Optimization of Ultrasonic-Assisted Extraction Process of Polysaccharides from American Ginseng and Evaluation of Its Immunostimulating Activity

Ultrasonic-assisted extraction （UAE） of American ginseng polysaccharides （AGP） was investigated using response surface methodology. Three-factor-three-level Box-Behnken design was employed to optimize the ultrasonic power, extraction time and ratio of water to raw material to obtain a high AGP yield. The analysis of variance and response surface plots indicated that ultrasonic power was the most important factor affecting the extraction yield. The optimal conditions were ultrasonic power 400 W, extraction time 71 min, and ratio of water to raw material 33 mL g-1. Under these conditions, the yield of AGP was 8.09%, which was agreed closely to the predicted value. Gas chromatography （GC） analysis showed that AGP was composed of arabinose, rhamnose, galactose, glucose, and galacturonic acid. Fourier transform infrared spectra revealed the general characteristic absorption peaks of AGP. In addition, AGP exhibited good immunostimulating activities by up-regulating the production of nitric oxide and cytokines. Compared with hot water extraction, UAE required shorter extraction time and gave a higher extraction yield, without changing the structure and immunostimulating activity of AGP. The results indicated that UAE could be an effective and advisable technique for the large scale production of plant polysaccharides.

Antioxidant and hepatoprotective effects of Ajuga nipponensis extract by ultrasonic-assisted extraction

Objective: To investigate suitable condition for extraction of the active components from Ajuga nipponensis(A. nipponensis). Methods: Orthogonal experimental design was used to determine the optimal extraction parameters for ecdysterones and flavonoids. Finally, the hepatoprotective abilities of A. nipponensis extracts were evaluated by CCl_4-induced animal models. Results:Maximum yields of flavonoids(7.87±0.10) mg/g and ecdysterones(0.73±0.02) mg/g could be obtained when the extraction time was 50 min, the extraction temperature was 60 ℃, and the ratio of sample to 70%(v/v) ethanol was 1:20(w/w). The antioxidant property of A. nipponensis was correlated to the concentration of its extracts. At 5 mg/m L, A. nipponensisextract scavenged 84.8% of DPPH radical and had absorbance values of 2.43±0.04 reducing power. Upon CCl_4-induced liver injury, glutamic oxaloacetic transaminase and glutamic pyruvic transaminase decreased significantly after the mice were treated with A. nipponensis. Histological researches also explained that A. nipponensis reduced the extent of liver lesions induced by CCl_4. Conclusions: A. nipponensis exhibited potent antioxidant activity in chemical experimental models and hepatoprotective effect against CCl_4-induced liver damage.

Salting-Out Assisted Liquid-Liquid Extraction Combined with HPLC for Quantitative Extraction of Trace Multiclass Pesticide Residues from Environmental Waters

In this study, salting-out assisted liquid-liquid extraction combined with high performance liquid chromatography diode array detector (SALLE-HPLC-DAD) method was developed and validated for simultaneous analysis of carbaryl, atrazine, propazine, chlorothalonil, dimethametryn and terbutryn in environmental water samples. Parameters affecting the extraction efficiency such as type and volume of extraction solvent, sample volume, salt type and amount, centrifugation speed and time, and sample pH were optimized. Under the optimum extraction conditions the method was linear over the range of 10 - 100 μg/L (carbaryl), 8 - 100 μg/L (atarzine), 7 - 100 μg/L (propazine) and 9 - 100 μg/L (chlorothalonil, terbutryn and dimethametryn) with correlation coefficients (R2) between 0.99 and 0.999. Limits of detection and quantification ranged from 2.0 to 2.8 μg/L and 6.7 to 9.5 μg/L, respectively. The extraction recoveries obtained for ground, lake and river waters were in a range of 75.5% to 106.6%, with the intra-day and inter-day relative standard deviation lower than 3.4% for all the target analytes. All of the target analytes were not detected in these samples. Therefore, the proposed SALLE-HPLC-DAD method is simple, rapid, cheap and environmentally friendly for the determination of the aforementioned herbicides, insecticide and fungicide residues in environmental water samples.

Ultrasonic wave extraction and simultaneous analysis of polycyclic aromatic hydrocarbons (PAHs) and phthalic esters in soil

A method is developed for detection of polycyclic aromatic hydrocarbons(PAHs) and Phthalic Acid Esters(PAEs) in soil samples. Ultrasonic Wave Extraction under airtight circumstances is adopted to extract the analytes in soil samples with n-hexane–acetone(V:V=1:1) as extraction solvent. This method has several advantages, including high extraction efficiency, short time, convenience and simplicity. It can be used to detect polycyclic aromatic hydrocarbons(PAHs) and Phthalic Acid Esters(PAEs) in soil.

Isolation and purification of carbazole contained in anthracene slag by extraction combined with medium pressure liquid chromatography

Ultrasonic-assisted extraction(UAE)combined with medium pressure liquid chromatography(MPLC)was designed for carbazole separation from anthracene slag(AS).The effects of liquid/solid ratio,temperature,and extraction times on carbazole separation were investigated.When using CC14 and ethyl acetate as extraction solvents and combining with MPLC,carbazole recovery and purity are 75.1%and 95.4%,respectively.The mechanism for carbazole separation were presumed by examining intermolecular interactions such as N-H…π,π-π,and C-Cl…πinteractions.These results demonstrate that UAE/MPLC has a considerable potential as a green and promising strategy for separating and purifying carbazole and other chemicals from AS.

Determination of Lignans in Schisandra sphenanthera and Schisandra chinensis Using Ionic Liquid-based Ultrasonic-assisted Extraction and High-performance Liquid Chromatography

A green, rapid and precise sample pretreatment technique, IL-based UAE（ionic liquid-based ultrasonic- assisted extraction）, was coupled with high-performance liquid chromatographic separation to identify the main effective components in Schisandra sphenanthera（S, sphenanthera） and Schisandra chinensis（S, ehinensis） including schisantherin A, schisandrin A, and deoxyschizandrin. Four different types of ionic liquids have been investigated, finally [C6MIM][BF4] was used as the extraction solvent. A powder form of S. sphenanthera and S. chinensis was mixed with the [C6MIM][BF4] to produce a suspension. This suspension was ultrasonically extracted in a water bath at room temperature. Several of the process parameters were optimized, including the type of ionic liquid used and its volume, the sample amount, the size of the sample particle, the extraction time, etc. HPLC calibration curves were estab-lished for all the analytes and proved to be linear（r〉0.9999）. The lowest detection level for schisandrin A was 0.12μg/mL, for schisantherin A was 0.08 μg/mL, and for deoxyschizandfin was 0.10μg/mL. The recoveries of the target compounds were from 74.19% to 109.33%. The standard deviations for detection were generally no more than 6.31%. In contrast to conventional extraction methods, the IL-based UAE did not involve volatile organic volatile solvents, and the analysis time, required sample and solvent vohtrnes were also lower than those of the conventional techniques.

萝卜叶多酚的超声波辅助提取工艺优化及抗氧化活性研究

为提高萝卜叶资源的利用率,并发掘其潜在应用价值,探究了萝卜叶多酚的超声波辅助提取工艺,并对其抗氧化活性进行了评估。通过在单因素实验基础上引入Box-Behnken响应面法,对萝卜叶多酚的超声波辅助提取工艺进行了优化。通过体外实验的评估,进一步验证了其抗氧化能力。结果表明,在超声温度为68℃、液料比为32 mL/g、乙醇体积分数为63%以及超声时间为31 min的最佳工艺条件下,萝卜叶多酚可以被高效地提取,其提取率达到了60.84 mg/g,且相对误差低至0.73%,充分证实了响应面分析方法优化该提取工艺的有效性和可行性。萝卜叶多酚展现出一定的抗氧化特性,对DPPH自由基、O_(2)^(-)自由基的半抑制质量浓度(half maximal inhibitory concentration,IC_(50))分别为78.91、403.55 mg/L,为进一步研发其作为天然植物源抗氧化剂提供了参考。

超声辅助水剂法提取硅藻土中玉米蜡脂的工艺优化

为了提高玉米油精炼的附加值,并实现硅藻土的可循环利用,以玉米油精炼副产物含蜡脂的硅藻土为原料,采用超声辅助水剂法提取玉米蜡脂,考察了不同提取条件对玉米蜡脂提取率的影响,并通过响应面法优化玉米蜡脂提取的工艺条件。结果表明:超声辅助水剂法提取玉米蜡脂的最佳工艺条件为超声功率480 W、超声时间4 h、提取温度95℃、料液比1∶3,在此条件下玉米蜡脂提取率为(59.46±0.91)%。综上,超声辅助水剂法可以有效提取硅藻土中的玉米蜡脂。

金花葵花黄酮超声辅助提取工艺优化及性能

以金花葵花为原料,采用超声辅助提取法提取了金花葵花黄酮,通过单因素实验和正交实验优化了提取工艺,评估了最佳工艺条件下提取的金花葵花黄酮的抗氧化活性及安全性。结果表明,金花葵花黄酮最佳提取工艺为:料液比(g∶m L)1∶15、体积分数80%的乙醇水溶液为溶剂、超声功率300 W、超声时间35 min、提取温度75℃,在该条件下,金花葵花黄酮提取率为89.97%。质量浓度为1.00 g/L金花葵花黄酮对1,1-二苯基-2-苦基苯肼自由基、羟基自由基和2,2’-联氮-双(3-乙基-苯并噻唑-6-磺酸)自由基的清除率最高,分别为94.81%、95.24%、82.80%;对三者的半数抑制质量浓度(IC_(50))分别为106.00、70.06和213.80μg/m L。金花葵花黄酮质量浓度≤0.4 g/L时,其对红细胞溶血率均<10%,属于轻度刺激;质量浓度为1.00 g/L的金花葵花黄酮对鸡胚绒毛尿囊膜无溶血。

响应面优化超声辅助乙醇提取银杏叶莽草酸工艺

以银杏干叶为试材,采用超声辅助70%乙醇提取莽草酸,通过单因素试验和响应面试验优化提取工艺,研究了料液比、提取温度、提取时间、提取次数对莽草酸提取得率的影响,优化了银杏叶莽草酸的最佳提取工艺,以期为银杏叶莽草酸的提取提供参考依据。结果表明:最佳工艺条件为料液比1∶8 g·mL^(-1),提取温度66℃,提取时间65 min(每提取1次),提取次数2次。该条件下测得银杏叶莽草酸提取得率量为1.805%,与理论得率(1.883%)接近。

超声辅助低共熔溶剂法提取太白贝母总黄酮及其抗氧化活性研究

采用超声辅助低共熔溶剂法提取太白贝母总黄酮,以太白贝母总黄酮提取率为考察指标,通过单因素实验和响应面法对提取工艺进行了优化,并通过DPPH自由基清除实验和ABTS自由基清除实验研究了其抗氧化活性。结果表明,在超声功率为69 W、料液比为1∶18(g∶mL)、超声温度为79℃、超声时间为27 min的最优工艺条件下,太白贝母总黄酮提取率可以达到17.7004%,与预测值相差极小;太白贝母总黄酮是一种强抗氧化剂,对DPPH自由基、ABTS自由基具有较强的清除能力,在浓度为16 mg·mL^(-1)时,清除率分别达到82.15%、90.42%,与VC无明显差异。超声辅助低共熔溶剂法操作简便、提取率高,适用于太白贝母总黄酮的提取。该研究为太白贝母药材资源的开发利用提供了参考。

利用响应面分析技术提升桑椹多酚超声提取得率研究

目的优化超声提取桑椹多酚的方法以增加桑椹中多酚类物质的提取得率。方法以多酚提取得率为考查指标,通过单因素和响应面法的结合探索桑椹多酚超声提取工艺,考察液料比、超声功率和乙醇体积分数等关键因素,利用福林酚试剂法测定收集的10批次桑椹样品中多酚含量。结果超声提取桑椹多酚的最佳工艺条件是60%乙醇体积分数、36 mL/g液料比、350 W超声功率和30 min超声提取时间,此条件下桑椹多酚提取得率最高可达2.86%;不同产地桑椹样品多酚含量存在差异,山东、北京和四川3地收集的桑椹样品中多酚含量较高。结论本研究优化了桑椹多酚的超声提取工艺,操作简单,用时短,有机试剂用量少,多酚类物质提取得率较高,为桑椹多酚的开发提供了实验参考。

超声波辅助低共熔溶剂提取荞麦壳中总黄酮的工艺研究

以荞麦壳为原料,采用超声波辅助低共熔溶剂提取荞麦壳中总黄酮。实验对低共熔溶剂(DES)的种类、摩尔比、含水量进行了筛选,在此基础上优化了超声提取工艺条件。结果表明,用摩尔比为1∶2的氯化胆碱/乙二醇合成的低共熔溶剂,当DES含水量为30%、液料比为30∶1(mL∶g)、超声温度为70℃、超声时间为40min时,总黄酮提取得率为8.26mg·g^(-1),高于传统醇提得率。此工艺绿色温和,适用于荞麦壳中总黄酮的高效提取,研究为植物源废弃物中天然产物的提取提供了新技术。

锦灯笼果实总黄酮超声辅助提取工艺研究

锦灯笼果实中黄酮类化合物具有抗肿瘤、抗氧化、抗菌、抗炎等生物活性。以锦灯笼果实为原料,乙醇溶液为提取剂,锦灯笼果实总黄酮得率为评价指标,采用超声波辅助乙醇溶剂提取法,分别对超声功率、提取温度、提取时间、乙醇体积分数、料液比进行单因素影响试验。在单因素实验基础上,结合正交试验优化工艺参数。结果表明:影响锦灯笼果实总黄酮提取效果因素的主次顺序为提取时间>乙醇体积分数>超声功率>料液比。在提取温度50℃、提取时间30 min、乙醇体积分数70%和液料比为1∶30的条件下,锦灯笼果实总黄酮得率为3.32%。

芦苇叶中总酚提取工艺及抗氧化性研究

以河北衡水湖芦苇叶为原料,选取超声波辅助法对其中的总酚进行提取测定。通过单因素实验探究了超声温度、乙醇浓度、超声时间和料液比对总酚得率的影响。在单因素实验基础上,结合响应面分析法优化提取工艺。分析实验数据得出:超声温度为48℃、体积分数为49%的乙醇溶液、超声时间为24 min、料液比为1∶67(mg/mL)时,总酚得率最高。抗氧化性实验表明:芦苇多酚具有一定的还原能力,且对自由基的清除能力与其浓度成正比。

瓶尔小草总黄酮提取工艺优化及不同采收期含量变化规律研究

探究瓶尔小草的最佳采收时期,优化瓶尔小草总黄酮的提取工艺,并评价其体外抗氧化活性。以总黄酮含量为考察指标,对乙醇浓度、料液比、超声时间、提取温度进行单因素实验,并结合响应面法设计优选超声波辅助提取工艺。结果表明:瓶尔小草总黄酮的最优工艺条件为超声提取温度为40℃,乙醇浓度为65%,料液比为1∶30(g/mL),超声时间为35 min;一年中瓶尔小草的总黄酮含量变化存在两个富集期,最佳采收期为8月,其次4月份也较为适宜采收。以维生素C为对照,瓶尔小草黄酮提取物对DPPH自由基、ABTS^(+)自由基清除率分别可达94.76%和98.33%,瓶尔小草总黄酮的总还原能力测定IC_(50)为0.0157 mg/mL,说明瓶尔小草总黄酮具有良好的体外抗氧化活性。本研究为瓶尔小草的采收、开发利用提供了试验依据。

超声辅助-GC-MS联用分析斯里兰卡桂叶油挥发性成分

采用超声辅助萃取结合气相色谱-质谱联用法(Gas chromatography-mass spectrometry,GC-MS)分析斯里兰卡桂叶油中挥发性成分。结果表明,①斯里兰卡桂叶油中共检测出32种挥发性成分,包含烯烃类、酚类、酯类、醇类、醛酮类、杂环类化合物;②其中酚类化合物总含量最高,为23.05 mg/g,占总挥发性物质的81.10%;③斯里兰卡桂叶油中含量较高的物质为丁香酚(23.05 mg/g)、苯甲酸苄酯(1.04 mg/g)、芳樟醇(0.53 mg/g)、氧化石竹烯(0.43 mg/g)、反式肉桂醛(0.15 mg/g)。

啤酒糟多酚的提取及抗氧化活性测定

以啤酒糟为原料,在单因素试验的基础上,采用正交试验优化超声辅助乙醇提取啤酒糟中多酚的工艺,并对粗提物进行了抗氧化性能测定。结果表明:啤酒糟多酚的最佳提取工艺为乙醇浓度60%、料液比1∶60、超声功率320 W、超声时长50 min,此条件下多酚得率为5.26 mg/g。啤酒糟多酚具有较强的抗氧化能力,当质量浓度为80μg/mL时,其羟自由基清除率为80.72%、DPPH自由基清除率为54.80%。

白丁香花多糖的提取、纯化及抗氧化活性研究

采用酶辅助超声提取法提取白丁香花多糖,利用响应面试验(RSM)法系统分析了不同实验条件对白丁香花多糖得率的影响。将粗多糖经DEAE-52纤维素柱和Sephadex G-100凝胶柱层析进行纯化,用高效凝胶渗透色谱法(HPGPC)、离子色谱法(IC)、紫外光谱、傅里叶红外光谱(FTIR)和扫描电镜(SEM)对多糖的初步结构进行了表征,并进行体外抗氧化活性研究。结果表明,白丁香花多糖最佳提取工艺:超声功率150 W、超声时间40 min、超声温度40℃、加酶量(纤维素酶、中性蛋白酶)2.2%、料液比1:40 g/mL,在此条件下白丁香花多糖的得率为3.03%±0.09%。经DEAE-52纤维素柱纯化后得到4个组分的多糖,收集主要组分SP-c;再经Sephadex G-100凝胶柱纯化后得到SP-c-1组分。得出SP-c-1的单糖组成及摩尔比为半乳糖醛酸、阿拉伯糖、半乳糖、鼠李糖、葡萄糖、葡萄糖醛酸、木糖=18.39:11.13:8.96:2.61:1:0.83:0.57。SP-c-1重均分子量(Mw)为14069 Da,数均分子量(Mn)为13637 Da,具有多糖特征吸收峰,含D-葡萄吡喃糖构型。SP-c-1对DPPH、ABTS+自由基的半抑制浓度(IC_(50))分别0.87、1.355 mg/mL。SP-c-1显示出良好的抗氧化活性。

抗癌药物喜树碱的超声辅助PEG400绿色提取工艺研究

目的:建立使用表面活性剂PEG400结合超声辅助从喜树种子中提取抗癌药物喜树碱的绿色提取工艺。方法:通过对不同表面活性剂对喜树碱的溶解度的考察,确定适合喜树碱提取的表面活性剂及其最佳浓度,同时对提取过程中的液料比、超声功率、超声时间、温度进行单因素实验和正交试验。结果:采用13%的PEG400水溶液结合超声提取喜树碱的最佳工艺条件为液料比90∶1、超声功率540W、超声时间90min、温度25℃,在此条件下的喜树碱提取率为1174.59μg/g。结论:使用PEG400水溶液成功提取了喜树种子中的喜树碱,喜树碱的提取率为1174.59μg/g。