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1.
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
2.
Ruiz-Matute AI Sanz ML Corzo N Martín-Alvarez PJ Ibañez E Martínez-Castro I Olano A 《Journal of agricultural and food chemistry》2007,55(9):3346-3350
The viability of the purification of lactulose from a mixture with lactose [70:30 (w/w)] using pressurized liquid extraction (PLE) at 1500 psi for 30 min was studied. Different temperatures (from 40 to 130 degrees C) and proportions of ethanol:water (70:30, 80:20, 90:10, 95:5, and 100:0) as the extraction solvent were assayed. Lactose and lactulose were measured by gas chromatographic analysis as their trimethylsilyl derivatives. Data were fitted through multiple linear regressions to different quadratic models to describe both the extraction yield (in terms of mg of lactulose) and the purity of the lactulose extracted. The optimum extraction conditions provided by the model were as follows: extraction temperature, 40 degrees C; and solvent composition, 70:30 ethanol:water. PLE extraction under the optimized conditions was also applied to purify lactulose from lactose in a synthesis mixture. To our knowledge, this is the first time that PLE has been tested for extraction and purification of lactulose from its mixture with lactose; this technique showed several advantages over classical methods such as the short extraction time and the low solvent consumption. 相似文献
3.
4.
Fernández-Bolaños J Rodríguez G Rodríguez R Heredia A Guillén R Jiménez A 《Journal of agricultural and food chemistry》2002,50(23):6804-6811
The effect of hydrothermal treatment of two-phase olive waste (alperujo) on the solubilization of hydroxytyrosol was studied. Different conditions of saturated steam were assayed. A high amount of hydroxytyrosol was solubilized and increased with increasing steaming temperature and time, reaching 1.4-1.7 g/100 g of dry alperujo. The effect of acidic (H(2)SO(4)) and basic (NaOH) catalysts was also evaluated. Acid-catalyzed treatment was more effective at milder conditions, whereas the alkali-catalyzed conditions were not very suitable. In the present study, the extracted hydroxytyrosol was purified by means of a new, simple, and inexpensive chromatographic system, under international patent application (PCT/ES02/00058). From 1000 kg of alperujo, with 70% humidity, can be obtained approximately 4.5-5 kg of hydroxytyrosol. After a purification process, at least 3 kg of hydroxytyrosol, at 90-95% purity, would be obtained. The purified compound was identified by HPLC/UV and (1)H and (13)C NMR analyses, and its antioxidant activity was tested on refined olive oil without antioxidants by Rancimat method. The oxidative stability of refined olive oil was increased by a factor of 1.71 in the presence of 100 ppm of hydroxytyrosol. 相似文献
5.
Zhang H Chen T Jiang J Wong YS Yang F Zheng W 《Journal of agricultural and food chemistry》2011,59(16):8683-8690
Both selenium and allophycocyanin (APC) have been reported to show novel antioxidant activities. In this study, a fast protein liquid chromatographic method for purification of selenium-containing allophycocyanin (Se-APC) from selenium-enriched Spirulina platensis and the protective effect of Se-APC on 2,2'-azobis(2-amidinopropane) dihydrochloride (AAPH)-induced oxidative stress have been described. After fractionation by ammonium sulfate precipitation, and separation by DEAE-Sepharose ion-exchange and Sephacryl S-300 size exclusion chromatography, Se-APC with purity ratio (A652/A280) of 5.30 and Se concentration of 343.02 μg g(-1) protein was obtained. Se-APC exhibited stronger antioxidant activity than APC by scavenging ABTS (2,2'-azinobis-3-ethylbenzothiazolin-6-sulfonic acid) and AAPH free radicals. The oxidative hemolysis and morphological changes induced by AAPH in human erythrocytes were effectively reversed by coincubation with Se-APC. Lipid oxidation induced by the pro-oxidant agent cupric chloride in human plasma, as evaluated by formation of conjugated diene, was blocked by Se-APC. The accumulation of malondialdehyde, loss of reduced glutathione, and increase in enzyme activities of glutathione peroxidase and reductase induced by AAPH in human erythrocytes were effectively suppressed by Se-APC. Furthermore, Se-APC significantly prevented AAPH-induced intracellular reactive oxygen species (ROS) generation. Taken together, our results suggest that Se-APC demonstrates application potential in treatment of diseases in which excess production of ROS acts as a casual or contributory factor. 相似文献
6.
盐酸提取的土壤无机磷酸盐中氧同位素分析 总被引：1，自引：0，他引：1
7.
Human caseinomacropeptide (hCMP) is 65 amino acids in length and was originally derived from the C terminus of human milk kappa-casein. As it is highly abundant in both essential amino acids and branched amino acids, it could be developed as a practical food and even as medicinal nutrition for patients. This study was undertaken to prepare recombinant hCMP without glycosylation using recombinant plasmid and prokaryotic expression system. The gene encoding hCMP was chemically synthesized and directly inserted into the pET28a(+) vector and then expressed in Escherichia coli BL21(DE3). The maximum amount of soluble protein was obtained by incubation with 0.5 mM isopropyl-alpha-D-thiogalactopyranoside at 30 degrees C for 4 h and accounted for 40% of the total intracellular protein. Most of the expressed fusion proteins, located in the cell periplasm and cytoplasm, could be adsorbed by nickel affinity chromatography and eluted with buffer containing 300 mM imidazole. The fusion proteins were cleaved by enterokinase to remove the 6-His tag. Gel filtration chromatography with Sephadex G-10 was performed for desalting and purification. A final yield of 25 mg of the mature protein with high purity up to 99% was obtained from 1 L of E. coli culture. The purified protein was confirmed by MALDI-TOF-MS analysis. This study overcame the problem of glycosylation in hCMP and established a novel approach for the preparation of unglycosylated hCMP. 相似文献
8.
D L Mount J W Miles F C Churchill 《Journal of the Association of Official Analytical Chemists》1986,69(4):624-629
A liquid chromatographic (LC) method is described for evaluating purity of pentamidine isethionate (PI), a life-saving drug used in the treatment of Pneumocystis carinii pneumonia, which is a leading cause of death in persons with acquired immunodeficiency syndrome (AIDS). Six potential impurity compounds were synthesized to test the selectivity of the chromatographic system and to permit quantitation of impurities in various lots of PI products. The drug and impurities were separated with gradient elution on a cyano-bonded LC column. The analytic system provided information on the identities and levels of impurities in early experimental lots of PI. These results assisted the manufacturer in altering reaction conditions and purification procedures to ensure that succeeding lots were within the specification limits, i.e., no more than 0.4% of any single impurity or 0.7% of total impurities found in the final product. 相似文献
9.
Anisuzzaman AK Amin M Ogg N Hoq F Kanithi MR Jenkins RE 《Journal of agricultural and food chemistry》2000,48(12):5893-5902
The dimethyl derivatives of imazaquin, imazapyr, imazmethapyr, imazethapyr, 2-[4,5 dihydro-1, 4-dimethyl-4-(1-methylethyl)-5-oxo-1H-imidazol-2-yl]-5-methoxymethyl- 3-pyridine carboxylic acid, 2-[4,5-dihydro-1,4 -dimethyl-4-(1-methylethyl)-5-oxo-1H-imidazol-2-yl]-4-methyl benzoic acid, and 2-[4,5-dihydro-1,4-dimethyl-4-(1-methyl ethyl)-5-oxo-1H-imidazol-2-yl]-5-methyl benzoic acid were prepared and fully characterized. The availability of these derivatives has led to the development of efficient and multiresidue gas chromatographic methods for trace level analysis of imidazolinone herbicides in matrixes such as water, soybean, and soil. 相似文献
10.
Condo AM Baker DC Moreau RA Hicks KB 《Journal of agricultural and food chemistry》2001,49(10):4961-4964
Phytosterols and phytostanols are known to lower low-density lipoprotein-cholesterol (LDL-C) levels in humans by up to 15%, and at least two products, Benecol and Take Control, are now on the market as naturally derived fatty acid esters of phytostanols (stanol esters) and phytosterols (sterol esters), respectively. A synthetic process was developed to synthesize gram quantities of trans-feruloyl-beta-sitostanol from ferulic acid and beta-sitostanol, with high purity and yields of approximately 60%. The process involves (a) condensation of trans-4-O-acetylferulic acid with the appropriate phytostanol or phytostanol mixture in the presence of N,N-dicyclohexylcarbodiimide and 4-(dimethylamino)pyridine, (b) separation of the trans-4-O-acetylferuloyl products by preparative liquid chromatography, (c) selective deacetylation of the feruloyl acetate, and (d) chromatographic purification of the feruloylated phytostanols. The process was successfully applied to synthesize stanol trans-feruloyl esters from "Vegetable Stanols", a mixture of approximately 70:30 beta-sitostanol and beta-campestanol, in comparable purity and yield. 相似文献
11.
Hayat Ullah Sangam Shrestha Siraj Ud Din 《Archives of Agronomy and Soil Science》2017,63(9):1198-1209
In this study, we have attempted to investigate the effect of different water-saving cultivation techniques on root systems of two Thai rice varieties. The variables were two rice varieties (RD6 and RD10), two cultivation methods (dry direct seeding [DS] and transplanting [TP]) and two soil moisture regimes (field capacity [FC] and 50% FC). RD6 variety had higher root number, root length and root length density compared with RD10 under TP method at FC. Higher root number was observed for TP than dry DS method under FC at flowering stage with 543 and 415 roots plant–1 for RD6 and 392 and 362 roots plant–1 for RD10 cultivated under TP and dry DS methods, respectively. Root dry matter (DM) was the highest for RD6 cultivated through dry DS method compared with TP method at FC for both tillering and flowering stages. RD6 variety resulted in 25% and 50% higher root DM at FC for dry DS than TP at tillering and flowering stages, respectively. The performance of RD10 was poor under 50% FC and dry DS method. With proper selection of variety, dry DS method could be a better alternative for sustainable rice cultivation under water-limited environments. 相似文献
12.
Extraction of DNA from soil 总被引：1，自引：0，他引：1
Patrick Robe Renaud Nalin Carmela Capellano Timothy M. Vogel Pascal Simonet 《European Journal of Soil Biology》2003,39(4):183-190
There is an increased interest in the extraction of nucleic acids from various environmental samples, since molecular techniques allow less biased access to a greater portion of uncultivable microorganisms. Two strategies have been developed to improve DNA recovery in terms of yield, purity and unbiased representation of the microbial diversity. The first approach consists of the direct extraction of nucleic acids from soil through in situ cell lysis followed by DNA purification. The alternative approach is based on the separation of bacteria from the soil particles followed by cell lysis and then DNA purification. Several published methods describe the recovery of highly purified nucleic acids that are well-suited for molecular purposes even though a new challenge concerns the recovery of large bacterial DNAs essential for functional investigation of gene clusters and biosynthetic pathways. This review presents an overview of the available methods to achieve this challenging objective. 相似文献
13.
With the aid of multilayer coil countercurrent chromatography, subsequent acetylation, and liquid chromatographic purification of a glycosidic mixture obtained from lulo (Solanum quitoense L.) leaves, three C(13)-norisoprenoid glucoconjugates were isolated in pure form. Their structures were elucidated by NMR, MS, and CD analyses to be the novel (6R,9R)-13-hydroxy-3-oxo-alpha-ionol 9-O-beta-D-glucopyranoside (4a), the uncommon (3S,5R,8R)-3, 5-dihydroxy-6,7-megastigmadien-9-one 5-O-beta-D-glucopyranoside (citroside A) (5a), and the known (6S,9R)-vomifoliol 9-O-beta-D-glucopyranoside (6a). Enzymatic treatment of compound 5a showed the formation of 3-hydroxy-7,8-didehydro-beta-ionone (7), an important lulo peeling volatile, which in its turn after chemical reduction and heated acid catalyzed rearrangement generates beta-damascenone (9) and 3-hydroxy-beta-damascone (10). 相似文献
14.
The present paper describes a liquid chromatographic (LC) method for purification of crude swine tissue extracts before gas chromatographic/mass spectrometric (GC/MS) quantitation and confirmation of sulfamethazine at low ppb levels. Fractions corresponding to sulfamethazine were collected, evaporated to dryness, N-methylated with diazomethane, concentrated, and analyzed by GC/MS. A mass spectrometer was set to selected ion monitoring (SIM) mode. Ions 233, 227, 228, and 92 m/z were detected. Ratio 227/233 m/z (sulfamethazine/internal standard, [phenyl 13C6] sulfamethazine) was used for quantitation, while ratios 228/227 and 92/227 m/z, respectively, were used for confirmation. Quantitation in spiked blank muscle tissue was tested from 100 to 1 ppb and found acceptable at all concentrations studied; coefficients of variations ranged from 4.9 to 14.4%. Similar results were obtained for liver tissue from 5 to 20 ppb; coefficients of variation ranged from 1.2 to 9.1%. 相似文献
15.
传统的微生物分离培养方法,在反映茶园土壤微生物基因信息上有很大的局限性,因此,目前逐步被分子生态学的方法替代,而获得高质量、大片段、无偏好的土壤微生物总DNA则是茶园土壤微生物分子生态学研究的基础。本文采用SDS高盐法、变性剂加SDS高盐法、脱腐SDS高盐法、CTAB法和Krsek改进法5种土壤微生物DNA提取方法分别从茶园土壤微生物中提取总DNA,并对5种方法提取的DNA的片段大小、质量和产量进行了综合评价。结果表明,Krsek改进法提取到的DNA片段最大（〉23kb）、纯度最高（OD2UOD280〉1．70;OD2UOD230〉1．35）、产量较高（〉34．50μg／gdrysoil）且不需纯化就可以用于PCR扩增和RFLP分析。因此,Krsek改进法是一种高效、可靠且适合于茶园土壤微生物分子生态学研究的DNA提取方法。 相似文献
16.
A procedure for the isolation of pure sterigmatocystin is described. It involves cultivation of an appropriate fungus on sterile maize, and extraction and column chromatographic purification of the crude extract. With this method sterigmatocystin may be obtained at a fraction of its commercial cost. Aspergillus versicolor seemed to be the best producer (5-12 g/kg) in 250 ml Erlenmeyer flasks. The yield dropped markedly with increasing flask size. 相似文献
17.
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
18.
Golubovic M van Hateren SH Ottens M Witkamp GJ van der Wielen LA 《Journal of agricultural and food chemistry》2005,53(13):5265-5269
A novel method for the purification of glycinin from soy meal is presented. The method is based on the isoelectric precipitation of glycinin by using carbon dioxide as a volatile precipitant. Gaseous CO(2) was pressurized into the protein solution, thus lowering the pH and initiating glycinin precipitation. Pressurization and, consequently, acidification were done in a slow and controlled manner, with the end point of pH 6.4. The acidity of the protein solution was well controlled via the pressure of gaseous CO(2). In this way simultaneous precipitation of other soybean proteins was prevented and very pure glycinin was obtained. Approximately 40% of the glycinin present in the protein solution was recovered with purity as high as 98%. The purification process was successfully performed on both small and large scales, without affecting glycinin purity. 相似文献
19.
鸡胸软骨硫酸软骨素的提取及分离纯化 总被引：4，自引：0，他引：4
为优化硫酸软骨素的提取工艺和初步分析其结构,采用中心组合设计和响应面分析优化鸡胸软骨硫酸软骨素的酶法提取工艺,三氯乙酸除蛋白质、乙醇沉淀以及柱色谱精细纯化得到高纯度硫酸软骨素,并采用高效凝胶过滤色谱判定其纯度,红外光谱和核磁共振初步分析其结构。结果表明,硫酸软骨素的最佳提取工艺参数为温度55.68℃,pH值为6.40,时间为3.85 h,葡萄糖醛酸和硫酸软骨素提取率分别达到9.82%和28.05%。高效凝胶过滤色谱分析其纯度为99.01%。红外光谱和核磁共振显示硫酸软骨素主要是4硫酸化软骨素。 相似文献
20.
Piletska EV Burns R Terry LA Piletsky SA 《Journal of agricultural and food chemistry》2012,60(1):95-99
A molecularly imprinted polymer (MIP) for the purification of N(1),N(12)-bis(dihydrocaffeoyl)spermine (kukoamine A) was computationally designed and tested. The properties of the polymer were characterized. The protocol of the solid phase extraction (SPE) of kukoamine A from potato peels was optimized. A HPLC-MS method for the quantification of kukoamine A was developed and used for all optimization studies. The capacity of the MIP in relation to kukoamine A from the potato peels extract was estimated at 54 mg/g of the polymer. The kukoamine A purified from potato extract using MIP was exceptionally pure (≈ 90%). Although the corresponding blank polymer was less selective than the MIP for the extraction of kukoamine A from the potato extract, it was shown that the blank polymer could be effectively used for the purification of the crude synthetic kukoamine (polymer capacity = 80 mg of kukoamine A/g of the adsorbent, kukoamine A purity ≈ 86%). Therefore, selective adsorbents could be computationally designed for other plant products, allowing their purification in quantities that would be sufficient for more detailed studies and potential practical applications. 相似文献