白芍中芍药苷的微波提取工艺研究

目的 研究微波提取白芍中芍药苷的工艺,得到优化工艺条件,建立芍药苷提取率与主要工艺参数之间的回归模型.方法 采用正交设计法和微波提取,应用STATISTICA6.0统计软件对正交实验结果进行分析,分别考察粒径、乙醇浓度、液固比、时间、温度、微波功率的选择对芍药苷提取率的影响.结果 优化工艺条件为粒径60目,乙醇浓度70...     

微波提取天麻中天麻素的工艺研究

目的 探索微波提取天麻中天麻素的最佳工艺.方法 采用正交实验设计方法,考察药材粒径、微波功率、温度、时间、溶剂(乙醇水溶液)组成和液固比等因素对天麻素提取率的影响,并用Statistica 6.0软件对正交实验结果进行分析.结果 优化工艺为药材粒径60～80目,微波功率300 W,温度40℃,时间2 min,乙醇体积分...     

微波辅助提取黄芩总黄酮工艺研究

目的:优化微波辅助提取黄芩总黄酮的工艺。方法:通过单因素和正交试验设计确定微波辅助提取黄芩总黄酮的优化工艺条件。结果:优化工艺条件为提取时间30min、乙醇浓度60%、微波功率600W、固液比1:15、反应温度80℃;在此条件下,总黄酮提取率为69·27%。结论:优化后的工艺稳定可行,可为黄芩总黄酮提取工艺的产业化提供理论参考。     

微波辅助提取雪莲果低聚糖的工艺研究

目的 确立雪莲果低聚糖的微波辅助提取工艺.方法 采用微波辅助提取雪莲果中的低聚糖,以雪莲果低聚糖提取率为考察指标,以提取温度、提取时间、料液比、微波功率、微波时间、解析剂比为考察因素进行正交试验,优化最佳提取工艺条件.结果 最佳提取工艺条件为:提取温度80℃,提取时间60min,液料比50:1,微波功率700W,微波时...     

正交优化微波提取女贞子中红景天苷工艺

目的 优选女贞子中红景天苷的提取工艺.方法 采用微波法提取女贞子中的红景天苷,且通过单因素及正交试验考察,用HPLC测定红景天苷含量,优化工艺条件.结果 优化工艺条件为:液固比为20mL·g-1,提取温度为45℃,微波提取时间为2min,提取剂乙醇浓度为30％,微波功率为600W,红景天苷的提取率为0.9113％.结论 所得优化工艺安全可靠,对工业生产具有指导意义.     

水栒子果肉低聚原花青素的提取工艺研究

目的:以水栒子果肉为实验材料,利用离子液体微波辅助提取法提取水栒子果肉中低聚原花青素,并对提取条件进行优化.方法:分别考察离子液体种类及浓度、液料比、浸泡时间、微波辐射时间及功率、提取次数,对低聚原花青素提取率的影响.结果:优化后工艺条件如下:1.00mol/L[C4mim]Br作为提取溶剂,液料比20:1(mL/g)...     

生姜总黄酮的微波-超声辅助协同提取工艺的研究

目的对微波-超声辅助提取生姜总黄酮的工艺条件及参数进行优化。方法在单因素试验的基础上,采用L9(34)正交设计,以生姜总黄酮提取率为指标,试验料液比、提取温度、提取时间、乙醇浓度对提取率的影响。结果最佳提取工艺参数为:提取温度85℃、提取时间60min、乙醇浓度φ=70%、料液比1∶30。结论采用微波-超声辅助协同提取生姜总黄酮工艺简单可行,是提取生姜总黄酮的有效工艺之一。用于提取生姜中的总黄酮,结果满意,回收率为98.4%～101.9%,RSD为1.5%。     

桂北金槐槐米中芦丁微波提取的工艺研究

目的研究微波辅助提取桂北金槐槐米中芦丁的工艺条件。方法采用乙醇为溶剂,以芦丁粗品的提取率为指标,考察微波功率、料液比、乙醇浓度、提取时间和静置时间对芦丁提取率的影响。结果微波辅助提取槐米中芦丁的最佳工艺条件为：微波功率为380 W,料液比为1∶20,乙醇浓度为55%,提取9 min,再静置8 h后芦丁提取率最高,达30.83%。结论应用微波辅助提取槐米中芦丁的提取时间短,提取率高,具有较好的发展前景。     

响应曲面法优化超声-微波协同提取澳洲坚果油的工艺研究

目的研究超声-微波协同提取澳洲坚果油的工艺。方法以提取率为指标,通过单因素实验分别考察了提取剂种类、微波功率、超声功率、液料比和提取时间对澳洲坚果油提取率的影响。利用Design-expert软件设计正交实验,用响应曲面法优化澳洲坚果油的提取工艺。结果确定的最佳工艺参数为:微波功率430 W,超声功率360 W,液料比20∶1mL·g~(-1),提取时间9min。在最佳条件下,澳洲坚果油的一次提取率为80.25%±0.18%(n=3),与理论计算值82.41%基本接近,说明回归模型能较好地预测坚果油的提取率。结论超声-微波协同提取澳洲坚果油具有提取率高、速度快和操作简便等优点,也为澳洲坚果的进一步开发提供了参考依据。     

正交试验优选蔓荆子总黄酮微波辅助提取纯化工艺

目的:优选蔓荆子总黄酮的微波辅助提取纯化工艺。方法:以乙醇浓度、反应温度、微波作用时间、微波功率、料液比为考察因素,以总黄酮含量为指标,通过正交试验优化提取工艺。用D101大孔吸附树脂纯化黄酮粗品。结果:最佳提取工艺为乙醇浓度60%、反应温度80℃、微波作用时间40min、微波功率600W、料液比1∶15;黄酮粗品经纯化后纯度可达84.93%以上。结论:优化后的工艺稳定、可行,可为蔓荆子总黄酮提取纯化工艺的产业化提供理论参考。     

改进鉴别荆芥穗中胡薄荷酮的薄层色谱法

目的利用薄层色谱法进行荆芥穗药材的定性鉴别研究。方法通过对样品不同提取方法的考察,在2015年版中国药典一部荆芥穗薄层鉴别方法的基础上进行了改进,有效降低薄层鉴别中的干扰。结果该方法能有效分离胡薄荷酮与其它成分。结论修订后的方法提取效率高、操作简便,能有效改善荆芥穗中胡薄荷酮的薄层色谱分离度。     

Biotransformation of monoterpenes by Mentha cell lines

Previous results indicated that all tested cell suspension lines derived from various MENTHA chemotypes were capable to biotransform (-) menthone to (+)-neomentol but only some of these lines converted (+)-pulegone to (+)-isomenthone. In order to quest whether only the natural secondary metabolites or also other compounds with similarities to pulegone are biohydrogenated by MENTHA cell suspensions, we incubated such suspensions with 5 unsaturated alpha-beta; ketones. No conversion was detected when mesityl oxide, trans-6-tert. butyl pulegone or 3-isopropylidine-9-methyl-decalone-2 were incubated with MENTHA cells, while saturation of the alpha-beta double bond of 2-isopropylidine cyclohexanone and of trans-6-methyl pulegone was observed in suspensions of those cell lines which are capable of pulegone transformation. Suspensions of MENTHA cell lines which were incapable to hydrogenate pulegone did not biotransform the two latter pulegone analogues.     

Hepatotoxicity of pulegone in rats: its effects on microsomal enzymes, in vivo

Oral administration of pulegone (400 mg/kg) to rats once daily for five days caused significant decreases in the levels of liver microsomal cytochrome P-450 and heme. Cytochrome b5 and NAD(P)H-cytochrome c-reductase activities were not affected. Massive hepatotoxicity accompanied by an increase in serum glutamate pyruvate transaminase (SGPT) and a decrease in glucose-6-phosphatase were observed upon treatment with pulegone. A significant decrease in aminopyrine N-demethylase was also noticed after pulegone administration. Menthone or carvone (600 mg/kg), compounds related to pulegone, when administered orally did not cause any decrease in cytochrome P-450 levels. The hepatotoxic effects of pulegone were both dose and time dependent. Pretreatment of rats with phenobarbital (PB) or diethylmaleate (DEM) potentiated the hepatotoxicity caused by pulegone, whereas, pretreatment with 3-methylcholanthrene (3-MC) or piperonyl butoxide protected from it. It appears that a PB induced cytochrome P-450 catalysed reactive metabolite(s) may be responsible for the hepatotoxicity caused by pulegone.     

金玄痔科熏洗散方中植物药超临界CO2萃取物的GC-MS分析

目的：分析金玄痔科熏洗散方中植物药超临界CO2萃取物的化学成分组成,诠释该中药复方制剂的药效物质基础。方法：采用超临界CO2萃取法得到超临界CO2萃取物,通过气相色谱-质谱法对其成分进行了分析鉴定。结果：共分离出34种成分,鉴定了其中33种化合物;主要成分为胡薄荷酮（23．17％）,棕榈酸（17．31％）、顺5-甲基-2-（1-甲基乙基）环己酮（11．74％）。结论：分析鉴定了金玄痔科熏洗散方中植物药超临界CO2萃取物有效物质部位中的33种化合物,占其总量的99％以上．这对于诠释该中药复方制剂的药效物质基础具有重要意义。     

响应面法优化连翘苷超声提取工艺

在单因素实验基础上,采用Box-Behnken中心组合设计原理优化提取溶剂甲醇的浓度、超声提取时间、超声功率和液料比.以连翘苷得率为响应值进行多元二次响应回归分析,得到连翘苷的最佳提取工艺条件为:甲醇浓度100%,超声提取时间27min,超声功率416 W,液料比12:1.回归模型预测最优条件下连翘苷得率为0.082%,验证值为0.080%,与预测值的相对误差为2.39%.     

Partial characterization of biliary metabolites of pulegone by tandem mass spectrometry. Detection of glucuronide, glutathione, and glutathionyl glucuronide conjugates.

The hepatotoxic monoterpene pulegone is a major constituent of the herbal abortifacient pennyroyal oil. An approximately equimolar mixture of 2H3- and 14C-labeled pulegone was administered to rats to study its phase II metabolism. Radioactive conjugates that were excreted into the bile were isolated by selective derivatization and HPLC separation, and subsequently characterized from the daughter ion mass spectra of protio- and deutero-analogs of each metabolite. The biliary metabolites characterized were glucuronide and glutathione (GSH) conjugates, accounting for approximately 3% of the radioactivity excreted in bile. The glucuronides, which were 2-fold more abundant than GSH conjugates, were mainly of hydroxylated pulegone and hydroxylated, reduced pulegone. The three GSH conjugates contained xenobiotic moieties that varied in their oxidation state; one of these was tentatively identified as the GSH conjugate of the proximate oxygenated metabolite, menthofuran. The two other GSH conjugates apparently underwent subsequent glucuronidation since novel glutathionyl glucuronide conjugates were identified that contained nonhydroxylated xenobiotic moieties. The results indicate that pulegone is bioactivated via at least three distinct pathways, each marked by a different GSH conjugate. Characterization of these conjugates represents a first step in the identification of the reactive metabolites from which they are derived.     

微波辅助萃取海芦笋中总黄酮工艺的研究

目的以海芦笋为原料、乙醇为浸提剂,在传统浸提技术基础上,辅以微波提取总黄酮。方法分别考察时间、温度、微波功率、料液比、乙醇浓度对总黄酮得率的影响,并在单因素试验基础上,运用正交试验,确定总黄酮提取最佳工艺条件。结果最佳提取工艺为:提取时间15 min,提取温度60℃,微波功率700 W,料液比1∶40,乙醇浓度55%,在此条件下提取海芦笋干粉中的总黄酮,得率为1.37%。结论微波辅助萃取海芦笋总黄酮的效率高于传统浸提工艺,乙醇浓度、提取时间和温度对总黄酮得率都有显著影响。     

14C-labeled pulegone and metabolites binding to alpha2u-globulin in kidneys of male F-344 rats

Pulegone is a major constituent of pennyroyal oil and a minor component of peppermint oil. Pulegone is biotransformed to menthofuran and menthones (diastereomeric menthone and isomenthone) in pennyroyal and peppermint as well as in rodents. Pulegone and menthofuran are hepatotoxic to rodents, and menthones are less toxic. The metabolism and disposition of pulegone and menthofuran were previously studied in rodents, and higher concentrations of pulegone- and menthofuran-derived radioactivity were observed in male than female rat kidney. One explanation is the association of pulegone and metabolites with a male rat-specific protein, alpha2u-globulin. To test this hypothesis, male and female rats were dosed orally with 14C-labeled pulegone (80 mg/kg, 120 microCi/kg) or menthofuran (60 mg/kg, 120 microCi/kg) or menthones (80 mg/kg, 120 microCi/kg) in corn oil, and the kidney cytosol was prepared 24 h after dosing. An equilibrium dialysis experiment showed that in all three studies the radioactivity was associated with kidney cytosol proteins of male but not female rats. The chemicals present in the male rat kidney cytosol after dialysis were extracted with dichloromethane and characterized by high-performance liquid chromatography (HPLC) and gas chromatography/mass spectrometry (GC-MS). All parent compounds were detected, and the metabolites characterized included piperitone from pulegone or menthones treatment, menthones and possibly 8-hydroxymenthones from pulegone treatment, and mintlactones (diastereomeric mintlactone and isomintlactone) and 7a-hydroxymintlactone from menthofuran treatment. Analysis of the male rat kidney cytosol by a gel filtration column demonstrated that the retention was due to reversible binding of these chemicals with the male rat-specific protein alpha2u-globulin. However, binding of pulegone and/or metabolites to alpha2u-globulin did not produce accumulation of this protein in the kidney.     

GC法测定感冒清热颗粒中胡薄荷酮的含量

目的:建立GC法测定感冒清热颗粒中胡薄荷酮的含量。方法:色谱柱为FFAP毛细管色谱柱(30 m×0.53 mm×1.0μm),柱温230℃,FID为检测器,选用乙酸乙酯作提取溶剂。结果:胡薄荷酮进样量在0.17～2.73μg范围内与峰面积线性关系良好(r=0.9999),平均加样回收率(n=6)为97.8%,RSD为1.0%。结论:该方法简便、可靠、准确,可用于该制剂的质量控制。