkin maturing. Potassium, Mg, and Fe accumulation continued to increase in the mature catkin. Calcium accumulation decreased at a very late mature catkin phase. Total N, P, and K accumulation rates during the catkin fast growing phase were higher than the dry weight accumulation rate. Calcium, Mg, Fe, Mn, Cu, and Zn accumulation rates at the same period were lower or equal to dry weight accumulation rates. In mature catkins, the total N, P, Mn, Cu, and Zn depletion rates were higher than the dry weight depletion rate. The continual increase of K, Ca, Mg, and Fe accumulation in mature catkin resulted in the increase of nutrients concentration also. Total N and P showed the highest remobilization values from mature catkin of 51.4% and 45%, respectively. Calcium, K, Mg, Cu, Mn, and Zn remobilization values estimated to be 22.1%, 7.5%, 3.2%, 45.3%, 33.4%, and 31.8%, respectively. Iron showed no remobilization at all. Nutrients remobilization from catkins as compared to the leaves had almost similar values for total N, Zn, and Cu, higher for P, Ca, and Mn, and lower for Mg, Fe, and K. Accumulation of all nutrients in female flowers increased after fertilization. The dry weight accumulation rate was higher than the nutrient accumulation rates.  相似文献   

5.
The validity of 2 electrothermal atomic absorption spectrometric methods for determination of selenium in foods and diets was tested. By using 0.5% Ni(II) as a matrix modifier to prevent selenium losses during the ashing step, it was shown that selenium can be determined in samples containing greater than or equal to 1 microgram Se/g dry wt without organic extraction. The mean recovery tested, using NBS Bovine Liver, was 98%; recovery of added inorganic selenium in Bovine Liver matrix was 100%. In addition, this method gave values closest to the median value of all participating laboratories using hydride generation AAS or the spectrofluorometric method in a collaborative study on high selenium wheat, flour, and toast samples. For samples with concentrations less than 1 microgram Se/g dry wt, separation of selenium from interfering Fe and P ions by organic extraction was necessary. Using inorganic 75Se in meat and human milk matrixes, an ammonium pyrrolidine dithiocarbamate-methyl isobutyl ketone-extraction system with added Cu(II) as a matrix modifier yielded the best extraction recoveries, 97 and 98%, respectively. Accuracy and precision of the method were tested using several official and unofficial biological standard materials. The mean accuracy was within 4% of the certified or best values of the standard materials and the day-to-day variation was 9%. The Se/Fe or Se/P interference limits proved to be low enough not to affect selenium determinations in practically all foods or diets. The practical detection limit of the method was 3 ng Se/g dry wt for 1.0 g dry wt samples.(ABSTRACT TRUNCATED AT 250 WORDS)  相似文献   

6.
An ETAAS method was validated to quantify total Cr and Cr(VI) in mushrooms and the underlying soils. The method includes a sample pretreatment for total Cr dissolution using a wet acid digestion procedure and a selective alkaline extraction for Cr(VI). The limits of detection were, expressed in microg/L, 0.15 and 0.17 for total Cr and Cr(VI), respectively. The linearity ranges under the optimized conditions were 0.15-25.0 and 0.17-20.0 microg/L for total Cr and Cr(VI), respectively. The limits of quantification were, expressed in microg/g of dry weight, 0.0163 and 0.0085 for total and hexavalent chromium, respectively. The precision of the instrumental method for total Cr and Cr(VI) was lower than 1.6%, and for the analytical method, it was lower than 10%. The accuracy of the method for Cr(VI) quantification was evaluated by the standard additions method, with the recoveries being higher than 90% for all of the added concentrations. For total Cr, certified reference materials (lichen CRM 482 and soil sample NCS ZC73001) were used. An interference study was also carried out in a mushroom simulated matrix, and it was verified that the deviations of the expected values were lower than 4.0% for both total Cr and Cr(VI). The validated method was applied to the evaluation of total Cr and Cr(VI) in 34 wild mushrooms and 34 respective underlying soil samples collected in two different regions of Portugal (Beira Interior and TrAs-os-Montes), with different locations regarded as noncontaminated or contaminated areas. The species were identified by a mycologist and subdivided into 10 genera and 15 species: Amanita (rubescens, muscaria, and ponderosa), Boletus (regius), Lactarius (deliciosus, vellereus, and piperatus), Suillus (granulatus and luteus), Tricholoma (acerbum), Agaricus (sylvicola), Volvariella (gloiocephala), Lecopaxillus (giganteus), Macrolepiota (procera), and Psilocybe (fascicularis). The mean values found for total Cr were 1.14 and 1.11 microg/g of dry weight, and for Cr(VI), the mean values were 0.103 and 0.143 microg/g of dry weight for cap and stalk, respectively. For soils, the mean concentrations found were, for total Cr, 84.0 microg/g and, for Cr(VI), 0.483 microg/g. The bioconcentration factors (BCFs) based on dry weight for cap and stalk were determined, and the values found, for both total Cr and Cr(VI), were always <1, although for hexavalent chromium, the BCFs were 10 times higher than for total chromium.  相似文献   

7.
A simplified liquid chromatographic (LC) method for determining vitamin D in vitamin AD concentrates (greater than or equal to 5000 IU vitamin D/g) was collaboratively studied. In the simplified method, the 2 columns specified in AOAC LC method 43.101-43.109 are replaced by a single column, which separates the vitamin D isomers and the vitamin A esters. The procedure for oils includes dissolution and quantitation by normal phase LC. Dry multivitamin concentrates and aqueous dispersions are treated with an enzyme system and the vitamins are extracted with n-pentane. Six coded samples were distributed to 16 laboratories; 15 collaborators returned their results. Estimates of repeatability and reproducibility for the oil samples were 1.1 and 3.1%, respectively; for the high-level concentrated dry preparation 1.4 and 3.9% and for the low-level concentrated dry preparation 1.3 and 11.4%, respectively. These values are a considerable improvement over the results obtained in the 1979 multivitamin collaborative study. The method has been adopted official first action for determination of vitamin D in vitamin AD concentrates containing greater than or equal to 5000 IU vitamin D/g.  相似文献   

8.
A process was developed to separate fiber from distillers dried grains with solubles (DDGS) in a dry‐grind corn process. Separation of fiber from DDGS would provide two valuable coproducts: 1) DDGS with reduced fiber, increased fat, and increased protein contents; and 2) fiber. The process, called elusieve process, used two separation methods, sieving and elutriation, to separate the fiber. Material carried by air to the top of the elutriation column was called the lighter fraction and material that settled to the bottom of the column was called the heavier fraction. We evaluated the compositions of fractions produced from sieving and elutriation. Two commercial samples of DDGS were obtained from two dry‐grind corn plants. Sieving over four screens (869, 582, 447, and 234 μm openings) created five size categories. The two smallest size categories contained >40% (w/w) of the original DDGS and had reduced fiber and increased protein and fat contents relative to the original DDGS. Elutriation of the remaining three size categories increased protein and fat contents and reduced fiber contents in the heavier fractions. Elutriation at air velocities of 1.59–5.24 m/sec increased the protein content of the heavier fraction by 13–41% and increased the fat content of the heavier fraction by 4–127% compared with the bulk fractions of each size category. This process was effective in separating fiber from both DDGS samples evaluated. Elusieve process does not require changes in the existing dry‐grind process and can be implemented at the end of the dry‐grind process.  相似文献   

9.
In the dry‐grind process, starch in ground corn (flour) is converted to ethanol, and the remaining corn components (protein, fat, fiber, and ash) form a coproduct called distillers dried grains with solubles (DDGS). Fiber separation from corn flour would produce fiber as an additional coproduct that could be used as combustion fuel, cattle feed, and as feedstock for producing valuable products such as “cellulosic” ethanol, corn fiber gum, oligosaccharides, phytosterols, and polyols. Fiber is not fermented in the dry‐grind corn process. Its separation before fermentation would increase ethanol productivity in the fermenter. Recently, we showed that the elusieve process, a combination of sieving and elutriation (air flow), was effective in fiber separation from DDGS. In this study, we evaluated the elusieve process for separating pericarp fiber from corn flour. Corn flour remaining after fiber separation was termed “enhanced corn flour”. Of the total weight of corn flour, 3.8% was obtained as fiber and 96.2% was obtained as enhanced corn flour. Neutral detergent fiber (NDF) of corn flour, fiber, and enhanced corn flour (dry basis) were 9.0, 61.5, and 5.7%, respectively. Starch content of corn flour, fiber, and enhanced corn flour (dry basis) were 68.8, 23.5, and 71.3%, respectively. Final ethanol concentration from enhanced corn flour (14.12% v/v) was marginally higher than corn flour (13.72% v/v). No difference in ethanol yields from corn flour and enhanced corn flour was observed. The combination of sieving and air classification can be used to separate pericarp fiber from corn flour. The economics of fiber separation from corn flour using the elusieve process would be governed by the production of valuable products from fiber and the revenues generated from the valuable products.  相似文献   

10.
Settleability of dry and wet weather flow samples from a combined sewer system was examined by settling column tests, in order to improve understanding of settling processes and obtain information for design of settling tanks. In fact, these tests mimic the actual settling processes and allow evaluating total suspended solids (TSS) removal by settling. Therefore, it is also possible to assess, indirectly, removals of other pollutants, such as heavy metals, which are generally transported by solid particles in sewage. Towards this end, dry and wet weather flow samples were collected in the Liguori Channel catchment and analyzed in the laboratory for Water Supply and Sewerage (Acquedotti e Fognature) of the University of Calabria for TSS concentrations according to the Standard Methods. The settleability study revealed that removals of TSS in dry weather samples (i.e., sanitary sewage) were greater than in wet weather samples (WW), using the same experimental procedures. In particular, 65% of TSS was removed in dry weather samples at a depth of 3?m for a detention time of 40?min; while in wet weather samples the comparable removal efficiency was less than 60%.  相似文献   

11.
By a leaching experiment with glass columns packed with submerged paddy soils, the relationships among numbers of total bacteria, total Gram-positive bacteria, culturare aerobic bacteria and a amount of bacterial biomass both in the leachate, and in the subsoil after leaching incubation were studied. The leachate from soil columns was collected every 3 d during the 30-d incubation period. The soil columns were packed with plow layer soil samples with and without rice straw (RS) amendment, and the subsoil column was connected to the plow layer soil column without RS. Numbers of total bacteria, culturable aerobic bacteria, and a amount of bacterial biomass in the leachate decreased with the incubation time. There was no correlation between the number of total bacteria in the leachate and the concentration of total organic carbon in the leachate. Bacteria less than 0.1 µsm3 in size predominated in the leachate, especially in that from the plow layer soil column with RS. Percentages of the number of Gram-positive bacteria in the leachate were very low (less than 7% of the total bacterial number), while the percentage in the subsoil after the leaching experiment was in the range of 21–82%. The sum of the number of bacteria percolated from the plow layer soil column with RS during the 30-d period of incubation and the sum of the amount of biomass C were 39 and 77% less than the corresponding values for the bacteria percolated from the plow layer soil column without RS. Percentages of culturable aerobic bacteria among the total bacteria ranged between 2.8 and 37% in the leachate, while less than 0.6% in the subsoil after the leaching experiment.  相似文献   

12.
A simple, rapid, and efficient partitioning column consisting of acetonitrile on Florisil has been developed for the separation of pesticides from fish, beef, and butter fat. The efficiency of the cleanup column is between 97 and 100%. Nine pesticides having partition coefficients between n-hexane and acetonitrile of less than or equal to 0.05 were satisfactorily separated from fat with good recoveries. When the column was used to clean up temephos in a fish extract, 99.91% of the fat was eluted with 20 ml n-hexane with no loss of the pesticide.  相似文献   

13.
A new cleanup procedure is described for chlorinated hydrocarbon residues in butterfat. The method is based on the dropwise addition of H2SO4 to a fat solution column and continuous removal of the lipids and the acid. The cleanup of 0.25-2.0 g fat requires only 10-40 ml sulfuric acid and 12-17 ml petroleum ether. There is no need for any further cleanup step, solvent evaporation, or centrifugation. The method is easy to standardize and is suitable for automation. At least 30 fat samples can be cleaned up manually by one analyst in one day. Recoveries were complete (greater than 90%) for polychlorinated biphenyl compounds and for 13 chlorinated pesticides of 16 examined. The method was tested on chlorinated hydrocarbon residues in commercial butter and the results were compared with those obtained with the acetonitrile method. The versatility and limitations of the method were investigated by varying the sulfuric acid strength, initial fat solution concentration, and column dimensions.  相似文献   

14.
The Diagnosis and Recommendation Integrated System (DRIS) of interpreting results of foliar analysis is an alternative to the Critical Nutrient Level (CNL) system. DRIS uses indices of ratios of nutrient concentrations and has been found to be more accurate in predicting nutrient needs for numerous crops than the CNL system. The objectives of this research were to estimate and validate DRIS norms for dry bean (Phaseolus vulgaris L.) determined from a broad‐based data set. The previously recommended foliar CNL's of 3.0% N, 0.25% P, and 1.0% K were found to be too low to be useful in predicting responses to applied fertilizers in the test environments. Prediction based on levels of 4.7% N, 0.32% P, and 1.4% K was more accurate than with the lower CNL values. DRIS was more accurate than either set of CNL values in predicting responses to applied N, P, and K. Diagnosis with DRIS was less affected by plant age than CNL.  相似文献   

15.
新疆麦后复播大豆适宜滴灌量研究   总被引:1,自引:0,他引:1  
【目的】随着北疆地区麦-豆两熟种植面积的不断扩大,麦后复播大豆加剧了与春播作物的用水矛盾,因此,为缓解农业用水压力,本研究通过设定不同滴灌量,从中筛选出适宜复播大豆种植的灌水量,为复播大豆节水、 优质高产栽培技术提供理论依据。【方法】在大田滴灌条件下,以‘黑河43′为试验材料,采取单因素随机区组试验设计,通过设置3000、 3600、 4200、 4800 m3/hm2四个灌溉量处理,研究滴灌量对复播大豆干物质积累、 分配及植株中养分吸收特征的影响。【结果】复播大豆干物质、 植株中N、 P2O5及K2O的积累均符合Logictic生长函数模型。复播大豆单株干物质重随着滴灌量的增加呈“先增后降”的变化趋势,以灌水量4200 m3/hm2处理最高; 各处理干物质最大积累速率均在出苗后49.5~53.0 d,快速积累期为30.3~31.9 d,最大积累速率平均为0.48 g/(plant·d)。不同滴灌量处理大豆植株中N、 P2O5和K2O含量随着滴灌量的增加亦呈“先增后降”的变化趋势,最大吸收速率分别出现在苗后47.1~49.9 d、 44.8~45.1 d和44.6~46.1 d,快速积累期分别为31.7~36.4 d、 22.2~22.4 d和28.7~31.46 d,最大积累速率平均分别为26.35、 8.15和9.30 mg/(plant·d)。滴灌量和产量之间的关系呈开口向下的抛物线,以4200 m3/hm2(W3处理)最高,为3741.23 kg/hm2,分别较3000、 3600和4800 m3/hm2三个处理增产30.42%、 13.98%和8.44%。子粒中蛋白质和脂肪含量呈负相关关系,蛋白质和脂肪总量以4200 m3/hm2处理最高,为53.03%。【结论】适当增加灌水量,不仅能够促进复播大豆植株养分的吸收、 积累,增加干物质积累量,同时还提高了子粒中蛋白质和脂肪的总含量。但灌水量过多或过少,均不利于复播大豆干物质积累及养分的吸收利用,导致产量降低。因此,推荐灌水量为4200 m3/hm2作为北疆复播大豆高产、 节水的合理灌溉定额。  相似文献   

16.
A procedure is described for the isolation and cleanup of hexachlorobenzene (HCB) and mirex in fats and oils for gas-liquid chromatographic (GLC) analysis. The fat or oil is distributed on unactivated Florisil, and the HCB and mirex are eluted with acetonitrile. The pesticides are then partitioned into petroleum ether. Elution through activated Florisil with methylene chloride-hexane (20+80) is used for the final cleanup. HCB and mirex are then measured by GLC, using the appropriate electron capture conditions with a 15% OV-210 column for HCB and a 3% OV-101 column for mirex. The method demonstrates recoveries greater than 90% for HCB and mirex and allows screening at or below the 0.1 ppm level in fats with a 3 mg fat injection.  相似文献   

17.
Determination of halogenated contaminants in human adipose tissue   总被引:2,自引:0,他引:2  
A method has been developed for determination of organochlorine contaminants in human adipose tissue. After fat extraction from the tissue with acetone-hexane (15 + 85, v/v), organochlorines were fractionated from fat by gel permeation chromatography with methylene chloride-cyclohexane (1 + 1, v/v) as solvent. After Florisil column cleanup, the GPC extract was analyzed by capillary column gas chromatography using 2 columns of different polarity. Compound identity was confirmed by gas chromatography-mass spectrometry using selected ion monitoring. Recoveries for fortification levels of 10-500 ng/g were greater than 80% except for trichlorobenzene and hexachlorobutadiene (ca 60%).  相似文献   

18.
Leafy vegetables [Basella rubra L., Peucedanum sowa Roxb., Moringa oleifera Lam., Trigonella foenum-graecum L., Spinacia oleracea L., Sesbania grandiflora (L.) Poir., and Raphanus sativus L.] that are commonly used by the rural population in India were evaluated in terms of their main carotenoid pattern. The extracted carotenoids were purified by open column chromatography (OCC) on a neutral alumina column to verify their identity by their characteristic UV-visible absorption spectra. Reverse-phase high-performance liquid chromatography (HPLC) on a C18 column with UV-visible photodiode array detection under isocratic conditions was used for quantification of isolated carotenoids. Acetonitrile/methanol/dichloromethane (60:20:20 v/v/v) containing 0.1% ammonium acetate was used as a mobile phase. The major carotenoids identified by both methods were lutein, beta-carotene, violaxanthin, neoxanthin, and zeaxanthin. Among the carotenoids identified, lutein and beta-carotene levels were found to be higher in these leafy vegetables. Results show that P. sowa and S. oleracea are rich sources of lutein (77-92 mg/100 g of dry wt) and beta-carotene (36-44 mg/100 g of dry wt) compared with other leafy vegetables. The purity of carotenoids eluted by OCC was clarified by HPLC, and they were found to be 92% +/- 3% for neoxanthin, 94% +/- 2% for violaxanthin, 97% +/-2% for lutein and zeaxanthin, and 90% +/- 3% for beta-carotene. It could be recommended to use P. sowa and S. oleracea as rich sources of lutein and beta-carotene for health benefits. The OCC method proposed is relatively simple and provides purified carotenoids for feeding trials.  相似文献   

19.
The ignition method and the perchloric acid (HClO4) digestion method for the determination of total phosphorus (P) content in 65 agricultural soils of Taiwan were compared. The average amount of total P obtained by the ignition method was 4.3% less than that obtained by the HClO4 method. There was a wide range of variation, from 37% less to 21% more in the ignition method than those results obtained by the HClO4 digestion method. Because the ignition method can also be used for the estimation of soil organic P and is thus worthy of further study, it should be adopted as a routine procedure.  相似文献   

20.
Soybean (Glycine max (L.) Merrill) plants normally abort a high percentage of flowers and pods. This study was conducted to determine the effect of P nutrition on flower and pod abscission in soybean. Williams 82 soybeans were established in hydroponic culture in the greenhouse at four levels of P (0.45 mM, 0.20 mM, 0.10 mM or 0.05 mM), and main stem flowers and pods were counted every two days from flowering to maturity. The two highest P treatments had similar flower production, pod production, pod abortion, seed weight and seeds per pod, but the 0.20 mM P treatment had 20% lower dry matter production and 19% lower seed yield. At P supplies of 0.10 or 0.05 mM, flower production, pod production, flowers per node, pods per node, seed yield, seed number and weight per seed were less (P < 0.05) than at 0.20 mM. Flowers produced per main stem node and seeds per pod were largely unaffected by limited P. Plants supplied 0.10 or 0.05 mM P aborted more flowers and pods than did those supplied 0.45 or 0.20 mM P. At P supply of 0.05 mM, flower, pod and total abortion was 80%, 49% and 90%, respectively. Flower and pod production were 50% and 78% less, while plant dry weight, seed yield and weight per seed were 83%, 90% and 23% less, respectively for the 0.05 mM P treatment compared to control. The data indicate that the primary effect of limited P on reproductive growth of soybean is to increase flower and pod abortion.  相似文献   

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