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。     

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。     

正交试验优化超临界CO2萃取法提取黄芪中黄芪甲苷工艺

目的:优化超临界CO₂萃取法提取黄芪中黄芪甲苷工艺。方法:用超临界CO₂萃取法提取黄芪中黄芪甲苷,以萃取温度、萃取压力、萃取时间、萃取剂流速为考察因素,黄芪甲苷得率为考察指标,运用正交试验优化提取的最佳工艺条件,同时用方差分析对其进行评价。结果:实验结果表明,超临界CO₂萃取法提取黄芪中黄芪甲苷的最佳工艺条件为:萃取温度为45 ℃、萃取压力为45 MPa、萃取时间为2 h、萃取剂流速为20 L·h^-1。结论:本提取工艺条件可行,为黄芪中黄芪甲苷的提取方法的及黄芪甲苷的研究提供科学依据。     

HPLC-ELSD法测定胃康颗粒中人参皂苷Rb1和黄芪甲苷的含量

目的 优化胃康颗粒中人参皂苷Rb₁和黄芪甲苷的提取方法,并建立其含量测定方法。方法 以人参皂苷Rb₁和黄芪甲苷的含量作为指标,采用单因素考察法对提取工艺进行优化;采用高效液相色谱-蒸发光散射法（HPLC-ELSD）,XBridge^®Shield RP₁₈（4.6 mm×250 mm,5 μm）为色谱柱;乙腈-水（32：68）为流动相;柱温为30 ℃;漂移管温度为60 ℃,载气流量为1.7 SLM,建立测定胃康颗粒中人参皂苷Rb₁和黄芪甲苷含量的方法。结果 当采用甲醇回流提取1.5 h,正丁醇提取5次,氨水洗涤2次时,人参皂苷Rb₁和黄芪甲苷的提取含量较高;建立的HPLC-ELSD法测定人参皂苷Rb₁和黄芪甲苷含量,线性关系良好（r > 0.9997）,日内日间精密度均小于1%,加样回收率分别为95.65%和100.57%,稳定性和重复性的RSD均小于3%,含量分别为2.8630 mg/g和0.2576 mg/g,RSD分别为0.62%和1.51%。结论 优化了胃康颗粒中人参皂苷Rb₁和黄芪甲苷的提取方法,建立了可靠、准确、重现性好的测定胃康颗粒中人参皂苷Rb₁和黄芪甲苷含量的HPLC-ELSD方法。     

正交试验-多指标权重分析法优选芪苓益肾颗粒的提取工艺

目的 优选芪苓益肾颗粒的提取工艺。方法 以黄芪甲苷得率、总多糖得率、干膏得率的综合评分为评价指标,采用层次分析法（AHP）确定这3个指标权重系数,设计L₉（3⁴）正交试验筛选最佳加水量、提取次数和提取时间,并进行验证试验。结果 以AHP法确定的权重系数合理有效。筛选的最优提取工艺为加8倍量水,提取3次,每次1 h。3次验证试验结果显示,黄芪甲苷、总多糖、干膏得率的平均值分别为0.10%、2.51%、43.09%;平均综合评分为99.88,RSD值为0.03%。结论 正交试验设计结合AHP确定的多指标权重系数法可较好地优化芪苓益肾颗粒的提取工艺。     

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。     

正交试验法优选芪葛颗粒的提取工艺

摘 要 目的：优化芪葛颗粒的提取工艺。方法: 建立芪葛颗粒中黄芪甲苷、葛根素2 种成分测定的HPLC 方法。采用 L9(34)正交设计,以黄芪甲苷、葛根素 2 种成分含量综合评分法进行数据分析,对芪葛颗粒的加水量、提取时间和提取次数3个因素进行优化。结果: 最佳提取工艺为：加入 12倍水,提取3次,每次 30 min。结论: 优选芪葛颗粒提取工艺能较好地保证制剂的质量。     

镇癫开窍颗粒提取工艺研究

目的 确定镇癫开窍颗粒的最佳提取工艺。方法 应用HPLC同时测定龙胆苦苷、芍药苷、黄芩苷的含量,并以含量测定的综合评分为考察指标,采用正交试验法L₉（3⁴）优选提取工艺条件。结果 对提取工艺的影响因素从大到小依次为提取次数、提取时间、乙醇浓度、加入溶媒量,最适工艺条件为8倍量的80%乙醇,浸泡30 min,提取3次,每次60 min。结论 该工艺稳定、可行。     

赤丹肝纤颗粒的醇提工艺研究

摘 要 目的： 优选赤丹肝纤颗粒的醇提最佳工艺。方法: 以虎杖苷含量为考察指标,先优选出最佳乙醇浓度,再采用L₉(3⁴)正交试验法,考察提取次数、提取时间及乙醇用量对提取效果的影响。结果: 最佳醇提工艺条件为以70%乙醇为溶媒回流提取2次,每次2 h,每次溶媒量为药材量的5倍。结论: 优选的工艺合理可行、重复性良好、提取效率高,适合于工业化生产。     

闪式提取红景天苷工艺优化研究

摘 要 目的： 用闪式提取法优化红景天苷的提取工艺。方法: 在单因素试验研究基础上,利用L₉(3⁴)正交试验设计对闪式提取红景天苷工艺进行优化,根据结果分析得出闪式提取红景天苷的最佳优化方案为A₂B₂C₂D₂,即料液比例1∶20,提取电压140 V,提取时间40 s,提取次数2次（40 s/次）。结果: 经验证,红景天苷提取率（3.83±0.12）%;试验对比闪式提取和其他提取方式发现,闪式提取较普通提取提高165.37%,较超声提取提高58.26%。结论:闪式提取法较有利于红景天苷的提取。     

Modifier effects on supercritical CO2 extraction efficiency of cephalotaxine fromCephalotaxus wilsoniana leaves

The effects of modifiers such as methanol, water, diethylamine in methanol (10 v/v %), and diethylamine in water (10 v/v %) were investigated at three different concentrations (1, 5, and 10 v/v %) of the modifiers in supercritical CO2 (SC-CO2) in order to enhance the supercritical fluid extraction (SFE) efficiency of cephalotaxine from Cephalotaxus wilsoniana leaves. Among the modifiers employed, methanol basified with diethylamine was found to greatly enhance the extraction efficiency relative to any other modifiers employed. The results suggest that cephalotaxine in plant matrices may be readily changed from SC-CO2-insoluble salt to SC-CO2-soluble free base by basified modifiers. In addition, SC-CO2 modified with basified methanol could enhance the extraction efficiency of cephalotaxine more than 30% when compared to the conventional organic solvent extraction.     

Polydopamine and silica nanoparticles magnetic solid phase extraction coupled with liquid chromatography-tandem mass spectrometry to determine phenolic acids and flavonoids in fruit wine

Magnetic solid phase extraction (MSPE) have been widely applied in a variety of sample preparation techniques. Herein, Fe₃O₄@pDA as the sorbents for MSPE, were developed for the determination of phenolic acids and flavonoids in fruit wine samples in combination with LC-MS/MS. The Fe₃O₄@pDA were characterized by Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), Superconducting Quantum Interference Device Magnetometer (SQUID) and thermogravimetric analysis (TGA) in detail. In the present study, a new, rapid, and efficient MSPE by LC-MS/MS was established for the extraction and sensitive detection of phenolic acids and flavonoids. Under the optimized condition of extraction procedure including the pH value of 4.0, 10 mg of Fe₃O₄@pDA, 60 s extraction time, and 600 μL desorption solvent volume, good responses were investigated. Results showed that the limits of detection (S/N = 3) for phenolic acids and flavonoids were in the range of 0.01–0.29 ng/ mL. The correlation coefficients of all analytes were more than 0.9985. The method was satisfactorily used for the detection of eleven analytes, and the recoveries of these targets for the two spiked wines (white grape wine and litchi wine) ranged from 80.03 to 116.68% and from 84.00 to 116.1%, respectively.     

Application of totally automated on-line sample clean up system for extraction and high-performance liquid chromatography separation of peptide leukotrienes

We have developed a fully automated on-line extraction—purification method for peptide leukotrienes in biological fluids using a column-switching technique. Individual leukotrienes in HPLC-collected fractions are determined by immunoassay techniques. Leukotrienes were extracted from nasal lavage samples and eluted from the solid-phase extraction cartridge into the HPLC column with methanol—ammonium acetate buffer (60:40, v/v) pH 5.4, as a mobile phase. This method provides good recoveries, excellent resolution of leukotrienes and is suitable to be combined with off-line radioimmunoassay (RIA) or enzymoimmunoassay (EIA). The most important losses are observed after evaporation—concentration and lyophilization. We also have compared RIA with EIA determination. Significant differences are found between RIA values and EIA values.     

基于近红外光谱分析技术的注射用益气复脉(冻干)红参醇提过程在线监测

目的 利用近红外光谱分析技术建立注射用益气复脉（冻干）主要原料红参醇提过程中3种单体皂苷——人参皂苷Rg₁、Re和Rb₁的定量模型,实现提取过程中关键指标的快速检测。方法 在线采集红参醇提过程的近红外光谱,以超高效液相色谱（UPLC）法测定提取过程药液中人参皂苷Rg₁、Re和Rb₁的量为参考值,采用偏最小二乘法建立光谱与测定值之间的定量校正模型,进而对提取过程进行在线分析。结果 人参皂苷Rg₁和Re的建模波段均为9 403.7～7 498.3 cm^-1和6 102～5 446.3 cm^-1组合波段;人参皂苷Rb₁的建模波段为5 774.1～5 446.3 cm^-1。人参皂苷Rg₁、Re、Rb₁定量模型的交叉验证决定系数（R²）分别为99.40、99.44、99.41,交叉验证均方根误差分别为5.18、2.77、11.00。结论 所建立的3种单体皂苷定量模型预测性能良好,能够有效测定红参醇提过程中人参皂苷Rg₁、Re和Rb₁的量。     

Composition of Asarum heterotropoides var. mandshuricum radix oil from different extraction methods and activities against human body odor-producing bacteria

In this study, oils from Asarum heterotropoides were extracted by traditional solvent extraction and supercritical CO₂ (SC-CO₂) extraction methods and their antioxidant activities along with antimicrobial and inhibitory activities against five human body odor-producing bacteria (Staphylococcus epidermidis, Propionibacterium freudenreichii, Micrococcus luteus, Corynebacterium jeikeium, and Corynebacterium xerosis) were evaluated. The oil was found to contain 15 components, among which the most abundant component was methyl eugenol (37.6%), which was identified at every condition studied in different extraction methods. The oil extracted with n-hexane and ethanol mixture exhibited a strong antioxidant activity (92% ± 2%) and the highest ABTS and 2,2-diphenyl-1-picrylhydrazyl scavenging activities (89% ± 0.2%). The highest amounts of total phenolic content and total flavonoid content were 23.1 ± 0.4 mg/g and 4.9 ± 0.1 mg/g, respectively, in the traditional method. In the SC-CO₂ method performed at 200 bar/50°C using ethanol as an entrainer, the highest inhibition zone was recorded against all the aforementioned bacteria. In particular, strong antibacterial activity (38 ± 2 mm) was found against M. luteus. The minimum inhibitory concentration (MIC) for the oil against bacteria ranged from 10.1 ± 0.1 μg/mL to 46 ± 2 μg/mL. The lowest MIC was found against M. luteus. Methyl eugenol was found to be one of the major compounds working against human body odor-producing bacteria.     

Ultrasonic-assisted liquid-liquid extraction and HILIC-ELSD analysis of ginsenoside Rb(1), astragaloside IV and dulcitol in sugar-free "Fufangfufangteng Heji"

A simple method for the extraction and determination of ginsenoside Rb₁, astragaloside IV and dulcitol in sugar-free “Fufangfufangteng Heji” was developed using an ultrasonic-assisted liquid-liquid extraction (UALLE) coupled with Hydrophilic Interaction Liquid Interface Chromatography and Evaporative Light Scattering Detector (HILIC-ELSD) analysis. Good chromatographic separation was achieved using a Phenomenex Luna HILIC column (250 mm × 4.6 mm i.d., 5 μm), and a mobile phase consisting of acetonitrile-water at a flow rate of 1.0 ml/min with a gradient elution within 25 min was also used. Compared to the conventional analysis method, the proposed method had the advantages of a longer column life, shorter analysis time, lower baseline noise, short sample pretreatment time and low consumption of organic solvent. The linear ranges for ginsenoside Rb₁, astragaloside IV and dulcitol were 0.0256-0.179, 0.110-0.770, 0.105-0.630 mg/ml, respectively. The recoveries of ginsenoside Rb₁, astragaloside IV and dulcitol during the pharmaceutical preparation were within the range of 97.2-100.3%, and their relative standard deviations were 1.2-3.1%.     

三七果中有效成分的闪式提取工艺研究

目的 选用闪式提取法对三七果进行提取工艺的考察,并通过采用高效液相色谱法对三七果所含的主要单体皂苷进行测定,优选出最佳提取方式。方法 采用闪式提取法提取三七果中的总皂苷,制备出9个供试品;以人参皂苷Rb₁为对照品,应用HPLC-UV法测定各个供试品中的单体皂苷。色谱柱条件：Hypersil C₁₈柱（200 mm×4.6 mm,5 μm）,流动相为乙腈-水梯度洗脱（0 min,20∶80→30 min,45∶55→48 min,70∶30→50 min,80∶20→60 min,100∶0）;检测波长203 nm;体积流量1.0 mL/min。结果 闪式提取可得到较高收率的总皂苷,且单体皂苷人参皂苷Rb₁的量较高。结论 闪式提取法速度快,效率高,耗材少,适用于三七果总皂苷的提取和制备。     

Determination of the adenosine A1 agonist N-cyclopentyladenosine in rat blood by solid-phase extraction and HPLC

A solid-phase extraction procedure has been developed for the isolation of the adenosine A1 receptor agonist N⁶-cyclopentyladenosine from rat blood. The biological samples were spiked with N⁶-cyclopentyladenosine and the analogue N⁶-cyclohexladenosine (internal standard), diluted with sodium hydroxide, loaded onto disposable cartridges with subsequent desorption with methanol and analysis by HPLC. The performance of columns pre-packed with different C18-bonded silica phases or with a polymeric reversed-phase sorbent (Oasis HLB) was assessed. The highest extraction efficiencies (recovery rates>83.3%) for the two N6-alkyl substituted adenosines were achieved by the Oasis HLB cartridges. In addition, the polymeric sorbent provided reproducible recoveries (relative standard deviation<4.8%), whereas large variations (relative standard deviation values, 9–16.3%) in the extraction yields were observed using the conventional silica-based C18 cartridges. The described sample preparation method is rapid, simple, selective and it is suitable for pharmacokinetic studies.     

抗生素提取过程中溶剂萃取技术新方法--超滤/萃取法

本文介绍了抗生素提取过程中溶剂萃取新方法－超滤／萃取法,用超滤法解决了萃取过程中一直未能很好解决的难题－乳化,提高了萃取收率和产品质量。并对抗生素萃取过程中乳化现象的预测与控制进行了讨论,提出了蛋白质临界乳化分子量的概念。