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1.
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
2.
Steinke G Weitkamp P Klein E Mukherjee KD 《Journal of agricultural and food chemistry》2001,49(2):647-651
Fatty acids obtained from seed oils of crambe (Crambe abyssinica) and camelina (Camelina sativa) via alkaline saponification or steam splitting were esterified using lipases as biocatalysts with oleyl alcohol and the alcohols derived from crambe and camelina oils via hydrogenolysis of their methyl esters. Long-chain wax esters were thus obtained in high yields when Novozym 435 (immobilized lipase B from Candida antarctica) and papaya (Carica papaya) latex lipase were used as biocatalysts and vacuum was applied to remove the water formed. The highest conversions to wax esters were obtained with Novozym 435 (> or =95%) after 4-6 h of reaction, whereas with papaya latex lipase such a high degree of conversion was attained after 24 h. Products obtained from stoichiometric amounts of substrates were almost exclusively (>95%) composed of wax esters having compositions approaching that of jojoba (Simmondsia chinensis) oil, especially when crambe fatty acids in combination with camelina alcohols or camelina fatty acids in combination with crambe alcohols were used as substrates. 相似文献
3.
《Communications in Soil Science and Plant Analysis》2012,43(21-22):3211-3224
Crambe (Crambe abyssinica L.) is a specialty oilseed crop. By‐product crambe meal has a high glucosinolate content, restricting its use for animal feed. The purpose of this study was to evaluate crambe meal for various types of soil application. When incubated with soil, crambe meal mineralized more slowly than soybean meal, with an average of 38% of the added nitrogen (N) from crambe meal appearing as mineral N after 12 weeks of incubation, compared with 57% for soybean (Glycine max L. Merr.) meal. Sulfur mineralization from crambe meal was rapid. Bioassays indicated no phytotoxicity to seedlings from crambe meal. In a second experiment, high rates of crambe meal inhibited the nitrification of urea added to soil, but this effect was short‐lived. In a third experiment, crambe meal–ferrous sulfate mixtures applied to calcareous soil partially alleviated iron deficiency chlorosis of soybean, but the response was less than observed with iron–ethylenediaminedi(o‐hydroxyphenylacetic) acid. 相似文献
4.
Tilay A Bule M Kishenkumar J Annapure U 《Journal of agricultural and food chemistry》2008,56(17):7644-7648
Ferulic acid (FA) is a phenolic antioxidant present in plants, which is widely used in the food and cosmetic industry. In the present study, various agricultural wastes such as maize bran, rice bran, wheat bran, wheat straw, sugar cane baggasse, pineapple peels, orange peels, and pomegranate peels were screened for the presence of esterified FA (EFA). Among the sources screened, maize bran was found to contain the highest amount of EFA. Pineapple peels, orange peels, and pomegranate peels were also found to contain traces of EFA. Alkaline extraction of EFA from maize bran was carried out using 2 M NaOH. Response surface methodology (RSM) was used for optimization of EFA extraction, which resulted in a 1.3-fold increase as compared to the unoptimized conventional extraction technique. FA was analyzed by means of high-performance liquid chromatography (HPLC). Purification was carried out by adsorption chromatography using Amberlite XAD-16 followed by preparative high-performance thin-layer chromatography (HPTLC). The recovery of Amberlite XAD-16 purified FA was up to 57.97% with HPLC purity 50.89%. The fold purity achieved was 1.35. After preparative HPTLC, the maximum HPLC purity obtained was 95.35% along with an increase in fold purity up to 2.53. 相似文献
5.
In order to produce large amounts of pure sulforaphane for research purposes, a novel method using high-speed countercurrent chromatography (HSCCC) was developed. Without any initial cleanup steps, sulforaphane was successfully purified from the ethyl acetate extract of the broccoli seed meal by HSCCC. The separation was performed with two-phase solvent systems: n-hexane/ethyl acetate/methanol/water (1:5:1:5, v/v/v/v). From 850 mg of the ethyl acetate extract, 186 mg of sulforaphane was isolated with the solvent system. The purified compound was over 97% purity as determined by HPLC analysis, and the chemical structure was confirmed by MS and (1)H and (13)C NMR. 相似文献
6.
Dell'Agli M Giavarini F Ferraboschi P Galli G Bosisio E 《Journal of agricultural and food chemistry》2007,55(9):3363-3367
This work describes a sensitive high-performance liquid chromatography (HPLC) method for the quantification of aloesin and aloeresin A in alcoholic beverages containing aloe as a flavoring agent. The compounds were prepared from Aloe ferox juice. Sephadex LH20 and ion-exchange resin AG1X2 column chromatography were used for aloesin. Aloeresin A was obtained by Sephadex LH20 and silica gel column chromatography followed by purification on Discovery DSC-18 solid-phase extraction tubes. A 98 mg amount of aloesin (>99% purity) and 34 mg of aloeresin A (>98% purity) were recovered from 2.5 g of aloe juice. The HPLC method was validated, and intra- and interday performances were established. In-house validation was carried out by analyzing samples of beverages with and without aloe as a flavoring agent. 相似文献
7.
We investigated an improved method for the separation of high-purified lutein from a commercially available spray-dried Chlorella powder (CP) using fine grinding by jet mill and flash column chromatography on a silica gel. Saponification and extraction of lutein were enhanced 2.3-2.9-fold in jet mill-treated CP (mean particle size, 20 microm) as compared to untreated CP (mean particle size, 67 microm). The carotenoid extract was dissolved in ether-hexane (1:1 v/v) and subjected to flash column chromatography on silica gel. A mixture of alpha- and beta-carotene was eluted with hexane, followed by elution with hexane-acetone-chloroform (7:2:1 v/v). Lutein (dark-orange band) was collected after the elution of an unknown colorless compound (detected based on UV absorbance). The purity of lutein in this fraction was over 99%, and the yield was 60%. The present study provides key information for obtaining highly purified lutein using flash column chromatography on a silica gel. 相似文献
8.
Preparative HPLC method for the purification of sulforaphane and sulforaphane nitrile from Brassica oleracea 总被引：1，自引：0，他引：1
Matusheski NV Wallig MA Juvik JA Klein BP Kushad MM Jeffery EH 《Journal of agricultural and food chemistry》2001,49(4):1867-1872
An extraction and preparative HPLC method has been devised to simultaneously purify sulforaphane and sulforaphane nitrile from the seed of Brassica oleracea var. italica cv. Brigadier. The seed was defatted with hexane, dried, and hydrolyzed in deionized water (1:9) for 8 h. The hydrolyzed seed meal was salted and extracted with methylene chloride. The dried residue was redissolved in a 5% acetonitrile solution and washed with excess hexane to remove nonpolar contaminants. The aqueous phase was filtered through a 0.22-microm cellulose filter and separated by HPLC using a Waters Prep Nova-Pak HR C-18 reverse-phase column. Refractive index was used to detect sulforaphane nitrile, and absorbance at 254 nm was used to detect sulforaphane. Peak identification was confirmed using gas chromatography and electron-impact mass spectrometry. Each kilogram of extracted seed yielded approximately 4.8 g of sulforaphane and 3.8 g of sulforaphane nitrile. Standard curves were developed using the purified compounds to allow quantification of sulforaphane and sulforaphane nitrile in broccoli tissue using a rapid GC method. The methodology was used to compare sulforaphane and sulforaphane nitrile content of autolyzed samples of several broccoli varieties. 相似文献
9.
基于颜色特征的玉米种子纯度识别 总被引：5，自引：1，他引：4
为准确快速的识别出玉米种子中的杂粒,提高玉米种的纯度,该文提出一种以玉米种子冠部与侧面颜色作为特征向量进行纯度识别的新方法。该方法首先将玉米种子原始图像进行背景分割、单粒提取,然后进行冠部核心区域及侧面RGB、HSV颜色特征向量的提取,最后采用Fisher判别理论将多维特征向量投影到一维空间中,进行K-均值聚类分析。试验结果证明：利用Fisher判别理论在一维空间上进行K-均值聚类分析,玉米种子纯度的识别率高于93.75%。影响玉米种子正确识别率的主要因素是投影方向的选择及正确的冠部核心区域的提取。 相似文献
10.
11.
基于分裂Bregman算法的玉米种子品种识别 总被引：3，自引：1，他引：2
摘要：玉米品种的纯度和玉米产量密切相关,因此玉米品种的筛选对提高粮食产量具有非常重要的作用。基于机器视觉的自动品种筛选技术通常分为图像分割、特征获取和分类等三步。图像分割的精度直接决定了种子识别准确度。在众多的图像分割技术中,本研究尝试将图像分割变分模型及其对应的数值求解方法-分裂Bregman算法应用于玉米种子自动识别中。该方法具有精度高,分割边界封闭连续等有利于玉米特征提取的优点。此外,本文还将自适应小波配置法用于求解分裂Bregman算法中的最优条件,得到一种更为精确高效的分裂Bregman算法。进而结合改进分裂Bregman算法得到的不同玉米品种特征和支持向量机技术得到了一种新的玉米品种分类器。采用该方法对玉米品种农大108和鲁丹981进行实验,识别精度分别达到97.3%和98%,相对于由其他分割方法得到的分类结果精度（95%）要高。 相似文献
12.
Wells RJ Hook JM Al-Deen TS Hibbert DB 《Journal of agricultural and food chemistry》2002,50(12):3366-3374
Comparison of quantitative NMR spectroscopy (QNMR) with chromatographic methods such as gas chromatography (GC) or high-pressure liquid chromatography (HPLC) for the determination of the purity of and impurities in technical grade agrochemicals, 2,4-dichlorophenoxyacetic acid (2,4-D), 1, and Dalapon sodium (sodium 2,2-dichloropropionate), 10, has revealed that QNMR is more precise and accurate than the chromatographic methods. Quantitative impurity profiling of technical grade 1 is rapid and accurate using 600 MHz (1)H NMR. Extra dispersion at the relatively high frequency allowed full assignment of the NMR spectrum of 1 and its related organic impurities in technical samples. The percentage purity of 1 was measured by the difference QNMR method, which involves summing the amounts of impurities and subtracting from 100%. Results are superior in consistency to those obtained by chromatographic methods. The percentage purity of Dalapon sodium, 10, in technical grade batches is readily obtained by (1)H QNMR, using either the difference method or the internal standard method, using dimethyl sulfone (DMSO2) internally as a reference material, that is chemically unrelated to the analyte. The latter method also allows the simultaneous identification and quantification of impurities, many of which are either not accessible to or detectable by the chromatographic methods. Uncertainty budgets for the QNMR method are presented and demonstrate that the major contributors to uncertainty lie in the weighing of the chemicals and in purity of the standard reference material prior to the QNMR experiment. 相似文献
13.
Bernardi R Finiguerra MG Rossi AA Palmieri S 《Journal of agricultural and food chemistry》2003,51(9):2737-2744
On the basis of previous studies on the mechanism-based inhibition, activation, and active site structure of myrosinase(s) isolated from Sinapis alba and other cruciferous seeds, crambe myrosinase shows uncommon properties and behavior. For this reason homogeneous crambe myrosinase was isolated and investigated to establish the most important physicochemical features, including kinetic properties determined with the epimers progoitrin (R) and epi-progoitrin (S) as substrates, with and without ascorbate as an activator. The results of this study demonstrate that crambe myrosinase is highly specific for epi-progoitrin due to a better stabilization of the enzyme-substrate complex. This stabilization is caused by additional hydrogen bonding that only epi-progoitrin can set up between its hydroxyl group and a suitable residue in the hydrophobic pocket where the "docking" of the glucosinolates side chain takes place. 相似文献
14.
Cold pressed, nonraffinated evening primrose oil (EPO) was recently found to contain lipophilic triterpenoidal esters with radical scavenging and anti-inflammatory properties. A simple and robust method for the quantitative analysis of these 3-O-trans-caffeoyl derivatives of betulinic, morolic, and oleanolic acid was developed and validated. Separation was achieved by normal phase chromatography on a Diol column and with hexane/ethyl acetate (50:50) as eluent. The analytes could be determined directly in the oil matrix, without need of a previous removal of the triglycerides. Normal phase LC ESI-MS with a makeup flow of polar modifier was used for checking the identity and purity of analyte peaks. Samples from 22 commercially available EPOs were analyzed. The average caffeoyl ester contents were 58 mg/100 g in cold pressed oils and 4.7 mg/100 g in partially raffinated oils. In fully raffinated EPO samples, the concentration was below the limit of detection. The influence of extraction temperature on the content of caffeoyl esters in nonraffinated EPO was investigated with seeds of Oenothera biennis and Oenothera lamarckiana, respectively. With O. lamarckiana, the concentration of caffeoyl esters in the oil increased with rising pressure and temperature, whereas no such dependency was found with O. biennis. Microscopic analysis revealed some differences in the histology of the seed testa, which may explain in part the differing behaviors in the extraction experiments. There was a difference between O. biennis and O. lamarckiana oils with respect to the relative amounts of the three esters. The temperature of the extraction process had no effect on the ratio of the compounds. 相似文献
15.
HPLC method for the quantification of procyanidins in cocoa and chocolate samples and correlation to total antioxidant capacity. 总被引：5，自引：0，他引：5
G E Adamson S A Lazarus A E Mitchell R L Prior G Cao P H Jacobs B G Kremers J F Hammerstone R B Rucker K A Ritter H H Schmitz 《Journal of agricultural and food chemistry》1999,47(10):4184-4188
Monomeric and oligomeric procyanidins present in cocoa liquors and chocolates were separated and quantified in four different laboratories using a normal-phase high-performance liquid chromatography (HPLC) method with fluorescence detection. Procyanidin standards through decamers were obtained by extraction from cocoa beans, enrichment by Sephadex LH-20 gel permeation chromatography, and final purification by preparative normal-phase HPLC. The purity of each oligomeric fraction was assessed using HPLC coupled to mass spectrometry. A composite standard was then prepared, and calibration curves were generated for each oligomeric class using a quadratic fit of area sum versus concentration. Results obtained by each of the laboratories were in close agreement, which suggests this method is reliable and reproducible for quantification of procyanidins. Furthermore, the procyanidin content of the samples was correlated to the antioxidant capacity measured using the ORAC assay as an indicator for potential biological activity. 相似文献
16.
A rapid confirmatory method for monitoring chloramphenicol (CAP) residues in honey, whole milk, and eggs is presented. This method is based on the polymer monolith microextraction (PMME) technique and high-performance liquid chromatography (HPLC)-electrospray ionization mass spectrometry (MS). A poly(methacrylic acid-ethylene glycol dimethacrylate) monolithic capillary column was selected as the extraction medium. To obtain optimum extraction efficiency, several parameters related to PMME were investigated. After dissolution in 20 mM phosphate solution at pH 4.0 and centrifugation, honey, eggs, or milk samples were directly passed through the extraction tube. The LC-MS instrument was equipped with an electrospray ion source and a single quadrupole. The eluates were analyzed by LC-MS in the negative-ion mode and by monitoring a pair of isotopic ions for the target compound. The in-source collision-induced dissociation process produced confirmatory ions. The recoveries of CAP from real samples spiked at 0.1-10 ng/g (honey), 0.2-10 ng/mL (milk), and 0.2-10 ng/g (egg) were in the range of 85-102%, with relative standard deviations ranging between 2.1% and 8.9%. The limits of detection (S/N = 3) were 0.02 ng/g, 0.04 ng/mL, and 0.04 ng/g in honey, milk, and eggs, respectively. The proposed method was proved to be robust in monitoring CAP residue in honey, milk, and eggs. 相似文献
17.
Organochlorine pesticide residues in strawberries from integrated pest management and organic farming 总被引：1，自引：0，他引：1
Fernandes VC Domingues VF Mateus N Delerue-Matos C 《Journal of agricultural and food chemistry》2011,59(14):7582-7591
A rapid, specific, and sensitive method based on the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) method and a cleanup using dispersive solid-phase extraction with MgSO(4), PSA, and C18 sorbents has been developed for the routine analysis of 14 pesticides in strawberries. The analyses were performed by three different analytical methodologies: gas chromatography (GC) with electron capture detection (ECD), mass spectrometry (MS), and tandem mass spectrometry (MS/MS). The recoveries for all the pesticides studied were from 46 to 128%, with relative standard deviation of <15% in the concentration range of 0.005-0.250 mg/kg. The limit of detection (LOD) for all compounds met maximum residue limits (MRL) accepted in Portugal for organochlorine pesticides (OCP). A survey study of strawberries produced in Portugal in the years 2009-2010 obtained from organic farming (OF) and integrated pest management (IPM) was developed. Lindane and β-endosulfan were detected above the MRL in OF and IPM. Other OCP (aldrin, o,p'-DDT and their metabolites, and methoxychlor) were found below the MRL. The OCP residues detected decreased from 2009 to 2010. The QuEChERS method was successfully applied to the analysis of strawberry samples. 相似文献
18.
MM Araújo E Marchioni AL Villavicencio M Zhao P Zimmermann E El-Khoury M Bergaentzle 《Journal of agricultural and food chemistry》2012,60(31):7629-7633
A pressurized liquid extraction (PLE) method using phosphate buffer as solvent was applied for folic acid (FA) extraction from fortified wheat flours and was compared to a standard solid-liquid extraction (SLE) method. Extracted FA was quantified by reverse phase high-performance liquid chromatography (RP-HPLC) hyphenated with a phenyl column and an absorption photometric detector (λ = 280 nm). Detection and quantification limits were 0.12 and 0.4 ng, respectively, corresponding to 0.06 and 0.2 μg g(-1) of analyzed wheat flour. Equivalent FA contents were found by both extraction methods, but a single PLE allowed a total recovery of FA content, whereas at least three successive SLEs were needed to achieve a total recovery of FA. The obtained results indicated that PLE is a rapid and efficient technique for FA extraction from fortified wheat flour. 相似文献
19.
Huang SC Yen GC Chang LW Yen WJ Duh PD 《Journal of agricultural and food chemistry》2003,51(8):2380-2383
The antioxidant activity and identification of the antioxidant component of peanut seed testa were investigated. The antioxidant activity of peanut seed testa was studied in the linoleic acid model system by using the ferric thiocyanate method. Among the five organic solvent extracts, the ethanolic extracts of peanut seed testa (EEPST) produced higher yields and stronger antioxidant activity than other organic solvent extracts. EEPST was separated into 17 fractions on silica gel column chromatography. Fraction 17, which showed the largest yield and significant antioxidant activity, was separated by thin-layer chromatography. Four major antioxidative subfractions were present. Subfraction 17-2 was found to be effective in preventing oxidation of linoleic acid. This subfraction was further fractionated and isolated and characterized by UV, MS, IR, and (1)H NMR techniques. The active compound was identified as ethyl protocatechuate (3,4-dihydroxybenzoic acid ethyl ester). 相似文献
20.
A modified version of the Haug and Lantzsch method for rapid photometrical phytate determination was applied for the analysis of phytate in soybean, wheat, and maize meals. In comparison to the original protocol, the amount of the toxic reagent thioglycolic acid is reduced substantially to minimize potential health risks for laboratory personnel. Different extraction conditions for soybean meal were tested, and boiling for at least 30 min was found to be necessary to remove an interfering compound in soybean meal extracts. Phytate contents determined according to the modified Haug and Lantzsch method did not differ from those obtained by measuring total precipitated phosphorus or by sensitive and specific high-performance ion chromatography. Applicability and accuracy of the modified method for phytate analysis in major feed substrates, including soy-based textured vegetable protein, were demonstrated. 相似文献