淫羊藿饮片指纹识别模式的建立与评价

摘 要 目的： 建立淫羊藿饮片的综合质量评价模式,为其质量控制提供参考。方法: 通过指纹识别模式的建立,对市售淫羊藿饮片指纹峰进行双向反馈,评价淫羊藿饮片整体质量。采用HPLC Agilent ZORBAX Eclipse XDB-C₁₈(150 mm×4.6 mm,5 μm)色谱柱,乙腈-水梯度洗脱,流速：1.0 ml·min^-1,柱温：30℃。结果: 初步建立了市售淫羊藿饮片HPLC指纹图谱,确定共有峰16个,市售淫羊藿饮片整体被分为两类,并且两类质量相差较大。结论:建立淫羊藿饮片指纹图谱的11批饮片相似度相差较大,不同产地、采集时间等因素对淫羊藿饮片整体质量影响较大。指纹评价模式能很好的反应出中药饮片质量的整体趋势,适合多成分中药及其制剂的综合质量评价。     

正交试验优选微波辅助提取淫羊藿中淫羊藿苷的工艺

目的:优选微波辅助提取淫羊藿中淫羊藿苷的工艺。方法:设计L(34)正交试验,以辐射温度、辐射时间、乙醇浓度、料液9比倍数为考察因素,以淫羊藿苷含量为考察指标,优选微波辅助提取淫羊藿中淫羊藿苷的工艺。结果:淫羊藿苷的最佳提取工艺为辐射温度60℃、提取时间6min、乙醇浓度30%和料液比1∶20。结论:用本方法提取淫羊藿苷,效率高、时间短、成本低。     

淫羊藿中淫羊藿苷提取工艺研究

目的:优选淫羊藿中淫羊藿苷的提取工艺。方法:以淫羊藿苷提取转移率为考察指标,对不同提取方法和提取条件进行考察。结果:最佳提取工艺为采用渗漉法,用60%～75%乙醇作溶媒,收集渗漉液的量为药材的8倍。此时,淫羊藿苷提取转移率为90%。结论:该提取工艺效率高、节约能源,方法可行。     

淫羊藿提取工艺研究

目的：研究淫羊藿提取工艺。方法：以淫羊藿甙含量作为检测指标,选用L9(34)正交试验表安排试验。结 果：水煎法与醇提法提取效果相近。结论：淫羊藿采用水煎法,工艺简便,成本低,提取效率高,是较理想的生产工 艺。     

乳疾灵颗粒辐照前后淫羊藿苷含量变化研究

摘 要 目的： 对比乳疾灵颗粒辐照前后淫羊藿苷含量差异。方法: 采用HPLC色谱法,色谱柱为Thermo ODS-2 HYPERSIL色谱柱(250 mm×4.6 mm,5 μm);流动相为乙腈-0.033 mol·L^-1磷酸二氢钾(30∶70);检测波长为265 nm;流速为1.0 ml·min^-1;柱温30℃。结果:淫羊藿苷在浓度3.44～34.40 μg·ml^-1范围内呈现良好的线性关系,r=0.999 7(n=6);平均回收率为98.18%,RSD=0.32%。乳疾灵颗粒辐照前后淫羊藿苷含量变化差异无统计学意义(P>0.05)。结论: 常规剂量照射处理对乳疾灵颗粒中淫羊藿苷影响较小。     

淫羊藿不同提取物的体外抑菌实验研究

摘 要 目的：考察淫羊藿不同提取物的体外抑菌作用。方法: 采用倍比稀释法考察淫羊藿不同提取物对金黄色葡萄球菌、大肠埃希菌、白色念珠菌和枯草芽孢杆菌的抑菌作用,测定抑菌圈大小、最小抑菌浓度（MIC）和最低杀菌浓度（MBC）。结果: 淫羊藿提取物对金黄色葡萄球菌、大肠埃希菌、白色念珠菌和枯草芽孢氏菌均呈现不同程度的抑菌能力,水提物的抑菌能力强于醇提物（P<0.05或P<0.01）;水提物经过不同温度热处理后对各菌株的抑菌能力无显著差异（P>0.05）,醇提物经高温处理后抑菌能力呈下降趋势,温度越高抑菌能力越弱（P<0.05）。淫羊藿水提物对金黄色葡萄球菌、大肠埃希菌、枯草芽孢杆菌的MIC和MBC相同,分别为7.81,1.95,31.25 mg·mL^-1,白色念珠菌的MIC和MBC分别为15.63,31.25 mg·mL^-1;淫羊藿醇提物对金黄色葡萄球菌、大肠埃希菌、枯草芽孢杆菌、白色念珠菌的MIC和MBC相同,分别为15.63,3.91,62.5,62.5  mg·mL^-1。结论:淫羊藿提取物具有明显的抑菌效果,其中水提物优于醇提物。淫羊藿不同化学成分的极性会对抑菌效果产生影响。     

Box-Behnken设计响应面法优选水杨梅总黄酮提取工艺研究

摘 要 目的： 采用Box Behnken设计响应面法优化水杨梅的最佳提取工艺。方法: 以水杨梅中总黄酮含量为评价指标,通过单因素试验分别考察乙醇浓度、液料比、提取时间三个因素对总黄酮含量的影响,采用Box Behnken设计响应面法对水杨梅的提取工艺参数进行优化。结果: 水杨梅的最佳提取工艺：乙醇浓度为 50%,液料比为4.2倍,提取时间为80 min,在该条件下平均提取量12.590 0 mg·g^-1。结论:Box Behnken设计响应面法优化水杨梅总黄酮提取工艺合理,建立的数学模型和试验数据相符,具有较好的预测性。     

黄麦合剂中淫羊藿苷、二苯乙烯苷、金丝桃苷的稳定性考察

摘 要 目的：考察黄麦合剂中淫羊藿苷、二苯乙烯苷、金丝桃苷的稳定性。方法: 以黄芪甲苷、巴戟天药材的TLC鉴别试验,以及淫羊藿苷、二苯乙烯苷、金丝桃苷的HPLC色谱法含量测定为指标,考察黄麦合剂在加速试验及长期试验条件下的稳定性。结果: 在加速试验及长期试验条件下,黄芪甲苷、巴戟天药材以及淫羊藿苷具有良好的稳定性;二苯乙烯苷、金丝桃苷在加速试验、长期试验条件下稳定性差。结论:黄麦合剂各成分中二苯乙烯苷、金丝桃苷稳定性不佳,应尝试改造成固体剂型,以保证稳定性。     

补肾温肺微乳中淫羊藿苷的大鼠在体肠吸收特征研究

摘 要 目的： 研究补肾温肺微乳中淫羊藿苷的大鼠不同肠段的吸收特性,并考察P 糖蛋白( P gp)对其肠吸收的影响。方法: 采用大鼠在体单向肠灌流实验,采用HPLC法测定淫羊藿苷的含量,分别研究肠段不同吸收部位、不同淫羊藿苷浓度、 P gp抑制药维拉帕米对淫羊藿苷单体及其在补肾温肺微乳中吸收的影响。结果: 淫羊藿苷单体在各肠段的吸收速率常数(Ka)和表观吸收系数(P_app)差异显著(P<0.01);在0.10～0.40 ml·min^-1流速内和0.1～1.0 mg·ml^-1质量浓度内,十二指肠吸收速率常数和表观吸收系数无显著差异;补肾温肺微乳中淫羊藿苷的肠灌流试验结果与淫羊藿苷单体相比略小,但无显著差异; P gp抑制药对淫羊藿苷的肠吸收有影响,加入0.1 mmol·L^-1盐酸维拉帕米后,Ka和P_app分别为（2.13±0.66）×10^-2h·cm^-1和（0.23±0.051）×10^-6 cm·s^-1,与不加P gp 抑制药组相比较差异显著(P<0.01)。结论: 淫羊藿苷属于难吸收化合物,淫羊藿苷和补肾温肺微乳中淫羊藿苷在大鼠不同肠段的吸收具有相似的吸收特性;其在大鼠肠内的吸收受 P gp外排转运影响。因此,推测淫羊藿苷可能是P gp的底物。     

基于网络药理学的淫羊藿治疗阿尔茨海默病作用机制研究

目的 基于网络药理学,探讨淫羊藿治疗阿尔茨海默病（Alzheimer’s disease,AD）的作用靶点及通路,明确其作用机制。方法 借助TCMSP数据库及Uniprot数据库筛选出淫羊藿有效成分及靶点基因。通过Drugbank、Dis Ge NET和TTD数据库筛选出AD的靶点基因;成分靶点与疾病靶点映射后使用Cytoscape 3.7.1软件构建药物有效成分-靶点蛋白相互作用网络,使用STRING数据库绘制靶点蛋白-靶点蛋白相互作用网络;对靶点蛋白利用Metascape数据库进行GO分析和KEGG分析,最后采用MTT试验和荧光实时定量PCR对网络药理学主要分析结果进行验证。结果 筛选得到23个淫羊藿活性成分,共预测获得239个淫羊藿药效靶点和2 156个AD的治疗靶点,取交集后得到152个淫羊藿治疗AD的靶点,蛋白互作分析提示GSK3β、AKT1、CDK5、CDK5R1、APP、MAPK1、MTOR为蛋白互作网络中的关键靶点。淫羊藿关键靶点主要关联AD、β-淀粉样蛋白聚集、tau蛋白异常磷酸化、炎症反应、氧化应激、细胞凋亡等;细胞实验提示,淫羊藿可显著提高Aβ_25-35诱导PC12细胞的细胞存活率,并参与调控GSK-3β、AKT1、CDK5介导的β-淀粉样蛋白聚集及tau蛋白磷酸化通路。结论 淫羊藿治疗AD具有多活性成分-多作用靶点-多联系通路的特点,本研究为系统阐明淫羊藿治疗AD作用机制提供了科学依据。     

正交试验优选益气固脱颗粒醇提工艺研究

摘 要 目的： 优选益气固脱颗粒醇提工艺。方法: 以正交设计的试验方法,对组方中有效成分黄芪甲苷、阿魏酸用HPLC法进行定量分析,选取L₉(3⁴)正交表,考察乙醇浓度、乙醇用量、提取次数、提取时间等工艺参数对益气固脱颗粒提取量的影响。结果:方差分析表明,乙醇浓度与提取次数对浸出物的含量及阿魏酸的提取有显著影响。最佳醇提工艺即加10倍量的70%的乙醇,提取3次,每次1.5 h。结论: 该工艺稳定可行,适于工业生产。     

Optimization of extraction conditions for osthol,a melanogenesis inhibitor from Cnidium monnieri fruits

Context: Coumarin derivatives have been reported to inhibit melanin biosynthesis.

Objective: The melanogenesis inhibitory activity of osthol, a major coumarin of the fruits of Cnidium monnieri Cusson (Umbelliferae), and optimized extraction conditions for the maximum yield from the isolation of osthol from C. monnieri fruits were investigated.

Materials and methods: B16F10 melanomas were treated with osthol at concentration of 1, 3, and 10?μM for 72 h. The expression of melanogenesis genes, such as tyrosinase, TRP-1, and TRP-2 was also assessed. For optimization, extraction factors such as extraction solvent, extraction time, and sample/solvent ratio were tested and optimized for maximum yield of osthol using response surface methodology with the Box–Behnken design (BBD).

Results: Osthol inhibits melanin content in B16F10 melanoma cells with an IC₅₀ value of 4.9?μM. The melanogenesis inhibitory activity of osthol was achieved not by direct inhibition of tyrosinase activity but by inhibiting melanogenic enzyme expressions, such as tyrosinase, TRP-1, and TRP-2. The optimal condition was obtained as a sample/solvent ratio, 1500?mg/10 ml; an extraction time 30.3 min; and a methanol concentration of 97.7%. The osthol yield under optimal conditions was found to be 15.0?mg/g dried samples, which were well matched with the predicted value of 14.9?mg/g dried samples.

Conclusion: These results will provide useful information about optimized extraction conditions for the development of osthol as cosmetic therapeutics to reduce skin hyperpigmentation.     

多指标综合评分法优化痛风巴布剂的醇提工艺

目的 优选痛风巴布剂的最佳提取工艺。方法 以青藤碱、总生物碱的含量和干浸膏得率为评价指标,采用正交设计试验,考察乙醇浓度、乙醇用量、提取时间和提取次数对提取结果的影响,确定痛风巴布剂处方药材的最佳提取工艺。结果 痛风巴布剂的最佳提取工艺为65%乙醇,提取3次,每次6倍量溶剂,提取总时间为1.5 h,在该工艺条件下得到的青藤碱含量、总生物碱含量和干浸膏得率分别为2.79 mg·g^-1、1.22%和13.06%。结论 优选的醇提工艺稳定、可行。     

黄麦颗粒制备工艺研究

摘 要 目的： 研究黄麦颗粒的制备工艺,确定最佳工艺条件。方法: 采用单因素筛选法和正交设计法,进行提取工艺和成型工艺优选。结果:最佳工艺为处方量的7味药材,加8倍量水,煎煮2 h,提取3次,合并水提液,减压浓缩、干燥成干浸膏。干膏粉与适量糊精混合均匀后,加40%乙醇湿法制粒,干燥后整粒,即得。结论: 所选工艺科学、合理、稳定,适合工业化生产。     

银屑净提取工艺的优化

优选银屑净的最佳提取工艺。方法：采用正交试验法,选择回流时间、回流次数、乙醇浓度、乙醇用量为考察因素,以大黄素、蛇床子素含量为评价指标,进行银屑净的工艺优化。结果：最佳提取工艺为8倍药材量的80％浓度乙醇回流2次,每次2h。结论：优选工艺稳定可行,可作为实际生产工艺。     

Microencapsulation of Theobroma cacao L. waste extract: optimization using response surface methodology

The cocoa extract (Theobroma cacao L.) has a significant amount of polyphenols (TP) with potent antioxidant activity (AA). This study aims to optimise microencapsulation of the extract of cocoa waste using chitosan and maltodextrin. Microencapsulation tests were performed according to a Box–Behnken factorial design, and the results were evaluated by response surface methodology with temperature, maltodextrin concentration (MD) and extract flowrate (EF) as independent variables, and the fraction of encapsulated TP, TP encapsulation yield, AA, yield of drying and solubility index as responses. The optimum conditions were: inlet temperature of 170?°C, MD of 5% and EF of 2.5?mL/min. HPLC analysis identified epicatechin as the major component of both the extract and microparticles. TP release was faster at pH 3.5 than in water. These results as a whole suggest that microencapsulation was successful and the final product can be used as a nutrient source for aquatic animal feed.

• Highlights

• Microencapsulation is optimised according to a factorial design of the Box–Behnken type.

• Epicatechin is the major component of both the extract and microcapsules.

• The release of polyphenols from microcapsules is faster at pH 3.5 than in water.

     

Enhanced ultrasound-assisted enzymatic hydrolysis extraction of quinolizidine alkaloids from <Emphasis Type="Italic">Sophora alopecuroides</Emphasis> L. seeds

Quinolizidine alkaloids are the main bioactive components in Sophora alopecuroides L. This study reports a novel ultrasound-assisted enzymatic hydrolysis method for the extraction of these important alkaloids. Box–Behnken design, a widely used response surface methodology, was used to investigate the effects of process variables on ultrasound bath-assisted enzymatic hydrolysis (UAEH) extraction. Four independent variables, pH, extraction temperature (°C), extraction time (min) and solvent-to-material ratio (mL/g), were studied. For the extraction of sophocarpine, oxysophocarpine, oxymatrine, matrine, sophoramine, sophoridine and cytisine, the optimal UAEH condition was found to be a pH of 5, extraction temperature of 54 °C, extraction time of 60 min and solvent-to-material ratio of 112 mL/g. The experimental values obtained under optimal conditions were fairly consistent with the predicted values. UAEH extraction was then compared with reflux heating, enzymatic extraction and ultrasound-assisted extraction. Of these extraction methods, UAEH extraction under optimal conditions produced the highest yield for seven types of alkaloids. In addition, UAEH extraction resulted in lower ingredient degradation than reflux heating extraction.     

三七醇回流法与超声法提取工艺比较研究

目的:优选三七药粉醇回流法提取与醇超声法提取最优工艺参数;探讨三七药粉超声提取的可行性,为工业化生产提供依据.方法:以三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1及三种皂苷总和的含量为评价指标,首先采用正交设计试验法筛选三七药粉醇超声提取与醇回流提取各自的最优工艺条件,再用配对t检验法对比分析试验数据.结果:三七醇超声提取最优工艺参数为:三七药材超微粉加入30%的乙醇浸泡30 min,30%乙醇体积为药材量的6倍,超声时间30 min.三七醇回流提取最优工艺参数为:三七药材超微粉加入50%的乙醇浸泡30 min,50%乙醇体积为药材量的10倍,水浴回流时间30 min.三七药粉醇回流与超声提取差别有统计意义,比较均值回流提取优于超声提取.结论:三七采用回流提取为佳,按最优工艺条件提取,三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1及三种皂苷总和的含量较高.     

正交实验法优选复方水牛角颗粒提取工艺的研究

目的选择复方水牛角颗粒制剂的最佳提取工艺。方法对提取溶剂、加水量、提取次数及提取时间作为考察因素,采用正交设计法每个因素拟订3个水平,并用相应的药效学实验结果评价每一种工艺的药效作用的优劣,再结合得率和实际生产选择最佳工艺。结果用8倍量50%乙醇提取3次、每次1 h,此工艺所得的复方水牛角颗粒制剂的得率和药效学结果最佳。结论采用正交设计和相应的药效学实验的结果优选提取工艺是一个合理的和值得提倡的方法。     

Optimization of ultrasonic extraction by response surface methodology combined with ultrafast liquid chromatography–ultraviolet method for determination of four iridoids in Gentiana rigescens

Gentiana rigescens is a rich source of iridoids and is commonly used as a folk medicine for treatment of hepatitis and cholecystitis for over 1000 years. A rapid ultrafast liquid chromatography–ultraviolet method was developed for simultaneous determination of four major iridoid glycosides in G. rigescens. Response surface methodology based on the Box –Behnken design was applied to optimize the extraction conditions of iridoid glycosides. Using the Shim-Pack XR-ODS III, four iridoid glycosides were efficiently separated with an acetonitrile:0.1% formic acid aqueous solution gradient at a flow rate of 0.25 mL/min for 8 minutes. All the regression equations revealed a good linear relationship (R² > 0.9995). The intraday and interday variations were <1.95%. The recoveries ranged from 99.7% to 103.2%. The optimal extraction conditions were as follows: methanol concentration, 82%; the ratio of liquid to solid material, 68:1 (mL/g); and extraction time, 32 minutes. The yield of the four iridoid glycosides under the optimal process was found to be 63.08 mg/g, which was consistent with the predicted yield. In addition, the total content of 50 cultivated samples from Lincang, Yunnan, China, was within the range of 33.6–113.26 mg/g, which provides a more reasonable foundation for utilization of G. rigescens.