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1.
超声波辅助提取裂褶菌多糖及分离纯化的研究 总被引：1，自引：0，他引：1
本文研究了超声波辅助法分离纯化裂褶菌多糖的工艺条件。分别从超声时间、超声功率、液料比、提取时间和提取温度5个因素考察了对裂褶菌多糖提取率的影响,且在此条件下进行响应面优化。试验结果表明,在超声时间30min、超声功率200W、液料比40∶1和提取温度40℃时裂褶菌多糖提取率为69.56%。经DEAE纤维素-52色谱柱和葡聚糖凝胶G-100分离各得到2种组分,对其进行紫外-可见光光谱(UV)分析和红外光谱分析得出,裂褶菌多糖Sp G不含蛋白质或核酸,可能为含呋喃环的α构型的多糖。研究为裂褶菌多糖的开发利用提供理论依据。 相似文献
2.
为了实现竹节虾加工副产物的高值化利用,以竹节虾加工废弃物中的虾头副产物为原料,以水解度和DPPH清除率作为评价指标,采用中性蛋白酶酶解,通过响应面法优化超声辅助酶解工艺,并依次通过超滤、凝胶层析色谱和反相高效液相色谱等分离方法,从竹节虾虾头酶解产物中分离制备抗氧化肽,采用超高压液相色谱串联质谱联用技术对肽的结构进行表征。结果表明,在中性蛋白酶添加量为3 000 U·g~(-1)、p H值7.0条件下,最佳超声辅助酶解工艺参数为超声时间41 min,超声温度55℃,超声频率22 k Hz,料液比1∶9(w/v),在此条件下获得的酶解产物DPPH清除率达69.50%。当水解时间为0.5~2.5 h时,超声辅助酶解的酶解产物水解度和DPPH清除率比非超声辅助酶解工艺分别高17.95%和18.83%,该工艺缩短了酶解时间,节约了能耗。酶解产物经超滤初步分离发现,相对分子质量在3k Da(SHP4)的组分具有显著的抗氧化活性。用凝胶层析法进一步分离纯化SHP4组分后得到4个峰,其中SHP4-II的DPPH清除率最高;SHP4-II通过反相高效液相纯化后也得到4个主要肽峰,在多肽含量为1.5 mg·m L~(-1)时,SHP4-II-4的DPPH清除率最高,达到85.69%,并且具有较好的分离度,质谱分析发现,该抗氧化肽的结构为Gly-Asn-Gly-Leu-Pro(455.99 Da)。本研究结果为虾肽抗氧化保健食品的研发提供了一定的科学依据。 相似文献
3.
刺葡萄皮中花色苷的分离纯化与结构鉴定 总被引：1，自引：0，他引：1
为研究刺葡萄花色苷的结构及其纯化分离的柱层析法,将刺葡萄色素粗提液依次经大孔树脂HP-20、聚酰胺树脂、葡聚糖凝胶Sephadex LH-20吸附纯化,利用超高效液相色谱三重四级杆飞行时间质谱联用技术对分离所得花色苷进行结构鉴定,并运用荧光光度法探索荧光图谱与花色苷结构的关系。研究发现,聚酰胺树脂对部分花色苷产生了吸附作用,而Sephadex LH-20凝胶能起到较好的分离作用,最终得到3种色素,经鉴定,确定色素I为锦葵素-3,5-O-双葡萄糖苷,通过质谱信息初步确定色素III可能为锦葵素-3,5-O-双葡萄糖苷-香豆酰,色素IV可能为飞燕草素-3-O-芸香糖苷和锦葵素-3-O-芸香糖苷的混合物,经高效液相色谱以归一法计算峰面积,色素I和色素III的纯度分别达到了98.64%、98.33%,得率分别为0.114%和0.076%。研究结果为花色苷的分离及鉴定提供参考。 相似文献
4.
超声波辅助酶法提取红腰豆多糖工艺优化 总被引：4，自引：7，他引：4
为了开发利用红腰豆多糖资源,该文探讨了超声波技术协同复合酶处理提取红腰豆多糖的工艺条件并对其结构进行了初步分析。在50℃下,以多糖得率为指标,通过正交试验筛选复合酶最佳配比,利用Plackett-Burman试验设计分析各因素显著性,再采用Box-Behnken中心组合设计原理进行响应面分析优化;采用紫外和红外光谱扫描及苷键分析对红腰豆多糖结构进行初步分析。结果表明:复合酶最佳质量配比为木瓜蛋白酶∶果胶酶∶纤维素酶=3∶1∶3。酶解p H值和超声功率对提取红腰豆多糖影响达到极显著效应,复合酶添加量和超声时间为显著因素。最佳工艺参数为液料比80∶1 m L/g、复合酶添加量4.0%、酶解p H值5.0、酶解时间1.5 h、超声功率400 W、超声时间34.0 min,红腰豆多糖得率为14.15%。经紫外和红外光谱扫描表明红腰豆多糖经DEAE-52纤维素层析柱和Sephadex G-200层析柱两步纯化后纯度较高,具有多糖的特征吸收峰;通过高碘酸氧化和Smith降解分析可推测红腰豆多糖的连接方式为α(1→4)和(1→6)连接。研究结果为酶法联合超声波处理技术在红腰豆多糖提取过程中的应用及其后续红腰豆多糖结构表征、生物活性等方面的研究提供理论依据。 相似文献
5.
本文以稀HCl从蚕粉中提取1-脱氧野尻霉素（1-deoxynojirimycin,1-DNJ）,通过单因素试验确定提取影响因素的水平,并采用响应面法研究料液比分数、浸提温度和浸提时间对蚕粉1-DNJ提取工艺的影响。其中1-DNJ含量测定采用9-芴基氯甲酸甲酯（FMOC-Cl）衍生化法,并用反相高效液相色谱对其衍生物进行测定。1-DNJ高效液相色谱检测谱图表明,通过液相色谱荧光可以检测蚕粉来源的1-DNJ。响应面优化实验结果表明,1-DNJ的最佳提取条件为：提取时间3.3h,浸提温度72.9℃,料液比分数为1：282。在此条件下,1-DNJ的理论提取率为0.493%,实际提取率为0.487%,相对误差为1.2%。本研究初步建立了稀酸浸提家蚕1-DNJ的二次多项数学模型,确定其最佳提取工艺条件,为工业化生产提供参考。 相似文献
6.
7.
荔枝低分子量多糖的分离纯化及抗氧化吸湿保湿性能分析 总被引：2，自引：1，他引：1
为进一步开发和利用荔枝中的多糖成分,该文对荔枝低分子量多糖组分进行分离纯化,并对其理化性质、抗氧化和吸湿保湿性进行研究。采用超声波辅助提取、分级醇沉、DEAE-cellulose 52和Sephadex G-100柱分离纯化荔枝多糖;紫外-可见光谱扫描法、比旋光度法、渗透凝胶色谱法3种方法验证纯度;高效凝胶渗透色谱法测定相对分子量,高效阴离子交换色谱测定单糖组成;清除DPPH自由基和羟基自由基评价体外抗氧化活性;体外法测定吸湿保湿性。结果表明:荔枝多糖经分离纯化后获得组分荔枝多糖PLC-1,经3种方法验证PLC-1为精多糖,相对分子量为2.35×104 Da,是由半乳糖、鼠李糖、葡萄糖组成,摩尔比为:1.00∶3.52∶5.89。抗氧化活性研究结果表明PLC-1对DPPH和羟基自由基呈良好的量效关系,半数清除浓度IC50分别为0.41和0.31 mg/m L。吸湿保湿性的结果表明,PLC-1具有良好的吸湿和保湿性,在32 h时的吸湿率为58.3%,32 h时的失水率为45.3%,荔枝多糖PLC-1为具抗氧化和吸湿保湿活性的多糖,研究结果可为荔枝的深加工和进一步研究开发提供一定的理论基础。 相似文献
8.
为提高对蛋黄卵磷脂(PC)的提取率,该文利用高压脉冲电场(PEF)辅助有机溶剂来进行提取试验。试验选定了影响PC提取率的3个主要因素:PEF场强、脉冲数和提取溶剂含水率,并采用Box-Behnken试验设计对提取工艺进行优化;并且,通过中红外光谱扫描分析了经PEF处理前后的PC分子结构变化。结果表明:PC提取的最佳工艺条件为场强39kV/cm,脉冲数31,提取溶剂含水率9%,其PC提取率比无PEF处理的传统有机溶剂提取法提高了10.2%;PEF对PC分子结构并没有显著影响,证实了PEF对食品营养成分破坏少,是一种温和的处理方式。该研究可为PEF技术应用于蛋黄卵磷脂的提取提供参考。 相似文献
9.
中国传统细菌型豆豉溶栓酶的提取纯化技术研究(简报) 总被引：1，自引：0，他引：1
为深入开发利用中国传统发酵细菌型豆豉溶栓酶,对豆豉溶栓酶分离纯化工艺进行了研究探讨,确认了最佳的纯化条件:首先用饱和度75%的硫酸铵沉淀豆豉溶栓酶;然后利用DEAE-Sepharose FF (Diethylaminoethyl Sepharose Fast Flow,二乙基氨基琼脂糖快速凝胶)阴离子交换柱进行层析,优化的层析条件为用10 mmol/L Tris(Trishydroxymethylaminomen,三羟甲基氨基甲烷)-HCI (pH 8.7)作为上样缓冲液,采用线性梯度洗脱,洗脱液为10mmol/L Tris-HCI(pH 8.7)和0.6mol/LNaCl,洗脱流速为1 mL/min;最后经过Sephadex G-75(葡聚糖凝胶G-75)凝胶过滤,得到纯化倍数为11.29倍的豆豉溶栓酶.利用SDS-PAGE (Sodium dodecyl sulphate-polylamide gel electroresis,十二烷基硫酸钠-聚丙烯酰胺凝胶电泳) 显示经纯化后的酶无杂蛋白,初步鉴定其分子量接近31 ku. 相似文献
10.
无花果多糖提取工艺优化及其超声波改性 总被引：6，自引：5，他引：1
为了推动无花果多糖产业发展,探讨无花果多糖分子修饰对其活性的影响,采用传统水提醇沉的方法和响应面设计法优化无花果多糖提取技术,进而对超声波修饰前后的无花果多糖进行抗氧化活性分析和分子结构表征,研究无花果多糖的提取技术及其超声波修饰效应。响应面试验结果表明其最佳提取条件为提取时间21 min、提取温度90℃、液料比49 mL/g,在此条件下无花果多糖第1次提取率达到3.03%,经过2次提取,多糖提取率和得率分别达到3.86%和94.62%。中红外光谱分析表明,超声波将其分子中大量的C-O-C和C-O-H键打断;尺寸排阻色谱-多角度光散射分析,超声处理后,其数均分子量和重均分子量分别从536 800、1 061 000 Da减少到46 410、93 870 Da。进一步对超声波修饰过的无花果多糖进行分级醇沉、SephadexG-150凝胶层析纯化得到较高抗氧化活性的组分,尺寸排阻色谱-多角度光散射分析表明该组分数均分子量为58 810 Da,重均分子量为157 300 Da;气相色谱分析其单糖组成及分子摩尔比为L-鼠李糖∶D-葡萄糖∶D-半乳糖=1.63∶0.88∶1。 相似文献
11.
Pedersen ME Kolset SO Sørensen T Eggen KH 《Journal of agricultural and food chemistry》1999,47(4):1445-1452
M. semitendinosus (ST) and M. psoas major (PM) were used as models for tough and tender meat to study a possible role of sulfated glycosaminoglycans (GAGs) for muscle tenderness. The difference in texture was confirmed by Warner Bratzler shear force measurements. No significant difference in total amount of GAGs in the muscles was found. In contrast, a significant difference in the ratio of GAG/collagen was found between the two muscles. After separation of the GAGs by density gradient ultracentrifugation and ion-exchange chromatography, dermatan sulfate (DS), keratan sulfate (KS), chondroitin sulfate (CS), and heparan sulfate (HS) were identified by cellulose acetate electrophoresis after use of specific enzymes and chemical methods. The content of DS was higher in the tougher muscle (ST) than in PM, and the difference in DS content was statistically significant. Furthermore, a significant difference in the GAG composition pattern of the two muscles was found. The yield of GAGs extracted from the muscles was 77% for ST and 87% for PM. The residue after extraction was further analyzed and found to contain mainly HS. Immunohistochemical studies using antibodies against CS/DS showed a staining pattern of the perimysium of ST different from that of PM. 相似文献
12.
Tilay A Bule M Kishenkumar J Annapure U 《Journal of agricultural and food chemistry》2008,56(17):7644-7648
Ferulic acid (FA) is a phenolic antioxidant present in plants, which is widely used in the food and cosmetic industry. In the present study, various agricultural wastes such as maize bran, rice bran, wheat bran, wheat straw, sugar cane baggasse, pineapple peels, orange peels, and pomegranate peels were screened for the presence of esterified FA (EFA). Among the sources screened, maize bran was found to contain the highest amount of EFA. Pineapple peels, orange peels, and pomegranate peels were also found to contain traces of EFA. Alkaline extraction of EFA from maize bran was carried out using 2 M NaOH. Response surface methodology (RSM) was used for optimization of EFA extraction, which resulted in a 1.3-fold increase as compared to the unoptimized conventional extraction technique. FA was analyzed by means of high-performance liquid chromatography (HPLC). Purification was carried out by adsorption chromatography using Amberlite XAD-16 followed by preparative high-performance thin-layer chromatography (HPTLC). The recovery of Amberlite XAD-16 purified FA was up to 57.97% with HPLC purity 50.89%. The fold purity achieved was 1.35. After preparative HPTLC, the maximum HPLC purity obtained was 95.35% along with an increase in fold purity up to 2.53. 相似文献
13.
R K Jhangiani A C Bello 《Journal of the Association of Official Analytical Chemists》1985,68(3):523-527
A liquid chromatographic (LC) procedure is described for the assay of morphine sulfate in bulk drug material and injection solutions. The bulk drug and injection samples are prepared by direct dilution with LC mobile solvent. The average bulk drug purity (5 manufacturers) determined by the LC method was 99.9% with a difference of 0.1% from the average purity (anhydrous) found by the official USP XX procedure. The average LC recovery (19 studies) of morphine sulfate added to injection samples was 99.4% with a coefficient of variation (CV) of 1.14%. Morphine sulfate content was determined in triplicate for 53 injection samples (1-15 mg morphine sulfate/mL) formulated by 6 manufacturers, using the proposed LC procedure. Individual sample CV (n = 3) averaged 1.14%. The LC method is simple and specific for morphine sulfate. Major degradation products, preservatives, and some contaminants and related compounds are separated during LC. 相似文献
14.
Dell'Agli M Giavarini F Ferraboschi P Galli G Bosisio E 《Journal of agricultural and food chemistry》2007,55(9):3363-3367
This work describes a sensitive high-performance liquid chromatography (HPLC) method for the quantification of aloesin and aloeresin A in alcoholic beverages containing aloe as a flavoring agent. The compounds were prepared from Aloe ferox juice. Sephadex LH20 and ion-exchange resin AG1X2 column chromatography were used for aloesin. Aloeresin A was obtained by Sephadex LH20 and silica gel column chromatography followed by purification on Discovery DSC-18 solid-phase extraction tubes. A 98 mg amount of aloesin (>99% purity) and 34 mg of aloeresin A (>98% purity) were recovered from 2.5 g of aloe juice. The HPLC method was validated, and intra- and interday performances were established. In-house validation was carried out by analyzing samples of beverages with and without aloe as a flavoring agent. 相似文献
15.
Luchtefeld R Luo R Stine K Alt ML Chernovitz PA Smith RE 《Journal of agricultural and food chemistry》2008,56(2):301-306
Procedures based on high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection and liquid chromatography-mass spectrometry (LC-MS) are described for analyzing diapocynin. Diapocynin was synthesized by oxidative coupling of two apocynin monomers, through the in situ generation of sulfate radicals. It was purified by washing 3 times each with boiling water, followed by boiling methanol. HPLC was used to determine the concentration of unreacted apocynin and other impurities and the purity of the diapocynin that had been synthesized. Negative-ion, atmospheric pressure chemical ionization (APCI) LC-MS was used to determine the molecular weights of impurities. The method using HPLC with UV detection provided a calibration curve that was linear from 0.16 to 24 microg/mL. The LC-MS method was linear from 0.005 to 2 microg/mL. It was found that diapocynin has low solubility in deionized water and corn oil but is soluble in dimethylsulfoxide (DMSO) and alkaline aqueous solutions. Also, diapocynin is 13 times more lipophilic than apocynin, even though both compounds have the same p K a of 7.4. The log of the octanol/water partition coefficient (log P) was 1.01 for apocynin and 1.82 for diapocynin. A solution of 5.5 mg/mL (16.7 mM) diapocynin in DMSO was found to be stable for at least 30 days when stored at room temperature. 相似文献
16.
G M Hanna C A Lau-Cam 《Journal of the Association of Official Analytical Chemists》1989,72(4):552-555
Optimum experimental conditions were developed for determination of the optical purity of samples of tranylcypromine sulfate by proton magnetic resonance spectroscopy after complexation with the chiral lanthanide chelate Eu(hfc)3. At a substrate concentration of 0.25M (0.125M as sulfate) in CDCl3 and an Eu(hfc)3 to substrate molar ratio of 1, the methine proton geminal to the amino group in the cyclopropane ring showed the largest induced shift and largest enantiomeric induced shift difference. From the relative intensities of the resolved (+)-CH-NH2 protons (15.77 ppm) and (-)-CH-NH2 proton (16.04 ppm), the enantiomeric purity and percentage compositions were readily calculated. The mean +/- SD recovery of (+)-tranylcypromine sulfate from synthetic enantiomeric mixtures was 101.02 +/- 2.59 (n = 6). 相似文献
17.
1-Cyano-2-hydroxy-3-butene (crambene) is a nitrile found in cruciferous vegetables that causes significant upregulation of quinone reductase and glutathione S-transferases in vivo and in vitro, making it a likely candidate as a cancer chemopreventive compound. To investigate further the putative anticarcinogenic mechanisms of crambene, a compound of the highest possible purity is vital. Therefore, a rapid and effective method of purification of crambene is necessary to continue studies of its beneficial health effects. A rapid method to isolate and purify natural crambene from either Crambe abyssinica (crambe) seed or commercially processed crambe seed meal was developed using immiscible solvent extraction followed by high-performance liquid chromatography. Use of this methodology eliminated the need for time-consuming and relatively inefficient column chromatography, improved extraction efficiency, and resulted in higher purity than previously used methodologies. Elimination of trace amounts of fatty acid residues, unachievable with previous methodologies, also was accomplished. 相似文献
18.
Lopes-Lutz D Mudge E Ippolito R Brown P Schieber A 《Journal of agricultural and food chemistry》2011,59(2):491-494
High-speed countercurrent chromatography (HSCCC) was used for the separation of alkylamides from the roots of Echinacea angustifolia (DC.) Hell. For this purpose, the alkylamides were extracted with hexane and subjected to semipreparative HSCCC using a two-phase solvent system consisting of n-hexane, ethyl acetate, methanol, and water (4:1:2:1). The lower aqueous phase was used as the mobile phase at a flow rate of 3 mL/min and a rotary speed of 1000 rpm. This procedure led to the isolation of four pure alkylamides, that is, dodeca-2E,4E,8Z,10E/Z-tetraenoic acid isobutylamide (38.9 mg, 97% purity), dodeca-2E,4E,8Z-trienoic acid isobutylamide (4.4 mg, 92% purity), dodeca-2E,4E-dienoic acid isobutylamide (3.2 mg, 99% purity), and dodeca-2E,4E-dienoic acid 2-methylbutylamide (0.3 mg, 92% purity). The identity and purity of the isolated alkylamides were confirmed by LC-ESI-MS and (1)H NMR and (13)C NMR data. To the best of the authors' knowledge, this is the first report of dodeca-2E,4E-dienoic acid 2-methylbutylamide in E. angustifolia roots. 相似文献
19.
L M Atkins D J Miner G S Sittampalam C D Wentling 《Journal of the Association of Official Analytical Chemists》1987,70(4):610-617
An integrated approach is presented for the establishment of purified protein and peptide reference standard materials suitable for both biological and chemical assays. Preliminary considerations, handling and storage conditions, and a variety of chemical methods for defining the reference standards are examined in detail. Of the chemical methods, liquid chromatography (LC), amino acid analysis, Kjeldahl protein assay, electrophoresis, and ion chromatography are key assays in determining the potency, purity, and identity of the reference standard preparation. Finally, the role of liquid chromatography in assessing reference standards for identity and chemical purity is examined and correlated with other methods. 相似文献
20.
(35)~S-多噻烷,即(35)~S-7-二甲氨基-1,2,3,4,5-五硫环辛烷,是由Na_2~(35)SO_4制备Na_2~(35)S,进而制备Na_2~(35)SS_x,再与氯化物缩合而成,放化收率33.6％,放化纯度97％。 相似文献