微波辅助萃取ICP—MS法测定土壤中有效硼

建立了一种应用微波辅助萃取ICP-MS法测定土壤中有效硼的方法,该方法与NY/T148-1990和NY/T1121.8-2006(姜黄素比色法和甲亚胺比色法)相比,不仅操作简便快速、无污染,而且具有很好的准确度和精密度,其相对标准偏差(RSD)为3.5%,回收率为94.0%～107.3%,方法的检出限为1.13 ng·g-1.     

用塑料杯进行姜黄法测硼显色条件的研究

土壤全硼、有效硼和植物含硼量的测定,常用姜黄素比色法。有关文献介绍,于水浴中脱水显色时可用塑料杯代替蒸发皿。我们认为塑料杯与蒸发皿的口径及高度差别很大,一定会影响其蒸发速度,如果仍用15 min 的脱水显色时间,必然会使测定值偏低。本文仅就测定土壤有效硼进行试验,以探索其最佳脱水显色时间(这里指蒸干后,继续烘焙的时间。下同.),同时试验不同相对湿度对测定结果的影响。     

黄土区环境土壤中有效硼测定方法探讨

本采用和姜黄素比色法相同的浸提剂提取土壤有效硼，研究了用等离子体发射光谱测定土壤有效硼含量，该法简便，快速，准确，干扰小，所得结果与姜黄素比色法一致。     

甲亚胺-H分光光度法测硼的条件及应用

国内外有关甲亚胺-H分光光度法测硼的报道已有不少,但是不同资料对反应酸度、光密度的稳定时间说法不一;有关甲亚胺-H浓度、反应温度的影响讨论很少。     

植烟土壤有效硼、锌及其交互作用对烟叶硼、锌及品质的影响

以云南陆良植烟土壤为基础,利用田间调查取样和室内测定检测方法,分析了319份土壤有效硼、有效锌和对应C3F烟叶硼、锌、化学成分、多酚类物质和感官质量,拟找出适宜的土壤有效硼和有效锌含量区间,指导调控烤烟微肥营养。结果表明:(1)土壤有效硼、锌平均含量分别为0.54、2.74 mg·kg-1,空间变异较强,两者均有近1/3呈偏低水平;(2)土壤硼和烟叶硼、土壤锌和烟叶锌元素间的关系为极显著正线性相关,而烟叶硼随土壤有效锌含量的增加呈先升高后降低的趋势,烟叶锌与有效硼关系与之相似,均表现为曲线相关;(3)中等含量土壤有效硼与高含量有效锌交互可显著提高烟叶硼、锌含量和多酚类物质总量,提升烟叶的感官质量,同时烟叶化学成分可用性指数(CCUI)表现最高。其中有效硼、有效锌及其互作对烟叶CCUI总变异贡献率分别为61.5%、9.0%、29.5%,对多酚类物质总量的贡献率分别为52.9%、33.0%、14.1%,对感官质量的贡献率分别为58.7%、20.2%、21.1%;(4)综合分析结果,当土壤有效硼含量为0.6～0.7 mg·kg-1、有效锌为3.0～4.0 mg·kg-1时,烟叶硼、锌含量均保持较高水平,同时烟叶内在品质最佳。     

芝麻叶中总黄酮的最佳提取工艺研究

该文测定了芝麻叶中总黄酮的含量，并对芝麻叶黄酮的提取工艺进行了研究。重点探讨了采用乙醇提取法和微波处理与乙醇提取相结合的方法提取芝麻叶黄酮类化合物的最佳工艺条件。试验结果表明：芝麻叶中总黄酮的含量为0.98%；乙醇提取法的最适工艺参数是浸提剂乙醇浓度为80%、浸提温度为80℃、料液比为1∶25、浸提时间为2.5 h，如此条件可使黄酮提取率达95.6%；微波处理与乙醇提取相结合的方法的最适工艺参数是微波功率200 W、微波处理时间70s，乙醇浓度为80%、浸提温度为80℃、料液比为1∶25、浸提时间为30 min，这种工艺可使黄酮提取率达95.8%。     

甲亚胺—H法测硼时抑制铁干扰的方法

对按特定次序添加巯基乙酸和其他几种试剂的甲亚胺－Ｈ分光光度法加以改良后用于测定土壤浸提液，植物材料消化液及浓ＨＣｌ消化液中的硼。     

超声波协同微波提取黑米原花青素的工艺研究

【目的】优化原花青素提取的工艺条件,为其在黑米原花青素提取工艺方面提供参考依据。【方法】采用超声波协同微波技术提取,以黑米原花青素提取率为参考指标,并分别考察了溶剂百分数、料液比、提取温度、超声时间、微波功率等5个方面加以讨论、验证,并利用单因素试验分别验证各因素的显著性。【结果】黑米原花青素提取的最佳工艺条件为丙酮体积分数82%、超声时间54min、微波功率480W,在此种情况下,黑米原花青素的提取率达到2.411%。【结论】黑米原花青素对提取溶剂、溶剂百分数、料液比、超声时间、微波功率等方面显著性不同,其中溶剂百分数、超声时间、微波功率对黑米原花青素的提取率影响较大。     

超声波提取 -电感耦合等离子发射光谱法测定土壤中游离铁

建立了超声波提取 -电感耦合等离子发射光谱法(ICP-OES)测定土壤中游离铁含量。在传统方法的基础上,用超声波替换了水浴搅拌提取方式,降低了人工,提高了效率;力求提取方法的准确可靠,用超声波提取方式对提取温度和提取时间进行了探索,选出了提取温度为(80±5)℃,提取时间 15 min的最佳提取条件;引入具有准确度高、快捷简便特点,并基于超声波提取的 ICP-OES法使土壤游离铁的测定方法有了更多选择。该方法准确度加标回收率为 97%～103%,相对标准偏差(n=6)为 1.43%和 0.79%,表明该方法对各类型土壤批量测定游离铁具有普遍适用性和可靠性。     

微波在党参多糖的提取技术上的应用研究

以党参为原料,与常规水提法为参照,研究微波对党参多糖提取率、效果和结构的影响,并在此基础上研究出经微波处理的党参多糖提取工艺和条件,解决目前水提法因沸水处理时间长而导致多糖生理功能下降的负面影响.以微波的功率、提取时间、料液比作为影响因素进行了正交实验设计,研究党参多糖提取率,并采用红外线扫描对党参多糖的结构进行了分析,用硫酸-蒽酮法对所提多糖含量进行了测定.确定了微波提取党参多糖的最佳提取方案小火(所设置的最高档位),20min,料液比125,最高得率33.7%,仅比经过3h水提后的多糖得率低2.3%.该方法节能、省时,微波提取与水提相比对结构未产生影响.     

The relationship between boron soil test results and boron uptake by bean plants

Abstract

Boron sensitive crops, kidney beans and soybeans, were grown in pots containing soil collected from a beet field and a nearby pasture. Two soil extraction procedures were used to measure boron concentrations in the soils. Dilute acid was used to extract what is believed to be readily available boron. A modified‐Soxhlet apparatus, which employed continuous leaching with hot water, measured what is believed to be slowly available boron. Plant boron status was determined by analyzing the above ground portion of the plants grown in two soils. The amount of boron in the plant tops provides an indication of biologically available boron or that boron actually available to plants. Although kidney beans and soybeans extracted more boron from the beet soil, both soil extraction procedures indicated that the concentration of boron was higher in the pasture soil. Neither extraction procedure proved reliable in predicting plant response.     

Simplification of the standard method for determination of non-exchangeable NH4−N in soil

The widely-used Silva-Bremner method for determining non- exchangeable NH₄?N in the soil was modified so as to reduce reagent requirement and the time taken to carry out the analyses. In the modification, boiling the mixture of soil and KOBr on a hot plate was replaced with heating the soil/KOBr mixture, directly placed in centrifuge tubes, in a boiling water bath or a microwave oven. The best procedure is to keep the soil/KOBr mixture for 10 minutes in the water bath or for 10 minutes at 50% of full power in a microwave oven. The modified method gave similar values to the standard method on 4 quite different soils and also slightly increased reproducibility.     

Extraction of boron from soil by microwave heating for ICP‐AES determination

Abstract

Extraction with hot water is the most widely used procedure to determine boron (B) in soils for the diagnosis of the nutrient availability for plants. However, this procedure is tedious for routine conditions and requires some special precautions. An alternative extraction procedure was developed, consisting in the extraction of B with a 1.25 g/L solution of barium chloride (BaCl₂) or with water heated in a domestic microwave oven. Boron was determined either by inductively coupled argon plasma emission spectrometry (ICP‐AES) and by spectrophotometry with azomethine‐H. Good correlations were found between the extraction by boiling water under reflux and the extraction by the microwave heating for 13 Brazilian soils, and the contents of B obtained by spectrophotometry did not differ significantly from those obtained by ICP‐AES. Considering the calculated standard deviations, it can be concluded that microwave heating followed by ICP‐AES determination is an adequate procedure for the determination of hot water extractable B in soils.     

Kinetics of the hot water soluble boron soil test

Abstract

A first order reversible reaction rate equation was modified to fit the conditions of the hot water soluble boron soil test. This equation was fitted to a boiling time study on one soil fertilized to three different boron levels. The common S‐minute boiling time did not remove enough boron to reach the plateau region of the fitted curve for any sample. It was also found that boiling for too short a time causes more error than excessive boiling. For these samples a boiling time could be more than a minute too short before a 10% error was introduced in the amount of boron extracted. A 10‐minute boiling time would reduce the timing error for these samples by removing enough boron to reach the plateau region of the extraction curve.     

Sources of variation in hot water extraction and colorimetric determination of soil boron

Abstract

The reliability of the soil test for boron (B) has been questioned in recent years. Two studies were initiated to identify some of the sources of variability in the extraction and analysis phases of the B soil test. The first study evaluated the influence of reflux and cooling times (10,20,30 min.) on B values. The second study investigated the effectiveness of CaCl₂ (0,3,6,9 mM) and charcoal (0,0.08, 0.16, 0.32, 0.64 g) as soil extract decolorizing agents. Hot water extraction, in plastic pouches, with azomethine‐H and/or ICP analysis was used to determine soil B. Increasing reflux time resulted in significantly higher B values, while increasing cooling time resulted in significantly lower B values (P = 0.05). Standardized refluxing/cooling conditions contributed to improved reprodudbility of B values obtained by hot water extraction. Increasing reflux CaCl₂ concentration and/or charcoal addition significantly lowered B values. The lower B values obtained with the CaCl₂ treatments were the direct result of decreased background color. Charcoal was also effective in reducing background color but higher additions of charcoal (greater than 0.16 g) resulted in excessive sorption of boron. Soils should be refluxed in 10 mM CaCl₂ to minimize extract color if azomethine‐H analysis is used. If extract color persists, a minimum addition (less than 0.16 g) of charcoal should be added prior to filtering. The conclusions of this study were incorporated into a soil test B procedure included in this report.     

固体发酵裂褶菌多糖提取方法比较

用热水、超声及微波法提取裂褶菌固体发酵基质中的裂褶菌多糖,研究了超声与微波提取工艺条件,并比较了3种提取方法下多糖的提取率及平均相对分子质量。结果表明,微波提取法效果最好,在微波功率3.5W/ml、作用时间8min、料水比1∶20条件下,多糖得率达到12.32%（g/100g干基）,分别较热水提取、超声提取法增加了70...     

Determination of Available Cadmium and Lead in Soil by Flame Atomic Absorption Spectrometry after Cloud Point Extraction

A cloud point extraction (CPE) procedure has been developed for the determination of available cadmium (Cd) and lead (Pb) in soil by flame atomic absorption spectrometry. The proposed method was based on the CPE of a complex from ammonium pyrrolidine dithiocarbamate (APDC) and metal Cd and Pb using emulsifier octyl polyethylene glycol phenol ether (OP) as surfactant. Conditions that would affect the complex formation and separation were researched in detail, including extraction conditions as well as pH, amount of the chelating agent, concentration of the surfactant, equilibration temperature and time, and salt effect. Under the optimized conditions, both of the calibration graphs were linear in range of 0–1.0 μg mL^?1 with detection limits of 0.29 ng mL^?1 for Cd and 2.10 ng mL^?1 for Pb. The relative standard deviation (RSD) for 11 replicate measurements at 0.10 μg mL^?1 of Cd and Pb were 2.18% and 4.04%, respectively. The enhancement factors were 48.8 and 61.6 for Cd and Pb, respectively. The recoveries of Cd and Pb at the spiking level of 0.10 μg g^?1 in soil samples were from 91.7% to 115% and from 91.0% to 115%, respectively. The proposed method has been applied to the determination of available Cd and Pb in soil.     

杏鲍菇深加工残渣多糖酶法微波辅助提取工艺优化

为了研究杏鲍菇残渣中多糖的酶处理-微波辅助提取工艺及生物活性,该文以杏鲍菇深加工后的残渣为原料,在纤维素酶处理的基础上,微波辅助法提取杏鲍菇多糖;利用响应面试验设计对提取工艺条件进行优化,并与传统热水提取方法进行比较;对杏鲍菇多糖进行抗氧化和抑菌活性评价。结果表明,微波辅助提取杏鲍菇多糖的较佳条件为:水料比35∶1 m L/g,提取时间15 min,微波功率570 W,此条件下多糖的提取率为12.11%±1.02%,比热水提取高出41.21%,且提取时间缩短了105 min。杏鲍菇多糖对1,1-二苯基-2-三硝基苯肼自由基、羟基自由基和超氧阴离子自由基具有一定的清除作用,其半数抑制浓度(IC50)分别为22.9、19和21.1 mg/m L,对枯草芽孢杆菌、大肠杆菌和金黄色葡萄球菌具有较好的抑制作用,其最低抑制质量浓度分别为8、16和16 mg/m L,对黑曲霉和酿酒酵母没有明显的抑制作用。研究结果为进一步开发杏鲍菇多糖功能和利用杏鲍菇残渣提供一定的技术依据。     

Pressurized Hot Water and DTPA‐Sorbitol as Viable Alternatives for Soil Boron Extraction. I. Boron‐Treated Soil Incubation and Efficiency of Extraction

Abstract

Serious challenges associated with hot water extraction, the standard extraction method for water‐soluble boron (B), limit its use in commercial soil‐testing laboratories. Several alternatives to make B testing more practical have been proposed and studied; none of the alternatives have readily replaced the hot water method. Two relatively new, promising B extraction methods are pressurized hot water and DTPA‐Sorbitol. Very little reported work compares B extraction values obtained from the standard hot water extraction method and these two alternative methods. This study was conducted to complete an initial step in validating new procedures—extracting the designated nutrient from fertilized, incubated soils by using standard and alternative extraction methods and comparing the resulting values. The three extraction methods were used to extract B from samples of calcareous sand and silt loam soils and limed, loamy fine sand, all which had been treated with 10 levels of B (0–8 mg kg^?1) and incubated for 7 and 28 days. The amount of B extracted increased as the rate of B application increased with all three soil‐extraction methods. High correlations (r 0.977–0.999) were observed between extractable B and rate of B application with all three procedures. Correlations between the amount of extractable B using hot water extraction and the value obtained with an alternative extraction method were similar for both methods (r=0.89). Hot water generally extracted the least and pressurized hot water the most B regardless of soil type, rate of application, or duration of incubation. This study suggests the more easily used methods of pressurized hot water and DTPA‐Sorbitol could be recommended as replacements to the cumbersome hot water extraction.     

Microwave-assisted headspace solid-phase microextraction for the analysis of bioemissions from Eucalyptus citriodora leaves

Microwave-assisted headspace solid-phase microextraction (MA-HS-SPME) was developed as a simple and effective method for fast sampling of volatile organic compounds (VOCs) from Eucalyptus citriodora Hook (E. citriodora) leaves. During microwave heating, a simple shielding device made of aluminum foil was used to protect the SPME fiber from microwave irradiation while allowing the sample to be heated. A room temperature water bath was also used to allow microwave heating to be conducted in a more controlled manner. The inner heating caused by microwave irradiation dramatically accelerated the emission of VOCs from the sample, but no marked change in headspace temperature in the sample vial was found. Under optimum conditions, the extraction efficiencies obtained with microwave heating were much higher than those obtained without microwave heating for all fibers used, namely, 7-microm polydimethylsiloxane (PDMS), 100-microm polydimethylsiloxane (PDMS), 65-microm polydimethylsiloxane/divinylbenzene (PDMS/DVB), and 75-microm carboxen/polydimethylsiloxane (CAR/PDMS). The improvement of extraction efficiency using MA-HS-SPME allowed more VOC events to be detected, with more balanced extraction of VOCs of lower and higher molecular masses. Moreover, a good linear relationship was found between sample size and GC-FID response (total peak area of VOCs), indicating the usefulness of MA-HS-SPME for quantitative analysis of individual volatile compounds in E. citriodora leaves.