麻疯树饼粕中植物甾醇的提取

建立超声辅助溶剂法提取麻疯树饼粕中的植物甾醇,以分光光度法检测提取物中甾醇含量。采用正交试验设计优选提取工艺,最佳提取工艺为麻疯树饼粕50g,丙酮100mL,超声提取1h。优化工艺条件下植物甾醇的萃取率可达0.347%。     

混合甾醇中β-谷甾醇和豆甾醇的红外光谱法分析测定

用傅里叶变换红外光谱法测定了混合甾醇中 β 谷甾醇和豆甾醇的含量 ,结果表明 β 谷甾醇和豆甾醇中的红外特征吸收峰面积比与 β 谷甾醇和豆甾醇的含量比成线性关系 ,红外光谱法测得混合物中各组成的含量与由气相色谱法得到的结果相近 ,表明用红外光谱法测定混合甾醇的含量是可行的。     

络合法提取麻疯树种子油中的植物甾醇

建立络合法提取麻疯树种子油中的植物甾醇,以分光光度法检测提取物中甾醇含量。采用正交试验设计优选提取工艺,最佳提取工艺非质子溶剂为乙酸乙酯,质子溶剂为甲醇,皂化物与氯化钙质量比为8:1,皂化物与乙酸乙酯料液比(g:mL)为16:27,皂化物与甲醇料液比(g:mL)为16:1,反应温度60℃,反应时间1 h。优化工艺条件下植物甾醇的萃取率可达2.72%。     

衍生化气相色谱质谱联用法同时测定烟叶多种植物甾醇

以丙酮为提取剂、1％硫酸-乙醇(V∶V)溶液和2.0 mol/L氢氧化钾-乙醇分别作水解剂和皂化剂,利用三甲基氯硅烷和六甲基二硅烷作为硅醚化衍生试剂,采用气相色谱质谱联用仪同时检测烤烟烟叶中的多种甾醇化合物.采用内标校准曲线法对胆甾醇、菜油甾醇、豆甾醇、β-谷甾醇进行准确定量分析;利用内标相对定量法对p香树脂醇、豆甾-...     

混合甾醇中β-谷甾醇和豆甾醇的紫外光谱法分析测定

用紫外光谱法测定了β-谷甾醇和豆甾醇与Deniges磺基醋酸汞络合物的紫外光谱,探讨了显色反应时间、显色剂用量及浓硫酸与冰醋酸配比对紫外吸收光谱的影响。结果表明在一定浓度范围内,甾醇络合物的吸光度A与其浓度成线性关系。并利用紫外光谱法测定了混合甾醇中β-谷甾醇和豆甾醇的含量,此法所得结果与用气相色谱法测试的结果相近。     

侧扁软柳珊瑚中的3个甾醇

从中国南海侧扁软柳珊瑚(Subergorgia suberos)乙酸乙酯萃取相中首次分离得到3个甾醇化合物,根据现代波谱技术(MS,1D NMR,2D NMR)鉴定它们的结构,分别为:孕甾-5-烯-3-醇-20-羧酸(1),胆甾-3β,5α,6β-三醇(2),胆甾-22-烯-3β,5α,6β-三醇(3)。肿瘤活性实验表明,甾醇3对7种肿瘤细胞株的IC50值分别为:14.51、19.82、10.22、16.49、29.16、41.72与50.12μg/mL。     

混合胶束增敏火焰原子吸收光谱法测定植物叶片中的痕量铅

研究了十二烷基磺酸钠（SDS）和乳化剂OP组成的混合胶束对植物叶片中痕量铅测定的增敏作用,建立了植物叶片中痕量铅的火焰原子吸收光谱测定新方法,灵敏度比不加混合胶束提高了29%,该法快速,简便,廉价。结果表明：在0—5.0μg/mL范围内吸光度与Pb2＋浓度呈良好的线性关系,线性回归方程为APb＋SDS＋OP=0.0391C（μg/mL）＋0.0073,r=0.9974,检出限为0.006μg/mL。植物样品采取先灰化再对干灰进行快速消解的方法处理后,应用该方法对不同地区不同植物叶片中的铅进行测定,测定的相对标准偏差RSD为0.50%—3.90%,加标回收率为96.9%—103%,结果显示同一地区植物叶片中的铅含量与植物种类有关、不同地区同种植物叶片中的铅含量与交通密度有关。     

南海圆形短指软珊瑚Sinularia Brassica的化学成分

从圆形短指软珊瑚Sinularia Brassica中分离出3种甾醇,通过波谱分析等方法,确定其结构为（1）柳珊瑚甾醇,（2）23-乙基-胆甾-5-烯-3-醇,（3）24-甲基-胆甾-5,22-二烯-3-醇。     

微波消解植物灰分与环境土壤中微量元素的ICP-AES方法研究

应用MDS-2002A犁压力自控密闭微波消解样品制备系统,针对研究样品的特性和共性,进行植物灰分和土壤样品相同微波消解条件的研究实验,并采用电感耦合等离子体原子发射光谱法测定其元素的含量.讨论了混合酸体系、混酸配比、固液比和微波消解时间对于样品制备结果的影响.最终的优选方案为A281C2,即微波程序为工步2,混酸配比为6:2:1:1,混合酸体系为HNO3-HCl-HF-HClO4,最高功率消解时间为10 min的条件下,消解结果最佳.在微波消解最佳条件下,进行了方法准确度实验和测量结果重现性实验,该方法经土壤(GBW07401)和植物(GBW07603)国家标准物质验证,所得测试结果的相对误差均在0.00%～7.14%之间,相对标准偏差均在0.87%～5.25%之间.结果表明,微波消解法处理植物灰分和土壤样品,具有快速、简便、节省试剂、消解完全等特点,测定结果的准确度和精密度令人满意.     

松香与甘油酯化稀土催化剂的研究

本文分别用三氧化二钇、三氧化二钕、混合稀土氧化物作为松香与甘油酯化时的催化剂，研究了稀土氧化物的用量对酯化反应的温度和产物色泽的影响。并用比色法测定了产物的色泽。     

Ultrasonic pretreatment for lipase-catalyed synthesis of phytosterol esters with different acyl donors

This study is focused on the enzymatic esterification of phytosterols with different acyl donors to produce the corresponding phytosterol esters catalyzed by Canadia sp. 99-125 lipase under ultrasound irradiation. An ultrasonic frequency of 35 kHz, power of 200 W and time of 1h was determined to guarantee satisfactory degree of esterification and lipase activity. The influence of temperature, substrates concentration and molar ratio was investigated subsequently. The optimum production was achieved in isooctane system at 60°C with phytosterol concentration of 150 μmol/mL and phytosterol to fatty acid molar ratio of 1:1.5, resulting in a phytosterol esters conversion of above 85.7% in short reaction time (8h). Phytosterols esters could also be converted in high yields to the corresponding long-chain acyl esters via transesterification with triacylglycerols (above 90.3%) under ultrasound irradiation. In optimum conditions, the overall esterification reaction rate using the ultrasonic pretreatment process was above 2-fold than that of mechanical stirring process without damage the lipase activity.     

核磁共振技术在SIPM开发生产中的应用

本文利用核磁共振氢谱技术，建立了生产间苯二甲酸二甲酯磺酸钠（SIPM）工序中磺化率、酯化率的快速测定方法，为工艺的进一步优化及常规的中控分析方法的建立提供了依据。并尝试利用核磁共振技术测定SIPM在水中及8％硫酸钠水溶液中不同温度下的溶解情况。对生产所用的原料、产品的纯度以及废水处理中的副产物进行了测定，结果令人满意。     

Sonochemical preparation of high surface area MgAl2O4 spinel

High surface area MgAl(2)O(4) has been synthesised by a sonochemical method. Two kinds of precursors were used, alkoxides and nitrates/acetates and in both cases nanostructured MgAl(2)O(4) was obtained. The effect of the addition of a surfactant during the sonication, cetyl trimethyl ammonium bromide, was also investigated. In the case of alkoxides precursors the as-made product is a mixture of hydroxides of aluminium and magnesium, while with nitrates/acetates a gel is obtained after sonication, containing the metal hydroxides and ammonium nitrate. Heating at 500 degrees C transforms the as-made products into MgAl(2)O(4) spinel phase. The surface area is up to 267m(2)/g after treatment at 500 degrees C and 138m(2)/g at 800 degrees C.     

Esterification of Dicarboxylic Acids with 2-Ethylhexanol under Supercritical Conditions

A study of esterification process of dicarboxylic acids with 2-ethylhexanol under supercritical conditions is presented. It was shown that the esterification reaction can be carried out without a catalyst. The esters formed with greater rate and selectivity.     

The use of ultrasound in the extraction of Ilex paraguariensis leaves: a comparison with maceration

The objective of this work is to discuss the main parameters that influence the sonication extraction of Ilex paraguariensis leaves. For this purpose, the extraction time, solvent polarity, solvent volume, sample mass and particle size were evaluated. Results showed that the main variable affecting the extraction process was the solvent polarity. Though in a less extent, temperature and extraction time also demonstrated to be important parameters, while the other variables did not present a significant influence on the extraction yield. The extracts at the optimized condition were compared with those obtained by maceration, in terms of mass yield and chemical composition. The major compounds identified in the extracts were caffeine and palmitic acid. Some saturated hydrocarbons such as fatty acids, fatty acid methyl esters, phytosterols, and theobromine were also identified in the fractions.     

超声波在乙酸乙酯和乙酸甲酯中的弛豫吸收

关于超声波在乙酸乙酯和乙酸甲酯中的吸收问题曾引起了多次热烈的争论,为此,作者采用了行波中的光衍射法做了进一步的实验研究。在实验过程中,特别注意了仪器的精确度问题,并且对许多种吸收系数已知的标准液体进行了多次重复的测量,结果很好地符合于一般的公认值,且误差不超出5％。对于两种乙酸酯,测量的频率范围是3-30Mc,温度保持20℃。测量结果表明,在实验的误差范围内,吸收的实验值很好地落在唯象单弛豫理论所预期的曲线上,弛豫频率对乙酸乙酯约在12Mc附近,对乙酸甲酯约在7Mc附近。并且通过对不同纯度的乙酸乙酯进行重复的测量,表示杂质引起的附加吸收并不影响吸收曲线的特性。因此也就明某些作者测量得到两个弛豫频率的结果是不真实的。作者并认为Karpovich首先提出的旋转异构的理论是适合于解释这两种液体的驰豫吸收的机理的。     

陈化温度和Fe/Zr配比对SO42-/Fe2O3-ZrO2固体超强酸结构与性能的影响

用低温陈化法制备了SO42 -/Fe2 O3 ZrO2 (简称SFZ)固体超强酸催化剂 ,用红外光谱 (IR)和X光衍射(XRD)对其结构进行了表征 ,并考察了它对合成癸二酸二正丁酯的催化性能 .IR谱显示 ,低温陈化的SFZ样品在10 70cm-1处吸收峰远强于常温陈化样品 .XRD分析则显示 ,在焙烧温度为 6 5 0℃、Fe/Zr为 2∶1时 ,低温陈化的样品出现了亚稳态的ZrO2 四方晶相 .该样品在催化酯化反应中使产率达 90 %以上 ,高于常温陈化样品的 30 % .研究结果表明 :在其他条件不变时 ,低温陈化所出现的亚稳态的ZrO2 四方晶相是表面酸性和催化活性增加的微观原因     

Ultrasound-assisted biodiesel production by a novel composite of Fe(III)-based MOF and phosphotangestic acid as efficient and reusable catalyst

In this work, esterification of oleic acid by various alcohols is achieved with high yields under ultrasonic irradiation. This reaction performed with a novel heterogeneous catalyst that fabricated by heteropoly acid and Fe(III)-based MOF, namely MIL-53 (Fe). Syntheses of MIL-53 and encapsulation process carry out by ultrasound irradiation at ambient temperature and atmospheric pressure. The prepared composite was characterized by various techniques such as XRD, FT-IR, SEM, BET and ICP that demonstrate excellent catalytic activities, while being highly convenient to synthesize. The obtained results revealed that ultrasound irradiation could be used for the appropriate and rapid biodiesel production.     

乙酸酐衍生化气相色谱法测定小麦非淀粉多糖的单糖组成

采取乙酸酐衍生化气相色谱法测定从小麦麸皮中提取的2种可溶性非淀粉多糖（non-starch polysaccharides,NSP）的单糖组成。所制备的小麦水提取NSP和碱提取NSP中主要的单糖组成是阿拉伯糖和木糖,另外还含有少量的葡萄糖、甘露糖和半乳糖。测定方法的回收率在95.56%—98.62%之间。