超临界CO_2萃取优化肺痿颗粒中黄芪甲苷提取工艺的研究

目的优化肺痿颗粒中黄芪甲苷的超临界CO_2萃取最佳工艺。方法以黄芪甲苷的含量为指标,选取粉碎粒度、萃取时间、夹带剂浓度和夹带剂流速为影响因素,采用L_9(3~4)正交试验法,优化提取工艺。结果处方最佳提取工艺为粉碎粒度40目、提取时间1.5 h、夹带剂浓度95%乙醇和夹带剂流速10 m L·min~(-1)进行超临界萃取。结论该优选工艺有效成分提取率高,条件可行,为肺痿颗粒工艺的优化提供科学依据。     

正交试验优选藏木香与干姜中挥发性成分萃取工艺

目的:优选藏木香与干姜中挥发性成分的最佳超临界CO2萃取工艺。方法以土木香内酯含量、挥发油得率为指标,以萃取压力、萃取温度、萃取时间及夹带剂用量为考察因素,采用正交试验优选最佳萃取工艺。结果:最佳萃取工艺为夹带剂量225mL,在萃取压力35Mpa下,于40℃萃取1h。结论:该工艺合理、操作可行、质量可控,可用于工业化生产。     

蒸馏-萃取耦合法提取川芎挥发油及质量评价

目的:建立蒸馏-萃取耦合法提取川芎挥发油新工艺和藁本内酯含量测定方法。方法:优选蒸馏-萃取耦合法提取川芎挥发油新工艺,气相色谱程序升温法测定藁本内酯含量。结果:确定了最佳提取工艺为以1.5 ml液体石蜡为萃取剂,用乙醇和20%的NaCl水溶液萃取分离得到川芎挥发油;建立了川芎挥发油中藁本内酯含量气相色谱测定法,藁本内酯在121.09~1 009.10 mg·ml^-1范围内线性关系良好,平均回收率为99.30% (n=9)。结论:所建立的蒸馏-萃取耦合法提取川芎挥发油的新工艺优于川芎挥发油的传统蒸馏法,其含量测定方法可用于川芎挥发油中藁本内酯的含量测定。     

超临界CO_2流体萃取莪术油的工艺研究

目的研究建立莪术油的最佳提取工艺。方法通过正交设计,用超临界CO2流体提取法(SFE)提取莪术挥发油,采用GC法、HPLC法测定莪术油中莪术醇、牦牛儿酮的含量,并以次为指标优化出合理的工艺条件。结果超临界CO2流体萃取莪术醇的最佳工艺为萃取温度45℃,萃取压力25MPa,提取时间2h,夹带剂(95%乙醇)用量10%。结论用SFE法提取莪术醇具有开发价值。     

超临界CO2萃取优化肺痿颗粒中黄芪甲苷提取工艺的研究

目的 优化肺痿颗粒中黄芪甲苷的超临界CO₂萃取最佳工艺。方法 以黄芪甲苷的含量为指标,选取粉碎粒度、萃取时间、夹带剂浓度和夹带剂流速为影响因素,采用L₉（3⁴）正交试验法,优化提取工艺。结果 处方最佳提取工艺为粉碎粒度40目、提取时间1.5 h、夹带剂浓度95%乙醇和夹带剂流速10 mL?min^-1进行超临界萃取。结论 该优选工艺有效成分提取率高,条件可行,为肺痿颗粒工艺的优化提供科学依据。     

超临界CO2萃取南方红豆杉中挥发油和10-DABⅢ的工艺优化

目的 优化超临界CO₂萃取法萃取南方红豆杉中挥发油和10-DABⅢ的工艺条件。方法 以萃取时间、萃取温度、萃取压力、分离温度、物料与夹带剂的比例和夹带剂浸泡时间等为考察因素，以红豆杉中挥发油的得率和10-DABⅢ的含量为评价指标，采用正交试验优选最佳工艺条件。结果 最佳工艺条件为以无水乙醇为夹带剂，物料与夹带剂比例为1:3,萃取压力270 bar、萃取温度35℃、分离温度40℃,萃取时间2.5 h。红豆杉挥发油的得率为23.422%,10-DABⅢ的含量0.546‰。结论 所用工艺稳定、可行，可用于红豆杉中挥发油和10-DABⅢ的提取。     

SFE-CO2与渗漉法提取丹参药渣中脂溶性成分比较

目的探寻大生产水提后丹参药渣中脂溶性成分的提取方法及其最佳工艺条件,以便对丹参药材进行综合利用。方法以丹参酮ⅡA的含量为指标,采用正交设计优选最佳提取工艺,并进行对比、验证。结果SFE CO2萃取法的最佳工艺为：萃取压力35 MPa,夹带剂乙醇用量为100%,萃取温度40 ℃,萃取时间2 h,含量为3.87 mg。渗漉法最佳工艺为乙醇浓度95%,乙醇用量16倍,流速1 mL•min 1,药材目数20目,含量3.28 mg。结论SFE CO2法优于渗漉法,并且提取含量高,丹参的综合利用完全可行。     

超临界CO2萃取三七中挥发油及皂苷的工艺研究

目的研究超临界CO2萃取三七中挥发油和皂苷的工艺。方法通过考察萃取压力、温度、萃取时间、CO2流量、夹带剂对萃取率的影响,确定三七中挥发油和皂苷的较佳萃取条件,采用薄层色谱法（TLC）鉴别挥发油和皂苷成分。结果萃取三七中挥发油较佳条件为：萃取压力30MPa,温度45℃;解析釜I压力为9MPa,温度40℃;解析釜II压力为6MPa,温度35℃;萃取时间2．5h;CO2流量为25kg·h^-1。皂苷的较佳萃取条件为：萃取压力35MPa,温度55℃;解析釜I压力为8MPa,温度45℃;解析釜II压力为5MPa,温度40℃;萃取时间4h;95％乙醇作夹带剂;CO2流量为25kg·h^-1。挥发油中含有人参炔醇,皂苷中含有总皂苷成分。结论超临界CO2萃取挥发油收率高,时间短。加入95％乙醇作夹带剂,升高压力和温度,能萃取出皂苷类成分。     

夹带剂在超临界CO2萃取黄芪甲苷中的影响

摘 要 目的：研究夹带剂对超临界CO²萃取黄芪中黄芪甲苷的影响。方法: 以夹带剂加入方式、夹带剂种类、夹带剂加入量及夹带剂流速为考察因素,黄芪甲苷的提取率作为考察指标, 用L₉(3⁴) 正交表优化工艺条件,并用高效液相色谱法对黄芪甲苷进行含量测定。结果: 夹带方式选择预浸+动态萃取模式,以95%乙醇作为夹带剂,加入量为300 ml,加入流速10 ml·min^-1);在以下条件进行超临界萃取时,黄芪甲苷提取率可达到0.040 7%：萃取温度45℃,出口温度55℃,萃取压力35 MPa,95%乙醇液态收集萃取物,动态萃取时间2 h。结论:本实验优选的工艺对超临界co²萃取黄芪中黄芪甲苷的提取有着明显提高。     

超临界CO2萃取川东獐牙菜总员(口山)酮的工艺优化

目的 优化超临界CO2萃取川东獐牙菜总(口山)酮的工艺.方法 以去甲基雏菊叶龙胆酮和总(口山)酮含量为指标,用正交试验法优选.结果 川东獐牙菜总山酮萃取的最佳工艺条件为:萃取温度40 ℃,萃取压力30 MPa,萃取时间80 min,夹带剂为95%乙醇.结论 采用超临界CO2萃取法提取脂溶性成分具有速度快、效率高和无污染的特点,工艺简便易行.     

Simultaneous determination of betulin and betulinic acid in white birch bark using RP-HPLC

A simple procedure is described for the simultaneous extraction and determination of betulin and betulinic acid in white birch bark. The extraction was checked using different solvents: dichloromethane, ethyl acetate, acetone, chloroform, methanol and 95% ethanol (aqueous solution, v/v). It was found 95% ethanol was a good extraction solvent that allowed extraction of triterpenoid with a highest content. Separation was achieved on a reversed phase C(18) column with acetonitrile-water 86:14 (v/v). Detection was accomplished with UV detection at lambda=210 nm. Using this method, the bioactive triterpenoid in white birch bark were simultaneously determined. Significant variations in the content of betulin and betulinic acid in white birch bark growing in different locations of China were also observed.     

Microwave-assisted hydrodistillation extraction based on microwave-assisted preparation of deep eutectic solvents coupled with GC-MS for analysis of essential oils from clove buds

In recent years, deep eutectic solvents (DESs) as green and sustainable solvents have been widely used in the effective extraction of natural products. Usually, DESs are synthesized by heating and stirring method which takes a long time and energy. In this case, a microwave assisted preparation technique was used to form DESs for saving time and energy. And the DESs as pretreatment solvents were combined with microwave-assisted hydrodistillation (MAHD) for the extraction of essential oils (EOs) from the clove buds in this work. The maximum essential oils yield of 4.60% was obtained with the microwave power of 600 W, the pretreatment time of 5 min and the hydrodistillation time of 40 min using a deep eutectic solvent composed of choline chloride and lactic acid (molar ratio with 1:2). In addition, the essential oil was analyzed by gas chromatography-mass spectrometry (GC-MS), a total of 40 compounds were identified. Compared with MAHD, water-based MAHD and traditional hydrodistillation (HD), the content and composition of essential oil extracted by DES-based MAHD were higher. Thus, the combination of deep eutectic solvents with a microwave-assisted technique in this study provided an eco-friendly way of extracting essential oils.     

正交试验法优选苦丁茶老叶中熊果酸的提取工艺

目的:优选苦丁茶老叶中熊果酸的提取工艺条件。方法:以熊果酸含量为考察指标,采用L9(34)正交试验法考查不同因素和水平对熊果酸提取工艺的影响。结果:影响工艺的因素次序为提取次数>液固比>乙醇浓度>提取时间;最佳提取工艺为在85℃水浴温度下,液固比为16∶1、乙醇浓度为80%、水浴提取2次、每次2.5h。在此条件下,熊果酸的含量可达45.65μg.g-1。结论:该提取工艺合理、可行。     

HPLC法测定疤痕止痒软化乳膏中丹皮酚的含量

目的建立用高效液相色谱法测定疤痕止痒软化乳膏中丹皮酚含量的方法。方法色谱柱为Shim-pack VP-ODS(150mm×4.6mm,5μm),流动相为甲醇-水(65∶45),流速为1.0mL.min-1,检测波长为274nm,柱温为30℃,进样量为10μL。结果线性范围为0.02094~0.19893μg(r=0.9999);平均回收率为98.3%(RSD=2.51%,n=6)。结论本方法分离度好、快速、简便,可作为产品的质量控制方法。     

产舒康颗粒的制备及质量标准研究

目的:制备产舒康颗粒并建立其质量标准。方法:以胎盘超微粉碎技术进行颗粒制备,通过氨基酸分析、薄层色谱法和高效液相色谱法进行质量控制。色谱柱为C18(200mm×4.6mm,5μm),流动相为甲醇-2%冰醋酸溶液(40∶60),检测波长为324nm。结果:胎盘超微粉粒度、色泽、味道、分散程度较好,经薄层鉴别、氨基酸分析与普通粉无显著差异。本品中用薄层色谱检出当归、川芎、胎盘、甘草;阿魏酸含量在0.625~3.750μg范围内线性关系良好;3批颗粒中阿魏酸含量分别为0.054%、0.037%、0.042%,平均回收率为96.2%(RSD=2.37%)。结论:可将胎盘制成超微粉用于产舒康颗粒,质控方法专属性强。     

HPLC-蒸发光散射检测法测定不同产地酸枣仁中白桦脂酸的含量

目的建立以高效液相色谱-蒸发光散射检测法测定酸枣仁中白桦脂酸含量的方法。方法色谱柱为Agilent C18(250mm×4.6mm,5μm),流动相为甲醇-水-三乙胺(用冰醋酸调至pH=5.7,86∶14∶0.03),流速为1.0mL.min-1,柱温为25℃,进样量为20μL,漂移管温度为80℃,气体(氮气)流速为2.0L.min-1。结果白桦脂酸检测浓度在10.10~161.60μg·mL-1范围内线性关系良好(r=0.9995,n=6);平均加样回收率为97.95%(RSD=0.25%)。结论本方法简便、准确、重现性好。     

格列齐特片(Ⅱ)鉴别与含量测定方法改进

目的:改进格列齐特片(Ⅱ)现有质量标准中鉴别与含量测定的方法。方法:采用紫外-可见分光光度法代替电位滴定法,溶剂为乙醇,检测波长为228nm,对格列齐特片(Ⅱ)进行鉴别和含量测定。结果:鉴别时无需前处理;改进后方法格列齐特检测浓度的线性范围为4.38～26.28μg·mL-1(r=0.9987);平均回收率为100.06%,精密度为0.17%。结论:与原有方法比较,本方法操作更简便安全,且结果准确,可用于该制剂的鉴别和质量控制。     

当归和欧当归中藁本内酯的薄层扫描测定法

藁本内酯(Ligustilide)是当归(Angelica sinensis Diels)和欧当归(Livisticum officinale koch)根挥发油中的主要成分。已报道当归和欧当归挥发油中含藁本内酯分别约为60％和35％。三桥博等人报道藁本内酯是一种新的活性物质。两种挥发油有相似的药理活性,对大鼠离体子宫有抑制其节律性收缩的作用。     

Fatty acid compositions in local sea cucumber, Stichopus chloronotus, for wound healing.

Fatty acid profile from crude extracts of local sea cucumber Stichopus chloronotus was determined using gas chromatography (GC) technique. The extracts were prepared separately in methanol, ethanol, phosphate buffer saline (PBS), and distilled water as part of our study to look at the affinity of these solvents in extracting the lipid from sea cucumber. The PBS and distilled water extractions indicate water-soluble components, while the organic fractions are extracted in methanol and ethanol as organic solvents. Furthermore, water extraction is the conventional method practiced in Malaysia. In our analysis the C14:0 (myristic), C16:0 (palmitic), C18:0 (stearic), C18:2 (linoleic), C20:0 (arachidic), and C20:5 (eicosapentaenoic, EPA) were significantly different (p < 0.01) in the four solvent extractions. However, the PBS extraction contained a much higher percentage of EPA (25.69%) compared to 18.89% in ethanol, 7.84% in distilled water, and only 5.83% in methanol, and variances were significantly different (p < 0.01 ). On the other hand, C22:6 (docosahexaenoic acid or DHA) is much higher in water extraction (57.55%), in comparison to the others where only 3.63% in PBS and 1.20% in methanol, and this difference is significant at p < 0.01. No DHA was detected in ethanol extractions. Subsequently, C18:1 (oleic acid) was only detected in PBS (21.98%) and water extraction (7.50%). It is interesting that palmitic acid, C16:() was higher in methanol (20.82%) and ethanol (2.18%), while 12.55% was detected in PBS and only 2.20% in water extraction: and again this was significantly different at p < 0.01. Although our results have shown that all four solvents were different in terms of their ability to extract fatty acids, the major component for tissue repair was well preserved. Probably this is one of the important precocious steps when working with a delicate sea cucumber, in both experimental and/or at the preparative stages. Freshness of the sea cucumber samples is important when undertaking this type of experiment. Finally, we believe that the local sea cucumber S. chloronotus contains all the fatty acids required to play a potential active role in tissue repair.     

协日嘎四味汤胶囊的制备工艺研究

目的研究协日嘎四味汤胶囊的制备工艺。方法将姜黄、黄柏、栀子、蒺藜四味药提取,制备成胶囊,采用水提醇沉,优选水蒸气蒸馏法提取挥发油及挥发油的吸附最佳工艺。结果挥发油的提取工艺为：加水14倍量,提取8 h;其最佳吸附工艺为：2倍量磷酸氢钙吸附24 h。醇沉最佳工艺：乙醇浓度为60%,醇沉24 h。结论协日嘎四味汤胶囊的制备工艺符合现代制剂的有关要求。