固相萃取和高效液相色谱法测定鱼腥草中的黄酮

 研究了用固相萃取预分离,高效液相色谱法测定鱼腥草根和鱼腥草叶中黄酮类物质的方法.鱼腥草根和鱼腥草叶中的黄酮用80%乙醇溶液加热回流提取,提取液用Waters Sep-Pak-C₁₈固相萃取小柱预分离脱脂,以Waters Nova-Pak-C₁₈(Φ3.9 mm×150 mm,5μm)色谱柱为固定相,以0.05 mol/L磷酸二氢钾缓冲溶液和甲醇的体积比为40:60的混合液为流动相,在该色谱条件下,鱼腥草中主要的黄酮成分均达到基线分离;用紫外二极管矩阵检测器在360 nm波长处检测,并作了色谱峰纯度分辨.方法标准回收率为98%~101%,相对标准偏差为0.85%~2.2%.     

鱼腥草多糖提取工艺及成分分析研究

 研究了鱼腥草多糖的提取工艺.结果表明,鱼腥草多糖的最佳提取工艺为:液固比(V/m,mL/g,下同)30:1,80℃水浴提取3次,每次2 h,多糖提取率达3.5%.除蛋白、上凝胶层析分离柱得多糖纯品,用WatersSep-pak C₁₈固相萃取小柱预分离,以Waters carbohydrate高效糖柱为固定相,V(乙腈):V(水)=70:30为流动相分离,蒸发光散射仪为检测器检测,得到鱼腥草多糖组成m(木糖):m(果糖):m(阿拉伯糖):m(半乳糖)=2.209:1.587:1.000:2.092.     

用固相萃取和微柱高效液相色谱法快速测定枸杞样品中的类胡萝卜素

研究了固相萃取富集和预分离,微柱高效液相色谱快速测定枸杞样品中类胡萝卜素的方法;枸杞样品中的类胡萝卜素用Waters Sep-Pak C18固相萃取小柱预分离,然后以Waters XterraTMRP18(1.0×50 mm,2.5μm)微柱为固定相,甲醇-四氢呋喃(80:20,V/V)为流动相分离,用二极管矩阵检测器检测,检测波长为450 nm,枸杞样品中的几种类胡萝卜素在5 min内可达到基线分离。方法标准回收率为95~103%,RSD为1.9~2.6%。用该方法测定了几种枸杞样品中的类胡萝卜素,结果令人满意。     

高效液相色谱法测定果酒中的糖、甘油和乙醇

 研究了高效液相色谱法测定果酒中的糖、甘油和乙醇的方法.果酒样品用Sep-Pak-C18固相微萃取小柱预分离,以WatersSugar-PakⅠ钙型阳离子交换柱为固定相,0.05g/LEDTA钙钠水溶液为流动相,示差折光仪为检测器,一次进样测定果酒样品中的蔗糖、葡萄糖、果糖、甘油和乙醇.最低检测限在微克级,相对标准偏差在0.92%～1.52%之间,标准回收率在97%～105%之间.方法用于果酒样品的测定,结果满意.     

SPE-UHPLC测定淀粉及淀粉制品中丁烯二酸类酸度调节剂

建立固相萃取-超高效液相色谱法测定淀粉及淀粉制品中的顺丁烯二酸、顺丁烯二酸酐和反丁烯二酸含量的检测方法。样品经ProElut PWA混合型弱阴离子交换固相萃取柱净化,超高效液相色谱分析,采用Waters Acquity UPLC HSS T3色谱柱,洗脱液为(磷酸)=0.10%水溶液与甲醇的体积比为98∶2,检测波长214nm,流速0.2mL·min-1。在此条件下,顺反丁烯二酸分离良好且无杂质峰干扰,样品加标回收率83.81%～108.03%,相对标准偏差(n=8)小于10%,顺丁烯二酸和反丁烯二酸的定量限为0.25mg·kg-1,能够满足实际检测需要。     

中药材丹参中4种主要丹参酮的超高效液相色谱法测定研究

建立了用超高效液相色谱法(UPLC)同时测定中药材丹参中隐丹参酮、丹参酮Ⅰ、丹参酮ⅡA和二氢丹参酮的超高效液相色谱法.中药材样品中的丹参酮用高速匀浆法提取,采用Waters ACQUITY UPLC BEHC18(1.7μm,2.1 mm×50 mm)超高效液相色谱柱为固定相,40%的乙腈(内含0.1%的磷酸)为流动相分离,检测波长为254 nm,流速为0.6 mL/min.在上述色谱条件下隐丹参酮、丹参酮Ⅰ、丹参酮ⅡA和二氢丹参酮在5.0 min内实现基线分离,加标回收率在91.5%~98.6%之间,日内相对标准偏差为2.1%,日间相对标准偏差为2.8%,结果满意.     

匀浆法提取、离子色谱法测定烟草中的糖

研究了用匀浆法提取、离子色谱法测定烟草中的糖.烟草样品用水匀浆法提取;提取液中的糖以CarboPac PA1(4×250 mm,5μm)阴离子交换柱为固定相,0.2 mol/L氢氧化钠溶液为流动相分离,脉冲安培检测器检测;1次进样可同时测定烟草样品中葡萄糖、果糖、蔗糖.方法加标回收率在96%～103%之间,相对标准偏差均小于2.6%.检测限均小于50μg/L,结果满意.     

用HPLC法测定猕猴桃鲜果中糖含量

采用氨基枉为固定相,乙腈/水为流动相和示差折光检测的高效液相色谱法,在乙腈/水组成比为78∶22的等组分洗脱条件下,20分钟内,可同时测定七种糖,即鼠李糖,果糖,葡萄糖,蔗糖,麦芽糖,乳糖和棉子糖;并应用这一方法,测定了猕猴桃鲜果中糖含量。分析结果表明,猕猴桃中主要糖成分是果糖、葡萄糖和蔗糖,而其总含糖量约为7～10％。     

LC-MS-MS测定河口及近岸海水中的氟喹诺酮类药物

建立了河口及近岸海水中氟喹诺酮类药物残留的固相萃取富集-高效液相色谱-串级质谱测定方法.以Waters HLB固相萃取（SPE）小柱富集水样中的氟喹诺酮类药物,用XDB-C18柱、乙腈、甲酸（体积分数为0.2%）水流动相进行分离,ESI正离子源、三重串级质谱及多反应监测模式（MRM）进行目标物的定性、定量测定.优化实验...     

煤基固废复合改性剂高温重构钢渣的性能及机理研究

为了促进钢渣和煤基固废的综合利用,研究了煤基固废复合改性剂(CMCSR)(煤气化渣-硅钙渣-煤田区域水库底泥)对高温重构钢渣的胶凝性能和体积稳定性的影响,采用XRD、SEM、EDS等测试方法,对重构钢渣的物相组成、微观结构及高温重构机理进行了分析。发现CMCSR可以提高钢渣的胶凝性能,显著降低了钢渣中f-CaO含量。当重构温度为1250℃,CMCSR掺量为25%时,重构钢渣28d活性指数比原钢渣可提高16.1%,重构钢渣中f-CaO的含量由4.04%降至1.90%,满足GB/T20491-2017《用于水泥和混凝土中的钢渣粉》中f-CaO含量≤3%的要求。CMCSR掺量由15%增加至35%,重构钢渣中形成透辉石(CMS₂)、钙铝黄长石(C₂AS)、C₃A等硅铝基矿物。高温重构过程促使RO相中的FeO转变为镁铁尖晶石(MgFe₂O₄)和磁铁矿(Fe₃O₄)。重构温度为1250℃,掺25% CMCSC的重构钢渣形成结晶良好、粒径可达10μm以上椭圆形的C₂S颗粒。研究表明,掺入煤基固废复合改性剂的高温改性钢渣,其体积稳定性、胶凝活性和易磨性得到了有效改善,从而为钢渣的低能耗细磨加工进行制品开发,或在水泥和混凝土中的直接应用提供了可能,实现了煤基固废与冶金固废的协同利用。     

丙酮/(NH4)2SO4双水相体系提取芦丁影响因素研究

【目的】研究丙酮/(NH4)2SO4双水相萃取体系对分离槐米中芦丁的影响因素。【方法】利用正交设计法进行优化,并把28.57%的硫酸铵溶液与等体积的70%的丙酮混合溶液,调至pH=9形成的双水相,两相的体积比(V上/V下)是1.62。【结果】萃取体系的上相中芦丁含量达到95.92%。【结论】丙酮/(NH4)2SO4双水相萃取体系分离芦丁具有良好的选择性。     

Synthesis mechanism of LiNiVO4 by wet chemical method and mixed valence of nickel and vanadium

The single phase LiNiVO₄ has been successfully synthesized by adopting a new mild liquid route with oxalic acid as both complexant and precipitant, and this method is named the CPG method. The products were obtained by sintering the dry gel precursor which was prepared by the CPG method at 200—850℃ for 2—10 h in air. The products were tested by XRD, XPS, ESR and TGA-DTA, and the results indicate that the single phase LiNiVO₄ could be obtained at 450℃ for 2—3 h in air and LiNiVO₄ was still steady at 850℃ for 10 h. The valence analyses show that in LiNiVO₄ the valence of lithium is +1, both nickel and vanadium have the mixed valence, namely +2, +3 for nickel and +4, +5 for vanadium respectively. The LiNiVO₄ can be expressed as LiNi³⁺_xNi²⁺_1-xV⁴⁺_xV⁵⁺_1-xO₄ (0≤x<1). The pyrolysis mechanism of the dry gel is also discussed.     

Experimental and theoretical studies of the reaction between cationic vanadium oxide clusters and acetylene

The time of flight mass spectrometer coupled with a laser ablation/supersonic expansion cluster source and a fast flow reactor was adopted to study the reactivity of cationic vanadium oxide clusters （VinOS,） toward acetylene （C2H2） molecules under gas phase （P, - 1.14 kPa）, under near room temperature （T, - 350 K） conditions. Association products, VmOnC2H2^＋ （m,n = 2,4; 2,6; 3,7-8; 4,9-11; 5,12-13; 6,13-16, and 7,17）, are observed. The oxidation of C2H2 by （V2Os）n^＋ （n = 1 -3） is experimentally identified. The reactivity of （V2O5）n^＋ decreases as n increases. Density functional theory （DFT） calculations were carried out to interpret the reaction mechanisms. The DFT results indicate that a terminal oxygen atom from V2O5^＋ can transfer overall barrierlessly to C2H2 at room temperature, which is in agreement with the experimental observation. Other experimental results such as the observation of V206C2H2^＋ and nonobservation of V2O7,8C2H2^＋ in the experiments are also well interpreted based on the DFT calculations. The reactivity of vanadium oxide clusters toward acetylene and other hydrocarbons may be considered in identifying molecular level mechanisms for related heterogeneous catalysis.     

Estimation of soil water retention curve: An asymmetrical pore-solid fractal model

The soil water retention curve is an important hydraulic function for the study of flow transport processes in unsaturated soils. The objective of this study was to develop a soil water retention function using a generalized fractal approach. The model exhibits asymmetry between the solid phase and pore phase, which is in marked contrast to the symmetry between phases present in a conventional fractal model. The retention function includes 4 parameters: the saturated water content θs, the air entry value ha, the fractal dimension Df, and an empirical parameter β, characterizing the complicated soil pore structures. Sixty one data sets, covering a wide range of soil structure and textural properties, were used to evaluate the applicability of the proposed soil water retention function. The retention function is shown to be a general model, which incorporates several existing retention models. The values of β/θs and (θs-θr )/β were used as indexes to quantify the relationships between the proposed retention function and the existing retention models. The proposed function fits all the data very well, whereas other tested models only match about 16%-48% of the soil retention data.     

红芪加工废弃物活性多糖对果蝇生育力和寿命及抗氧化能力的影响

研究红芪废弃物中提取的生物活性多糖对黑腹果蝇的生殖能力、寿命和抗氧化能力的影响。通过不同浓度的红芪多糖对黑腹果蝇的存活试验,研究了一代至四代(F1-F4)的生殖能力和寿命、雌雄个体数、抗氧化酶超氧化物歧化酶(SOD)、过氧化氢酶(CAT)的活性和丙二醛(MDA)含量的变化。结果表明,与对照组相比,添加多糖可提高F1-F4雌雄果蝇的繁殖能力,延长其寿命,降低果蝇体内丙二醛含量,提高了黑腹果蝇的抗氧化能力和生命力,表现出剂量效应,雌雄果蝇性比为接近1:1。     

Study on the flow injection micro-column pre-separation system coupled with high performance liquid chromatography for the determination of ecdysterone in traditional Chinese medicine

A flow injection (FI) micro-column system coupled with high performance liquid chromatography (HPLC) was proposed for the pre-separation and determination of active organic component (ecdysterone) in traditional Chinese medicine, Loulu. The factors influencing separation performance were investigated and optimized. Under the optimal conditions, the contents of ecdysterone in Loulu were determined by HPLC system using MeOH-H₂O (40∶60,V/V) as the mobile phase at a flow rate of 1.0 mL/min. The calibration curve was linear in the range of 0.5∼100 mg/L of ecdysterone concentrations. The detection limit of the analyte was 0.11 μmol/L (3σ) with a precision of 0.38% RSD (n=7,c=10.0 mg/L). The average recovery of the method was 98.7%. The proposed method has been applied to determine ecdysterone in practical samples, and the determined values by both external standard method and standard addition method were in good agreement. Compared to the traditional solid extraction method, the system proposed has the advantages of simple procedure, good reproducibility, minimum volume requirement, reduction of matrix interference and low contamination risk. Foundation item: Supported by Education Ministy Foundation for Chinese Returned Scholars and Nature Science Foundation of Hubei province (98J054). Biography: SHUAI Qin (1963-), famale, Ph.D. Candidate.     

Liquid-Liquid Equilibrium for 1-Butanol-Water-KF and 1-Butanol-Water-K2CO3 Systems

KF or K2CO3 was added into the 1-butanol-water system and two phases were formed： water-rich phase （water phase） and 1-butanol-rich phase （1-butanol phase）. The liquid liquid equilibrium （LLE） data for 1-butanol-water-KF and 1-butanol-water-K2CO3 systems were measured at 25℃ and showed that 1-butanol phase contained negligible salt and water phase contained negligible 1-butanol when the concentrations of KF and K2CO3 in the water phase were equal to or higher than 27.11% and 31.68% , respectively. Thus water could be separated efficiently from 1-butanol-water by adding KF or K2CO3 into the system. A theoretical calculation of LLE data was calculated by using the Pitzer theory to get water activity in the water phase, and by the models, such as the Wilson, NRTL or the UNIQUAC for the 1-butanol phase. For 1-hutanol-water-KF system, the experimental data were found in good agreement with the calculated results by using Pitzer theory and Wilson equa tion, while for 1-butanol-water-K2CO3 system, the experimental data were found in good agreement with the calculated results by using Pitzer theory and UNIQUAC eauation.     

Effects of synthetic conditions on the structure and morphology of open-ended vanadium oxide nanotubes and study of their growth mechanism

Vanadium oxide nanotubes (VOx-NTs) have been synthesized by using n-butylamine as structuredirecting template and V2O5 as precursor under hydrothermal conditions. XRD, FTIR, SEM, TEM, BET and TG-DTA characterizations have been performed to both optimize the synthetic conditions and understand the growth mechanism of VOx-NTs. The results showed that open-ended VOx-NTs were obtained under the optimized conditions (hydrothermal temperature: 150―160°C, hydrothermal time: 5―7 d, the molar ratio of V2O5 to n-butylamine is 1:1) with diameters ranging from about 30 to 100 nm and several micrometers in length. The BET surface area and the desorption cumulative pore volume of pores of the as-synthesized sample were about 27.4609 m2/g and 0.191087 cm3/g, respectively. The result presents that the synthesis of VOx-NTs is controlled by the "rolling" mechanism and temperature is primary driving force for rolling.     

Electro-deoxidation of V<Subscript>2</Subscript>O<Subscript>3</Subscript> in molten CaCl<Subscript>2</Subscript>-NaCl-CaO

The electro-deoxidation of V₂O₃ precursors was studied. Experiments were carried out with a two-terminal electrochemical cell, which was comprised of a molten electrolyte of CaCl₂ and NaCl with additions of CaO, a cathode of compact V₂O₃, and a graphite anode under the potential of 3.0 V at 1173 K. The phase constitution and composition as well as the morphology of the samples were studied by X-ray diffraction (XRD) and scanning electron microscopy (SEM). 3 g of V₂O₃ could be converted to vanadium metal powder within the processing time of 8 h. The kinetic pathway was investigated by analyzing the product phase in samples prepared at different reduction stages. CaO added in the reduction path of V₂O₃ formed the intermediate product CaV₂O₄.