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1.
A rapid, simple, and reliable method for the determination of individual glucosinolates in canola seeds was developed using a semiquantitative extraction of glucosinolates with anion exchange membranes and HPLC detection. In this one-step extraction procedure, a membrane (7 cm(2)) is placed in the seed suspension prepared by grinding and boiling 0.8 g of seeds in 20 mL of water. After 10 min of shaking on the mechanical shaker, the membrane is removed from the suspension, washed, and transferred to a vial containing 5 mL of 1 N tetramethylammonium chloride. The glucosinolates are eluted from the membrane by shaking the membrane for 10 min with the eluting solvent. The glucosinolate content in membrane eluates is determined by HPLC using sinigrin standards. A coefficient of variation ranging from 1.9 to 7.6% for aliphatic glucosinolates indicated very good reproducibility of the method. Because of the instability of 4-hydroxyglucobrassicin, the coefficient of variation for the determination of this indolyl glucosinolate was 13.9%. To verify the results of the membrane extraction/HPLC detection, this new method was compared with the existing colorimetric and GC procedures. Very good correlation (R(2) = 0.98) was obtained between the total glucosinolates determined by the membrane extraction/HPLC method and the palladate colorimetric procedure for 17 canola varieties. Concentrations of individual glucosinolates in five canola varieties were compared with the GC data. Very good agreement between these two methods was obtained for aliphatic glucosinolates. However, the membrane extraction/HPLC method yielded slightly higher values for 4-hydroxyglucobrassicin than the GC method, possibly indicating that the decomposition of this glucosinolate was reduced during the sample extraction with the membranes. The simplicity and low cost of the membrane extraction/HPLC method make it an attractive alternative to the existing procedures for glucosinolate analysis in canola seeds.  相似文献   

2.
Hydrophobic cyclic peptides, termed cyclolinopeptides, found in flaxseed are known for their immunosuppressive activity. This study is the first report of the occurrence of cyclolinopeptides in flaxseed fractions and products produced by aqueous processing and cold pressing. The distribution of cyclolinopeptides in flaxseed was determined after processing of flaxseed by various industrial and laboratory processes. Extracts of the water-soluble mucilage did not contain cyclolinopeptides. The cotyledon had the highest concentration of cyclolinopeptides, whereas seed coat had lower levels. An oil body fraction separated from seed after homogenization in water, followed by centrifugation, had the highest concentration of cyclolinopeptides of the fractions produced by this method. Further washing of the oil body fraction led to a loss of cyclolinopeptides. When oilseed was extruded using an expeller press, cyclolinopeptides were found in greater concentrations in crude oil and the solid sediment present in the oil fraction than in meal or the unprocessed seed. The concentration of cyclolinopeptides in crude flaxseed oil immediately after pressing was much higher than that observed in flaxseed oils purchased from a retail outlet. The effect of oil refining treatments on the removal of cyclolinopeptides was also tested. Acid degumming using aqueous H(3)PO(4) removed cyclolinopeptides from crude flaxseed oil. Alkali refining was less effective as this treatment failed to remove all peptides equally. This work illustrates ways that cyclolinopeptides may be extracted from flaxseed oil that could be developed for large-scale industrial extraction. The ability to extract cyclolinopeptides on a larger scale would allow faster exploitation of commercial applications of these molecules and provide the flaxseed industry with value-added coproducts.  相似文献   

3.
Chlorella is a nutrient-rich microalga that contains protein, lipid, minerals, vitamins, and high levels of lutein. This study evaluated the bioavailability of lutein from Chlorella vulgaris using a coupled in vitro digestion and human intestinal Caco-2 cell model. Lutein bioaccessibility was low, and approximately 75% of total C. vulgaris lutein was not micellized during the digestion process but remained in the insoluble digestate. Microfluidization improved lutein micellization efficiency during C. vulgaris digestion. C. vulgaris was microfluidized at a pressure exceeding 10000 psi, and the cell surface disruption was visualized by scanning electron microscopy. The mean C. vulgaris particle size was reduced from 3.56 to 0.35 μm with the microfluidization treatment. C. vulgaris microfluidization at 20000 psi was three times more efficient for aqueous lutein micelles production as compared with untreated C. vulgaris, and the final lutein content accumulated by intestinal Caco-2 cells was also higher with microfluidization. C. vulgaris lutein stability was not affected by microfluidization. These results indicate that microfluidization may be useful for improving lutein bioaccessibility from C. vulgaris during food processing.  相似文献   

4.
小叶女贞果实花青素组分鉴定及色谱纯化技术   总被引:2,自引:1,他引:1  
为提高小叶女贞果实的食用、药用价值,该文系统研究了果实中花青素种类构成及提取物的制备技术。试验采用紫外可见光谱法、高效液相色谱-质谱串联法、酸水解制备苷元等技术对小叶女贞果实花青素含量、单体种类进行了测定,并借助提取、萃取、柱层析等技术研究了花青素提取物的分离纯化过程。研究结果如下:测得每100 g小叶女贞果实中含花青素总量为(499±18.42)mg,从中鉴定出2种花青素单体,分别为矢车菊素-3-O-葡萄糖苷和牵牛花色素-3-O-葡萄糖苷,并以后者为主要存在形式;获得了纯天然、简单易行的花青素提取物制备技术,主要包括酸化乙醇提取、乙酸乙脂萃取、Amberlite XAD-7HP大孔树脂层析分离步骤,最终制得的花青素提取物纯度为35%、得率为0.6%。该研究为后期制备高纯度牵牛花素-3-O-葡萄糖苷单体提供了良好原料基础,为深入研究小叶女贞果实花青素功能活性及其在食品、药品领域潜在应用提供了参考。  相似文献   

5.
超声波辅助提取杠柳脂溶性成分工艺优化   总被引:1,自引:1,他引:0  
为了优化超声波辅助提取杠柳脂溶性成分的工艺,该文在单因素试验基础上,选取超声波功率、提取时间、液料比为主要影响因素,分析了3个主要影响因素对杠柳脂溶性成分提取结果的影响,应用响应面分析法优化了超声波辅助提取杠柳脂溶性成分的工艺方法,并使用GC-MS联用仪检测了杠柳脂溶性提取物的主要成分。结果表明:超声波辅助提取杠柳营养体脂溶性成分的最佳工艺为:在室温(20℃)及超声波频率20kHz条件下,提取试剂为石油醚,超声波辅助提取时间为70min,超声波功率为730W,料液比为1∶10g/mL。该工艺条件下,杠柳脂溶性成分的实际提取得率可达到6.14%。  相似文献   

6.
Crude glycerol is the primary byproduct of the biodiesel industry. Producing docosahexaenoic acid (DHA, 22:6 n-3) through fermentation of the alga Schizochytrium limacinum on crude glycerol provides a unique opportunity to utilize a large quantity of this byproduct. The objective of this work is to investigate the effects of impurities contained in the crude glycerol on DHA production and algal biomass composition. Crude glycerol streams were obtained from different biodiesel refineries. All of the glycerol samples contained methanol, soaps, and various elements including calcium, phosphorus, potassium, silicon, sodium, and zinc. Both methanol and soap were found to negatively influence algal DHA production; these two impurities can be removed from culture medium by evaporation through autoclaving (for methanol) and by precipitation through pH adjustment (for soap). The glycerol-derived algal biomass contained 45-50% lipid, 14-20% protein, and 25% carbohydrate, with 8-13% ash content. Palmitic acid (C16:0) and DHA were the two major fatty acids in the algal lipid. The algal biomass was rich in lysine and cysteine, relative to many common feedstuffs. Elemental analysis by inductively coupled plasma showed that boron, calcium, copper, iron, magnesium, phosphorus, potassium, silicon, sodium, and sulfur were present in the biomass, whereas no heavy metals (such as mercury) were detected in the algal biomass. Overall, the results show that crude glycerol was a suitable carbon source for algal fermentation. The crude glycerol-derived algal biomass had a high level of DHA and a nutritional profile similar to that of commercial algal biomass, suggesting a great potential for using crude glycerol-derived algae in omega-3-fortified food or feed.  相似文献   

7.
Thermally assisted hydrolysis and methylation-gas chromatography (THM-GC) in the presence of trimethylsulfonium hydroxide, using a vertical microfurnace pyrolyzer, was validated for the compositional analysis of fatty acid components in microalgae. The chromatograms of a microalga, Pavlova lutheri , obtained under optimized THM conditions clearly showed a series of fatty acid methyl esters including thermally labile polyunsaturated fatty acid components. On the basis of these peak areas, their chemical compositions were rapidly determined without using any tedious sample pretreatment with a precision of <8% relative standard deviation. Moreover, the compositions thus obtained were in good agreement with those obtained by the conventional technique involving solvent extraction. Finally, the THM-GC technique was applied for the compositional analysis of fatty acid components in a newly found microalga, Coccomyxa gloeobotrydiformis . The obtained data showed a high abundance (24 mol %) of α-linolenic acid components, suggesting its potential usefulness as feed sources and/or functional foods.  相似文献   

8.
Nonylphenol (NP), nonylphenol mono- and di-ethoxylate (NP1EO, NP2EO) and bisphenol A (BPA) were determined in water, suspended particulate matter (s.p.m.) and bed sediment collected from the most polluted stretch of Tiber river (Italy) in the neighbourhood of Rome. Analytes were recovered from water samples by solid-phase extraction (SPE) on Si–C18 cartridges and analysed by HPLC with fluorescence detection. Solid samples were extracted by using an aqueous solution of the non-ionic surfactant Tween 80. Results indicated that 2–42% of NP, 9–45% of NP1EO, 11–18% of NP2EO and 4–62% of BPA respectively occurred in the suspended phase. In general, for all compounds a higher affinity for s.p.m. than for bed sediments was observed, reflecting differences in the nature of particles and in their sorption capacity for organic micro-pollutants. The partition of target compounds in river compartments was affected by differences in hydrological conditions between the two sampling campaigns. Run-off from the basin or resuspension/redissolution from sediments was an important source of nonylphenol and bisphenol A during high discharge regimes. Partition coefficients of compounds (log K oc ) between water and s.p.m. were calculated under stable flow condition. K oc values, experimentally measured in the river, were higher than those predicted by K ow , implying that specific chemical interaction could occur in the sorption mechanisms for these group of compounds.  相似文献   

9.
A novel, rapid, and economical method to isolate and purify natural sulforaphane from broccoli seeds is described. The procedure involves solvent extraction of autolyzed seed meal, followed by separation by solid phase extraction (SPE) and purification by preparative high-performance liquid chromatography (HPLC). The SPE method provides higher yield of sulforaphane from crude extracts compared to conventional liquid-liquid extraction. High purity and recovery of sulforaphane product can be obtained by preparative HPLC with a C 18 column and 30% methanol in water as the mobile phase. The purified compound was characterized by MS and (1)H and (13)C NMR. The techniques described here are useful tools in the preparative-scale isolation of sulforaphane in a fast, cost-effective, and waste-conscious manner.  相似文献   

10.
With increasing production of distillers dried grains with solubles (DDGS), both fuel ethanol and animal feed industries are demanding standardized protocols for characterizing quality. AOCS Approved Procedure (Am 5‐04) was used for measuring crude oil content in milled corn and resulting DDGS. Selected factors, including sample type (milled corn, DDGS), sample origin (ethanol plant 1, 2, 3), sample particle size (original matrix, <0.71 mm, <0.50 mm mesh opening; the last two materials were obtained by grinding and sieving), solvent type (petroleum ether, hexane), extraction time (30, 60 min), and postextraction drying time (30, 60 min) were investigated by a complete factorial design. For milled corn, only sample origin and extraction time had significant effects (P < 0.05) on crude oil values measured, but for DDGS, besides those two factors, sample particle size, solvent type, and drying time also had significant effects. Among them, the particle size of DDGS had the most effect. On average, measured oil content in DDGS ranged from 11.11% (original matrix) to 12.12% (<0.71 mm) and to 12.55% (<0.50 mm). For measuring the crude oil content of DDGS, particle size reduction, 60 min of extraction, and 60 min of drying are recommended. Regardless of the underlining factors, the method was very repeatable (standard errors <0.05). The observed particle size effect on crude oil analysis of DDGS suggests the need for similar confirmations using other analytical methods.  相似文献   

11.
为了优化水提法小球藻多糖提取的工艺,该文在单因素试验的基础上,选择水料质量比、超声波功率、提取时间、冻融-超声波次数进行4因素3水平的正交试验提取小球藻多糖,采用三氯乙酸法去除游离蛋白质。结果表明:小球藻多糖最佳提取条件为水料质量比15,超声波功率600W,超声波作用时间6min和冻融-超声波2次,小球藻粗多糖得率为5.918%。三氯乙酸法脱游离蛋白质以pH值为4为最佳,多糖回收率为57.84%。该研究可为从小球藻中大规模分离和提取以及纯化多糖提供参考。  相似文献   

12.
The N-methylcarbamate pesticide carbaryl is one of the most important insecticides used worldwide. In the present work, the validation of a monoclonal antibody-based enzyme immunoassay (ELISA) for the determination of this compound in fruits and vegetables is described. The immunoassay is a competitive heterologous ELISA in the antibody-coated format, with an I(50) value for standards in buffer of 101.0 +/- 26.9 ng/L and with a dynamic range between 31.6 and 364.0 ng/L. For recovery studies, peppers, cucumbers, strawberries, tomatoes, potatoes, oranges, and apples were spiked with carbaryl at 10, 50, and 200 ppb. After liquid extraction, analyses were performed by ELISA on both extracts purified on solid-phase extraction (SPE) columns and crude, nonpurified extracts. Depending on the crop and the fortification level, recoveries in the 59.0--120.0% range were obtained for purified samples and in the 70.0--137.7% range for crude extracts. The carbaryl immunoassay performance was further validated with respect to high-performance liquid chromatography (HPLC) with postcolumn derivatization and fluorescence detection (EPA Method 531.1). Samples were spiked with carbaryl at several concentrations and analyzed as blind samples by ELISA and HPLC after SPE cleanup. The correlation between methods was excellent (y = 1.04x + 0.71, r(2) = 0.992, n = 33), with HPLC being more precise than ELISA (mean coefficients of variation of 5.2 and 12.0%, respectively). The immunoassay was then applied to the analysis of nonpurified extracts of the same samples. Results also compared very well with those obtained by HPLC on purified samples (y = 1.28x - 0.59, r(2) = 0.987, n = 33) while maintaining similar precision. Therefore, the developed immunoassay is a suitable method for the quantitative and reliable determination of carbaryl in fruits and vegetables even without sample cleanup, which saves time and money and considerably increases sample throughput.  相似文献   

13.
The N-methylcarbamate pesticide carbofuran is a very important insecticide used worldwide. In the present work, the validation of a monoclonal antibody-based enzyme immunoassay (ELISA) to determine this compound in fruits and vegetables is described. The immunoassay is a competitive heterologous ELISA in the antibody-coated format, with an I(50) value for standards in buffer of 740 ng/L and with a dynamic range between 200 and 3100 ng/L. For recovery studies, peppers, cucumbers, strawberries, tomatoes, potatoes, oranges, and apples were spiked with carbofuran at 10, 50, and 200 ppb. After liquid extraction, analyses were performed by ELISA on extracts purified on solid-phase extraction (SPE) columns and crude, nonpurified extracts. Depending on the crop, mean recoveries in the 43.9--90.7% range were obtained for purified samples and in the 90.1--121.6% range for crude extracts. The carbofuran immunoassay performance was further validated with respect to high-performance liquid chromatography (HPLC) with postcolumn derivatization and fluorescence detection (EPA Method 531.1). Samples were spiked with carbofuran at several concentrations and analyzed as blind samples by ELISA and HPLC after SPE cleanup. The correlation between methods was very good (y = 0.90x + 2.66, r(2)() = 0.958, n = 25), with HPLC being more precise than ELISA (mean coefficients of variation of 4.1 and 11.5%, respectively). The immunoassay was then applied to the analysis of nonpurified extracts of the same samples. Results also compared very well with those obtained by HPLC on purified samples (y = 1.02x + 10.44, r(2)() = 0.933, n = 29). Therefore, the developed immunoassay is a suitable method for the quantitative and reliable determination of carbofuran in fruits and vegetables even without sample cleanup, which saves time and money and considerably increases the sample throughput.  相似文献   

14.
重金属高污染农田土壤EDTA淋洗条件初探   总被引:7,自引:1,他引:6  
通过室内振荡淋洗试验研究了乙二胺四乙酸二钠(EDTA)浓度、淋洗时间、液固比、淋洗次数对甘肃省白银市某高污染农田土壤中重金属去除效果的影响,并测定了EDTA淋洗前后土壤中重金属形态的变化。结果表明:淋洗剂浓度和液固比越高、淋洗时间越长、淋洗次数越多,对重金属的去除效果越好。在EDTA浓度为5 mmol/L、液固比为2.5、连续振荡淋洗3次、每次1 h时,对土壤中Cd、Cu、Pb、Zn 4种重金属的总去除率分别为 55.2%、21.9%、19.3% 和20.9%,其中Cd 淋洗效率最高。EDTA对土壤中交换态、碳酸盐结合态和铁锰氧化物结合态重金属的去除效果明显,但不能有效去除有机及硫化物态和残余态土壤重金属。  相似文献   

15.
Arsenic, lead, and phosphorous contamination in soils represents a health risk. Chitosan (poly-N-acetyl glucosamine) inexpensive by-product derived from chitin has been used as a metals adsorbent. Objectives of this research were to evaluate the effectiveness of chitosan solution for arsenic, lead, and phosphorous extraction from lead-arsenate contaminated soils, and evaluate the effectiveness of protonated chitosan flakes (PCF) and ferric hydroxide chitosan beads (Fe(III)-CB) for water-soluble As removal from these soils. Percentage of arsenic, lead, and phosphorous removed from the soils by chitosan solution ranged from 0.96% to 17%, 1.80% to 31%, and 0.66% to 11%, respectively. Percentage of water-soluble arsenic removed by PCF and by Fe (III)-CB ranged from 12% to 47% and 36% to 77%, respectively. Averaged over soils, Fe (III)-CB removed slightly more arsenic (As) (42 mg kg?1) compared to Mehlich III (40 mg kg?1) extractant. Results indicate potential for the use of chitosan as an extraction for lead-arsenate contaminated soils.  相似文献   

16.
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   

17.
High‐intensity ultrasound (sonication) was investigated as a method to rapidly purify starch from sorghum and other cereal grains. To improve the process, buffers were optimized to solubilize sorghum proteins in combination with the sonication. Protein content and starch color were determined to evaluate the efficiency of the extraction process. Sonication times, SDS concentration, different types and concentrations of reducing agents (sodium metabisulfite, dithiothreitol, and β‐mercaptoethanol), and centrifugation speeds of the starch washing procedure were tested. Protein content of isolated sorghum starch was reduced to 0–0.14% (db) after 2 min of sonication (using any of the reducing agents tested). Sodium metabisulfite was chosen as the preferred reducing agent because of its lower toxicity and odor compared with other reducing agents tested. The optimum conditions for producing high‐purity sorghum starches (0.06% protein) were obtained using the following conditions: 2 min of sonication time with 12.5 mM sodium borate buffer, pH 10, containing 0.5% SDS (w/v) and 0.5% sodium metabisulfite (w/v) using 1,500 rpm centrifugation speed during starch washing. Starches separated by this method showed significantly less protein content and b values (yellowness) compared with starches separated by enzymatic methods or methods using NaCl solutions and protein extraction buffers with multiple washing steps, both of which take several hours to complete. Differential scanning calorimetry thermogram values for starches isolated by three different methods showed similar patterns, except that starches obtained with the enzymatic method had slightly higher values of To, Tp, and ΔH. Other cereal starches from whole wheat meal, wheat flour, corn, rice, and barley were also obtained rapidly using sonication.  相似文献   

18.
Commercially prepared marigold flower (Tagetes erecta) extract was saponified and analyzed for carotenoid composition. HPLC analyses were performed on two normal-phase columns (beta-Cyclobond and silica) and on a C(30) reversed-phase column. The extract contained 93% utilizable pigments (detected at 450 nm), consisting of all-trans and cis isomers of zeaxanthin (5%), all-trans and cis isomers of lutein, and lutein esters (88%). All were identified by chromatographic retention, UV-visible spectra, and positive ion electrospray mass spectrometry in comparison to authentic standards. Contrary to previous findings, insignificant levels (<0.3%) of lutein oxidation products were detected in the saponified extract. This compositional determination is important for the application of marigold extract in nutritional supplements and increases its value as a poultry feed colorant because it contains more biologically useful lutein compounds than previously believed.  相似文献   

19.
A study of the nonvolatile fraction of extracts from vine shoots obtained by superheated ethanol-water mixtures is presented. The influence of the temperature, extraction time, and percentage of ethanol on extraction was investigated by a multivariate experimental design to maximize the yield of total phenolic compounds, measured by using the Folin-Ciocalteu method. The best values found for these variables were 80% (v/v) ethanol, 240 degrees C, and 60 min. Under these conditions, the effect of pH was also investigated, and a strong improvement of yield was observed by decreasing the pH. The extracts were subject to liquid-liquid extraction with n-hexane. The remaining polar phase was dried in a rotary evaporator and then reconstituted in 10 mL of water. The insoluble residue was dissolved in 10 mL of methanol. Both fractions (aqueous and methanolic) were analyzed by HPLC, and the differences in composition according to the extraction conditions were studied. Compounds usually present in commercial wood extracts were identified (mainly benzoic and hydroxycinnamic acids and aldehydes); the most abundant were quantified, and the stability of the identified phenolic families under different extraction conditions was also investigated. Finally, the superiority of the superheated liquid extraction over conventional solid-liquid extraction was demonstrated.  相似文献   

20.
A process for the value addition of solid waste from two-phase olive oil extraction or "alperujo" that includes a hydrothermal treatment has been suggested. In this treatment an autohydrolysis process occurs and the solid olive byproduct is partially solubilized. From this water-soluble fraction can be obtained besides the antioxidant hydroxytyrosol several other compounds of high added value. In this paper three different samples of alperujo were characterized and subjected to a hydrothermal treatment with and without acid catalyst. The main soluble compounds after the hydrolysis were represented by monosaccharides xylose, arabinose, and glucose; oligosaccharides, mannitol and products of sugar destruction. Oligosaccharides were separated by size exclusion chromatography. It was possible to get highly purified mannitol by applying a simple purification method.  相似文献   

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