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A Study of the Elemental Profiles of Wines from the North-Eastern Coast of the Black Sea 黑海东北海岸葡萄酒元素特征研究
Pub Date : 2024-05-11 DOI: 10.3390/separations11050148
L. Oganesyants, Alexandr L. Panasyuk, D. Sviridov, O. S. Egorova, D. R. Akbulatova, M. Ganin, Aleksey A. Shilkin, Alexandr A. Il’in
Due to the increasing consumer interest in wines with a controlled place of origin, PGI (Protected Geographical Indication) and PDO (Protected Designation of Origin), the most acute question is how to identify them. One of the most effective ways to confirm the place of origin of wine in global practice is a comprehensive study of the elemental profile using statistical analysis methods. In the period from 2020 to 2023, 152 grape samples of grapes were collected from various wineries in Crimea and Kuban. The grape must that was obtained from them was fermented in laboratory conditions. The elemental profile was determined in the prepared wines, which included 71 indicators. In the conducted work, it was revealed that wines from Crimea and Kuban differ statistically significantly in the concentration of the elements B, Ca, Cu, Mn, Na, Ni, Re, Si, Sn and U. At the same time, the contents of the elements U, Sn and Re prevail in wines from Crimea, and those of B, Ca, Cu, Mn, Na, Ni and Si prevail in wines from Kuban. At the same time, methods of univariate and multivariate statistics do not allow us to reliably classify wine samples from Crimea and Kuban by their place of origin. In order to reveal the non-linear dependence of the studied indicators in wines on the geographical place of grape growing, the method of a supervised learning Random Forest was used. After training the model on the dataset, the proportion of its correct predictions was 96%. The model used 61 parameters, among which the most important were Ni, Re, Ba, Rb, Na, U, Sb, Zn, Bi, Ag and Ti.
由于消费者对具有受控原产地、PGI(受保护的地理标志)和 PDO(受保护的原产地名称)的葡萄酒越来越感兴趣,最尖锐的问题是如何识别它们。在全球实践中,确认葡萄酒原产地的最有效方法之一是利用统计分析方法对元素特征进行综合研究。在 2020 年至 2023 年期间,从克里米亚和库班的不同酒厂收集了 152 份葡萄样本。从中获得的葡萄汁在实验室条件下进行了发酵。对酿制的葡萄酒进行了元素分析,其中包括 71 项指标。研究结果表明,克里米亚和库班的葡萄酒在 B、Ca、Cu、Mn、Na、Ni、Re、Si、Sn 和 U 元素的含量上存在显著的统计学差异。同时,单变量和多变量统计方法并不能可靠地将克里米亚和库班的葡萄酒样品按产地进行分类。为了揭示所研究的葡萄酒指标与葡萄种植地理位置的非线性关系,我们使用了随机森林监督学习方法。在数据集上训练该模型后,其预测正确率为 96%。该模型使用了 61 个参数,其中最重要的是 Ni、Re、Ba、Rb、Na、U、Sb、Zn、Bi、Ag 和 Ti。
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引用次数: 0
Optimizing Operational Parameters for Lithium Hydroxide Production via Bipolar Membrane Electrodialysis 优化双极膜电渗析氢氧化锂生产的操作参数
Pub Date : 2024-05-09 DOI: 10.3390/separations11050146
Guoxiang Wei, Mengmeng Wang, Chenxiao Lin, Chuan Xu, Jie Gao
Traditional lithium hydroxide production techniques, like lithium sulfate and lithium carbonate causticizing methods, suffer from drawbacks including high specific energy consumption, time-consuming processes, and low recovery rates. The conversion of lithium chloride to lithium hydroxide using bipolar membrane electrodialysis is straightforward; however, the influence of operational parameters on bipolar membrane electrodialysis performance have not been investigated. Herein, the impact of the current density (20 mA/cm2~80 mA/cm2), feed concentration (0.5 M~2.5 M), initial feed pH (2.5, 3.5 and 4.5), and the volume ratio of the feed and base solution (1:1, 2:1 and 3:1) on the current efficiency and specific energy consumption in the bipolar membrane electrodialysis was systematically investigated. The bipolar membrane electrodialysis process showed promising results under optimal conditions with a current density of 50 mA/cm2 and an initial lithium chloride concentration of 1.5 M. This process achieved a current efficiency of 75.86% with a specific energy consumption of 3.65 kwh/kg lithium hydroxide while also demonstrating a lithium hydroxide recovery rate exceeding 90% with a purity of about 95%. This work will provide valuable guidance for hands on implementation of bipolar membrane electrodialysis technology in the production of LiOH.
传统的氢氧化锂生产技术,如硫酸锂和碳酸锂苛化法,存在比能耗高、工艺耗时长、回收率低等缺点。利用双极膜电渗析法将氯化锂转化为氢氧化锂是一种简单易行的方法,但操作参数对双极膜电渗析性能的影响尚未得到研究。本文系统研究了电流密度(20 mA/cm2~80 mA/cm2)、料液浓度(0.5 M~2.5 M)、初始料液 pH 值(2.5、3.5 和 4.5)以及料液和碱液的体积比(1:1、2:1 和 3:1)对双极膜电渗析电流效率和比能耗的影响。在电流密度为 50 mA/cm2、初始氯化锂浓度为 1.5 M 的最佳条件下,双极膜电渗析工艺取得了良好的结果。该工艺的电流效率为 75.86%,比能耗为 3.65 kwh/kg,氢氧化锂回收率超过 90%,纯度约为 95%。这项工作将为双极膜电渗析技术在氢氧化锂生产中的实际应用提供宝贵的指导。
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引用次数: 0
Ultrasonic Pretreatment Combined with Microwave-Assisted Hydrodistillation for Extraction of Essential Oil from Melaleuca bracteata ‘Revolution Gold’ Leaves Scales Induced by Cellulase-Inorganic Salt and Its Anti-Fungal Activity 超声波预处理结合微波辅助水蒸馏法提取纤维素酶-无机盐诱导的 Melaleuca bracteata 'Revolution Gold' 叶片鳞片中的精油及其抗真菌活性
Pub Date : 2024-05-09 DOI: 10.3390/separations11050147
Yan Huang, Xiaonan Zhang, Fajian Zeng, Jinmei Chang, Zhiwei Liu
In order to further develop the commercial use of Melaleuca bracteata (F. Muell), this report studied the extraction of essential oil from Melaleuca bracteata (F. Muell) leaves using ultrasonic pretreatment, cellulase-inorganic salt soaked and combined with microwave-assisted hydrodistillation. To optimize the primary contributing parameters, the Box–Behnken design (BBD) was applied. The optimum yield of essential oil was 9.61 mL/kg DW at a microwave power of 510.77 W, lithium chloride dose of 63.56 μmol, and microwave irradiation period of 46.97 min. The essential oil included a total of 41 compounds, and methyl eugenol (76.53%) and methyl cinnamate (12.62%) were the main compounds. The inhibitory impact was notable when the essential oil concentration was 1.6 mg/mL. Therefore, it has the potential to replace chemical pesticides. When the concentration of the essential oil solution was 1.6 mg/mL, the three pathogenic species of fungus (Pseudocercospora psidii, Colletotrichum eriobotryae, and Colletotrichum siamense) were greatly affected; at this dose, the fungus was unable to develop and its growth diameter was 0 mm. Additionally, the fungus’s inhibition rate reached 100%.
为了进一步开发白千层(Melaleuca bracteata (F. Muell))的商业用途,本报告研究了采用超声波预处理、纤维素酶-无机盐浸泡并结合微波辅助水蒸馏法从白千层(Melaleuca bracteata (F. Muell))叶片中提取精油的方法。为了优化主要贡献参数,采用了箱-贝肯设计法(BBD)。在微波功率为 510.77 W、氯化锂剂量为 63.56 μmol、微波辐照时间为 46.97 分钟时,精油的最佳产量为 9.61 mL/kg DW。精油中共含有 41 种化合物,其中丁香酚甲酯(76.53%)和肉桂酸甲酯(12.62%)是主要化合物。当精油浓度为 1.6 毫克/毫升时,抑制作用明显。因此,它具有替代化学农药的潜力。当精油溶液的浓度为 1.6 毫克/毫升时,三种致病真菌(Pseudocercospora psidii、Colletotrichum eriobotryae 和 Colletotrichum siamense)受到很大影响;在此剂量下,真菌无法发育,其生长直径为 0 毫米。此外,真菌的抑制率达到 100%。
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引用次数: 0
Natural Deep Eutectic Solvent-Based Ultrasound-Assisted Extraction of Flavonoids from Fagopyrum tataricum Bran 基于天然深共晶溶剂的超声波辅助提取鞑靼糙米中的黄酮类化合物
Pub Date : 2024-05-08 DOI: 10.3390/separations11050145
Zhou Xu, Xiaomei Da, Jipeng Qu, Shiming Xiao
In this study, eleven kinds of flavonoids were identified from F. tataricum bran (FTB) by UPLC-Q-TOF-MS, and HPLC-DAD analysis revealed that four compounds, including rutin, quercetin, kaempferol, and nicotiflorin, were the most significant components. Subsequently, natural deep eutectic solvent-based ultrasound-assisted extraction (NADES-UAE) was employed to extract flavonoids from FTB. Among the six kinds of NADES prepared, choline chloride–ethylene glycol (ChCl-EG) was identified as a promising candidate for extracting flavonoids due to its superior extraction performance. The extraction conditions were statistically investigated using response surface methodology conducted by Box-Behnken design (BBD). The optimal operational conditions were as follows: ultrasonic time 268 s, ultrasonic temperature 76 °C, and liquid–solid ratio 43 mL/g, which resulted in a high total flavonoid yield of 40.29 mg/g. Afterwards, the efficient extraction mechanism of NADES-UAE was comprehensively explored through FT-IR spectra, COSMO model, and microstructural analysis. In conclusion, NADES-UAE extraction is considered a green, efficient, and sustainable method for FTB flavonoids.
本研究采用UPLC-Q-TOF-MS鉴定了鞑靼藜麦麸(FTB)中的11种黄酮类化合物,HPLC-DAD分析表明,芦丁、槲皮素、山柰酚和烟花色苷等4种化合物是最主要的成分。随后,采用基于天然深共晶溶剂的超声辅助萃取(NADES-UAE)技术从枸杞多糖中提取黄酮类化合物。在所制备的六种 NADES 中,氯化胆碱-乙二醇(ChCl-EG)因其优异的萃取性能被认为是萃取黄酮类化合物的理想候选溶剂。采用方框-贝肯设计(BBD)的响应面方法对萃取条件进行了统计研究。最佳操作条件为:超声时间 268 s,超声温度 76 °C,液固比 43 mL/g,总黄酮产量高达 40.29 mg/g。随后,通过傅立叶变换红外光谱、COSMO模型和微观结构分析,全面探讨了NADES-UAE的高效提取机理。总之,NADES-UAE 是一种绿色、高效、可持续的萃取枸橼酸黄酮类化合物的方法。
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引用次数: 0
Achievements in Preparation of Cyclodextrin–Based Porous Materials for Removal of Pollutants 环糊精基多孔材料在去除污染物方面的制备成果
Pub Date : 2024-05-07 DOI: 10.3390/separations11050143
Kaiyue Bao, Anyun Zhang, Yiyao Cao, Lei Xu
Cyclodextrin–based porous materials have been widely applied in removing various organic pollutants from water environments, due to their unique physical and chemical properties, like the size–matching effect and hydrophobic interaction. Large numbers of hydroxyl groups in its external structure give cyclodextrin a high solubility in water, but the existence of these hydroxyl groups also endows cyclodextrin with the ability to be chemically modified with various functional groups to reduce its solubility in water and, meanwhile, to develop some novel functionalized cyclodextrin–based porous materials for selective removal of the target organic pollutants. This review focuses on the recent development in the synthesis of cyclodextrin–based porous materials (crosslinked cyclodextrin polymers and immobilized cyclodextrins), as well as highlighting their applications and mechanisms in the removal of dyes, endocrine disruptors, and mixed pollutants from water. Finally, the challenges and future perspectives in related research fields are discussed.
环糊精基多孔材料因其独特的物理和化学特性,如尺寸匹配效应和疏水作用,已被广泛应用于去除水环境中的各种有机污染物。环糊精外部结构中的大量羟基赋予了其在水中的高溶解度,但这些羟基的存在也赋予了环糊精用各种官能团进行化学修饰的能力,以降低其在水中的溶解度,同时开发出一些新型的官能化环糊精基多孔材料,用于选择性地去除目标有机污染物。本综述重点介绍了环糊精基多孔材料(交联环糊精聚合物和固定化环糊精)合成的最新进展,并着重介绍了它们在去除水中的染料、内分泌干扰物和混合污染物方面的应用和机理。最后,还讨论了相关研究领域面临的挑战和未来展望。
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引用次数: 0
Degradation of Levofloxacin by Electroactivated Sodium Persulfate on Carbon Cloth Cathode Modified with Cerium-Based Metal Organic Frameworks (Ce-MOF) Derivatives 经铈基金属有机框架 (Ce-MOF) 衍生物改性的碳布阴极上的电活性过硫酸钠降解左氧氟沙星
Pub Date : 2024-05-07 DOI: 10.3390/separations11050144
Xinbiao Mao, Mingyu Ou, Wenjun Zhao, Shuangting Yu, Hao Xu
Levofloxacin (LFX), which is difficult to degrade effectively due to its molecular stability, has become an problem that needs to be solved urgently. The advanced oxidation technology of persulfate has received increasing attention from researchers. In this study, a Ce-MOF derivative (Ce-MOF-T) was prepared by hydrothermal synthesis and calcination, which synergistically responded to electroactivation to generate sulfate radicals for the efficient degradation of LFX. It has been proven that electrical activation and the Ce-MOF derivatives work together to generate sulfate radicals and effectively degrade LFX. Ce-MOF-550-modified carbon cloth was used as the cathode and a platinum electrode as the anode, the concentration of LFX was 20 mg·L−1, the loading of Ce-MOF-550 was 15 mg, pH = 5, the concentration of sodium persulfate (PMS) was 0.3 g·L−1, the current density was 100 A·m−2, and the degradation rate was 82.05% after 1 h of reaction and 95% after 3 h of reaction. After five cycle tests, the degradation rate was still higher than 75.00%, indicating that the material had good stability. In addition, the degradation of LFX was consistent with a quasi-primary kinetic reaction with apparent rate constants of 2.26 × 10−2 min−1.
左氧氟沙星(LFX)因其分子稳定性难以有效降解,已成为亟待解决的问题。过硫酸盐的高级氧化技术越来越受到研究人员的关注。本研究通过水热合成和煅烧制备了一种 Ce-MOF 衍生物(Ce-MOF-T),该衍生物与电活化协同反应生成硫酸根自由基,可高效降解 LFX。实验证明,电活化和 Ce-MOF 衍生物共同作用生成硫酸根自由基,有效降解 LFX。以 Ce-MOF-550 改性碳布为阴极,铂电极为阳极,LFX 的浓度为 20 mg-L-1,Ce-MOF-550 的负载量为 15 mg,pH = 5,过硫酸钠(PMS)的浓度为 0.3 g-L-1,电流密度为 100 A-m-2,反应 1 h 后降解率为 82.05%,反应 3 h 后降解率为 95%。经过五个循环测试后,降解率仍高于 75.00%,表明该材料具有良好的稳定性。此外,LFX 的降解符合准一级动力学反应,表观速率常数为 2.26 × 10-2 min-1。
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引用次数: 0
Efficient Separation of Re (VII) and Mo (VI) by Extraction Using E-1006–Ammonium Sulfate Aqueous Two-Phase System 使用 E-1006-Ammonium Sulfate 水性两相体系通过萃取高效分离 Re (VII) 和 Mo (VI)
Pub Date : 2024-05-07 DOI: 10.3390/separations11050142
Linlin Fan, Wenhui Li, Zilong Dai, Min Zhou, Yunren Qiu
Aqueous two-phase extraction (APTE) stands out as an environmentally friendly technique for the separation of metal ions. The separation of Re (VII) and Mo (VI) in an aqueous solution was investigated using a novel aqueous two-phase system (ATPS) consisting of isodecanol polyoxyethylene ether (E-1006), ammonium sulfate, and water. A phase diagram of this system was developed, and the effects of pH, temperature, extraction time, the concentrations of E-1006 and (NH4)2SO4, and metal ions on the separation of Re (VII) and Mo (VI) were examined. The results show that at pH 7.0, Mo (VI) had almost transformed into the (NH4)2SO4-rich phase, while Re (VI) was extracted into the E-1006-rich phase. The increase in temperature induces a transition of Mo (VI) to the salt-rich phase, which is unfavorable for the extraction of Re (VII). The increase in the concentrations of E-1006 and (NH4)2SO4 has a positive effect on the separation of rhenium and molybdenum. Overall, the ATPS consisting of 200 g/L of E-1006, 200 g/L of (NH4)2SO4, and water yields an extraction efficiency of 97.2% for Re and a high separation factor of 2700 for Re (VII) and Mo (VI) from a mixture of 0.1 g/L of Re (VII) and 5 g/L of Mo (VI) at pH 7.0 and 323.15 K. Separation studies of the simulated leaching solution show that the extraction efficiency for Re (VI) is 99.1% and the separation factor of Re (VII) and Mo (VI) is 5100.
水相两相萃取(APTE)是一种分离金属离子的环保型技术。研究人员使用由异癸醇聚氧乙烯醚(E-1006)、硫酸铵和水组成的新型水相两相体系(ATPS),对水溶液中 Re (VII) 和 Mo (VI) 的分离进行了研究。绘制了该体系的相图,并考察了 pH 值、温度、萃取时间、E-1006 和 (NH4)2SO4 的浓度以及金属离子对 Re (VII) 和 Mo (VI) 分离的影响。结果表明,在 pH 值为 7.0 时,Mo (VI) 几乎转化为富含 (NH4)2SO4 的相,而 Re (VI) 则被萃取到富含 E-1006 的相中。温度的升高导致 Mo (VI) 向富盐相转变,不利于萃取 Re (VII)。增加 E-1006 和 (NH4)2SO4 的浓度对铼和钼的分离有积极作用。总之,由 200 克/升 E-1006、200 克/升 (NH4)2SO4 和水组成的 ATPS 对 Re 的萃取效率高达 97.2%,对 Re (VII) 和 Mo (VI) 的萃取效率高达 2700,从 0.模拟浸出液的分离研究表明,Re (VI) 的萃取效率为 99.1%,Re (VII) 和 Mo (VI) 的分离系数为 5100。
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引用次数: 0
Decoding the Volatile Profile of White Romanian Fetească Wines 解密罗马尼亚费塔斯卡白葡萄酒的挥发性特征
Pub Date : 2024-05-03 DOI: 10.3390/separations11050141
Fulvia-Ancuța Manolache, D. Duță, Gabriela Daniela Criveanu-Stamatie, T. Iordache, Maria-Cristina Todașcă
The wine’s volatilome, most of the time, defines not only its aroma, but also, its major attributes. In the case of wines, the authentication process has become imperative, in light of increased production of alcoholic beverages; consequently, reliable analytical methods have served for it. Therefore, the goal of this research was to establish the global volatile profile of traditional Romanian white wines from Fetească varieties (Fetească albă, Fetească regală) in order to identify its unique characteristics by means of a headspace solid-phase microextraction coupled with gas chromatography analysis (HS-SPME/GC-MS) and e-Nose devoted techniques. Statistics was also employed aimed at differentiating the analyzed wine by varietal groups. Consequently, 23 volatile compounds were detected and quantified in 39 Fetească white wine samples originating from various production areas (Muntenia, Oltenia, Transylvania, Banat and Dobrogea), then further classified according to their odor thresholds in five aromatic classes (floral, fruity, sweet, lactic (cheesy) and other). In addition, statistics (Principal Component Analysis (PCA), Hieratical Clustering Analysis (HCA)) were used aiming to differentiate the analyzed varietal groups. The outcomes have pointed out the existence of distinct clusters connected with ethyl esters or alcohol composition and production year, depending on each examined variety.
在大多数情况下,葡萄酒的挥发性不仅决定了它的香气,还决定了它的主要属性。就葡萄酒而言,随着酒精饮料产量的增加,鉴定过程已变得势在必行;因此,可靠的分析方法已为其服务。因此,本研究的目标是通过顶空固相微萃取-气相色谱分析(HS-SPME/GC-MS)和电子鼻专用技术,建立罗马尼亚传统白葡萄酒(白费特卡、雷加尔费特卡)的全球挥发性概况,以确定其独特特征。此外,还采用了统计学方法,以区分所分析葡萄酒的品种群。因此,在来自不同产区(蒙泰尼亚、奥尔特尼亚、特兰西瓦尼亚、巴纳特和多布罗盖亚)的 39 个费特斯卡白葡萄酒样品中检测并量化了 23 种挥发性化合物,然后根据其气味阈值进一步划分为五个芳香类别(花香、果香、甜味、乳酸味(芝士味)和其他)。此外,还使用了统计方法(主成分分析法(PCA)、层聚类分析法(HCA))来区分所分析的品种群。研究结果表明,根据所研究的品种,存在着与乙酯或酒精成分和生产年份相关的不同群组。
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引用次数: 0
Development and Validation of an LC-MS/MS Method for the Determination of Plasma and Red Blood Cell Omega Fatty Acids: A Useful Diagnostic Tool 开发并验证用于测定血浆和红细胞欧米茄脂肪酸的 LC-MS/MS 方法:一种有用的诊断工具
Pub Date : 2024-05-01 DOI: 10.3390/separations11050140
L. Farczádi, M. Dobreanu, A. Huțanu, Silvia Imre
Background: LC-MS is an ever-increasingly used methodology for clinical applications. Due to the superior selectivity and sensitivity, in certain situations, it can offer an advantage or be the only option for diagnostics and biomonitoring applications. Methods: A high selectivity sensitive LC-MS/MS method was developed for direct quantification of free plasma polyunsaturated fatty acids as well as conjugated membrane polyunsaturated fatty acids, using isocratic reverse phase elution. A quick and simple sample purification method was used in order to ensure high-throughput analysis of biological samples. The method was validated with regard to selectivity, sensitivity, linearity, accuracy, precision, carryover, and recovery, as well as other relevant parameters. Results and Conclusions: The method was developed and validated with respect to all relevant parameters and was successfully used in a number of clinical diagnostics and biomonitoring applications. The simple sample purification process allowed for an easy learning curve for analysts and other users, while ensuring a low chance of systematic or random errors and thus reliable results usable in a clinical setting.
背景:在临床应用中,LC-MS 是一种越来越常用的方法。由于其卓越的选择性和灵敏度,在某些情况下,它可以为诊断和生物监测应用提供优势或成为唯一的选择。方法:采用等度反相洗脱法,开发了一种高选择性、高灵敏度的 LC-MS/MS 方法,用于直接定量检测血浆游离多不饱和脂肪酸以及共轭膜多不饱和脂肪酸。为了确保生物样品的高通量分析,该方法采用了一种快速简便的样品纯化方法。对该方法的选择性、灵敏度、线性、准确度、精密度、携带率、回收率以及其他相关参数进行了验证。结果与结论:该方法的开发和验证涉及所有相关参数,并成功应用于多项临床诊断和生物监测。样品纯化过程简单,便于分析人员和其他用户学习,同时确保系统误差或随机误差的发生率较低,从而确保在临床环境中得到可靠的结果。
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引用次数: 0
Fertilizers’ Impact on Grassland in Northeastern Romania 化肥对罗马尼亚东北部草地的影响
Pub Date : 2024-05-01 DOI: 10.3390/separations11050139
O. Culicov, D. Tarcău, I. Zinicovscaia, O. Duliu, M. Stavarache, V. Vintu
In order to obtain more data concerning the influence of fertilizers (organic and mineral) on different forage plants in the northeastern Romanian grassland, the mass fractions of 14 essential, enzymatic, or toxic elements were determined by instrumental neutron activation analysis together with the amount of crude proteins, ash, fibers, as well as fat ether extract. The final results showed a significant variance in the content of analyzed elements on organic as well as on mineral fertilized experimental plots. At the same time, increased content of crude protein and fat ether extract was evident in fertilized grasses for all applied fertilizers, while other global indicators such as neutral and acid fibers of sulfuric lignin content decreased, suggesting significantly higher nutritional values for fertilized forage plants.
为了获得更多有关肥料(有机肥和矿物质肥)对罗马尼亚东北部草地上不同牧草植物影响的数据,通过仪器中子活化分析测定了 14 种必需元素、酶元素或有毒元素的质量分数,以及粗蛋白、灰分、纤维和脂醚提取物的含量。最终结果表明,有机肥和矿物质肥试验田的分析元素含量差异很大。同时,在施用所有肥料的情况下,受精牧草的粗蛋白和脂醚提取物含量明显增加,而其他综合指标,如硫化木质素的中性和酸性纤维含量则有所下降,这表明受精牧草的营养价值显著提高。
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引用次数: 0
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Separations
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