中药大黄中蒽醌的微波辅助流动萃取研究

利用微波辅助流动萃取法提取大黄中的蒽醌类化合物，考察了微波提取条件(包括溶剂浓度、微波辐射功率、溶剂提升量)对大黄中葸醌提取率的影响，采用分光光度法测定提取液中蒽醌的含量．结果表明溶剂为60%乙醇，提升量为4mL／min，微波功率为80％时，提取效率最佳．微波辅助流动萃取法与超声波法和索氏提取法相比，具有提取效率高，时间短且节能的良好特点．     

高效毛细管电泳-紫外检测法同时检测决明子中5种蒽醌类化合物

采用高效毛细管电泳-紫外检测技术研究了决明子中5种蒽醌类化合物的毛细管电泳迁移情况,并对所测对照品和供试品进行定性和定量分析。最佳分离条件为:检测波长284 nm,分离电压25 kV,进样时间5 s,运行缓冲溶液Na_2B_4O_7-H_3BO_3,浓度20 mmol/L,pH 8.50,β-环糊精浓度为5 mmol/L。在该条件下,大黄素,大黄酸,大黄酚,大黄素甲大黄素甲醚,橙黄决明素在10 min内实现分离,线性范围依次为4~350,2~350,3~300,4~400,5~400μg/mL,线性相关系数r大于0.9952,检出限分别为50.3,56.6,16.7,51.9,33.6 ng/mL(S/N=3),平均回收率在96.3%~103.6%(n=3)之间,RSD在1.4%~4.6%之间。方法可以为决明子中蒽醌类成分的分析提供一定的参考。     

高效液相色谱同时测定芦荟中8种蒽醌类物质的含量

建立了高效液相色谱(HPLC)-二级阵列检测器(DAD)同时测定芦荟中8种蒽醌类物质(芦荟苷B、芦荟苷A、大黄素-8-O-葡萄糖苷、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚)的方法。样品经5 mL 90%甲醇在30℃超声提取20 min后,以甲醇-乙腈-0.05%磷酸溶液为流动相梯度洗脱,经Eclipse XDB-C_(18)柱分离,多波长同时检测。8种蒽醌类待测物在14 min内获得满意的分离。方法的检出限(S/N=3)为0.55~1.02μg/g,样品平均加标回收率为90.3%~107.8%,RSD为4.8%。     

梯度加压毛细管电色谱同时分离大黄提取液中5种蒽醌类化合物

建立了同时分离药用大黄提取液中大黄酸、芦荟大黄素、大黄素、大黄酚和大黄素甲醚5种蒽醌类活性成分的梯度加压毛细管电色谱的新方法.实验结果显示,大黄提取液中的5种蒽醌化合物可在22min内完全分离,梯度洗脱微柱液相色谱的柱效为等度洗脱微柱液相色谱的6.63倍,梯度毛细管电色谱的柱效为梯度微柱液相色谱的4.6倍.     

中药材成分有机溶剂与离子液体分散液相微萃取方法的比较及其机理探讨

研究了离子液体分散液相微萃取(ILDLPME)机理;比较了ILDLPME和有机溶剂分散液相微萃取(OSDLPME)在测定蒽醌类化合物中的异同;建立了分散液相微萃取-高效液相色谱法测定药材中6种游离蒽醌类化合物(芦荟大黄素、大黄酸、丹蒽醌、大黄素、大黄酚和大黄素甲醚)含量的方法。在优化的实验条件下,OSDLPME和ILDLPME对6种分析物的富集倍数分别为101～230和76～181;6种分析物的检出限分别在20～200ng/L和40～400ng/L之间;精密度(RSD)分别在3.1%～10.0%和1.3%～7.0%之间;4种中药材中分析物的回收率在81.7%～110.7%和81.9%～110.8%之间。离子液体在水中分散的同时进行有序排列,形成分子有序组合体,对分析物进行萃取。ILDLPME达平衡时间更快,精密度更高,方法更简便;OSDLPME浓缩倍数更高,检出限更低;两种方法对中药样品中游离蒽醌类化合物含量测定结果无显著性差异。     

中药大黄蒽醌类物质电喷雾质谱裂解规律研究

大黄是一味临床常用药材,化学成分复杂,主要药效成分为蒽醌类衍生物.其中1,8-二羟基蒽醌类衍生物如大黄素(Emodin)、大黄酚(Chrysophanol)、大黄酸(Rheni)、大黄素甲醚(Physcion)、芦荟大黄素(Aloe-emodin)等在中药中分布较广泛.这类物质及其甙类具有泻下、抗菌、抗癌等多种生理活性.对于大黄蒽醌类物质的分离、含量测定、药理研究等一直是一个非常活跃的领域,但对大黄蒽醌类衍生物的电喷雾质谱裂解规律的研究还未见报道.本文我们应用电喷雾离子阱质谱(ESI-MS)研究了5种大黄素型蒽醌衍生物的裂解规律.为进一步开展大黄蒽醌类物质在生物体内的代谢规律等做了有益的探讨.     

大黄素的化学合成及结构修饰研究进展

大黄素是中药大黄的主要成分,也存在于虎杖、芦荟等药用植物中,是分布广泛的一种羟基蒽醌类化合物.其药理作用表现为抗肿瘤、扩张血管、抗菌、导泻、利尿等,具有很好的临床应用价值.结合本研究组的工作综述了大黄素的化学合成方法、结构修饰和生物活性等方面的新进展.     

微波辅助提取-可见分光光度法测定穿心莲中的总黄酮

比较了微波辅助提取、超声提取、索氏提取3种方式对穿心莲中总黄酮的提取效率.确定以微波辅助提取法最佳.实验结果表明:用60%乙醇在固液比为1:15的条件下提取6 min提取效率最高.用NaNO2-硝酸铝-NaOH-黄酮体系分光光度法测定总黄酮含量,平均回收率为103.00%,RSD=1.37%(n=5),证实了可以用微波辅助提取法提取,紫外可见分光光度法检测穿心莲中总黄酮的可行性.     

微波辅助-旋转回流提取仪的组装及其在叶下珠有机酸提取中的应用

组装了一种新型的微波辅助旋转回流装置,该装置的基本原理与微波辅助溶剂萃取的原理相同,但采用了旋转的技术以加速提取.应用该装置以正交实验筛选优化叶下珠中有机酸的提取工艺,并利用毛细管电泳技术分离测定了提取液中有机酸的含量以评价提取效果.最佳提取工艺:乙醚为溶剂,微波功率800 W,提取时间4 min,溶剂用量300 mL.在该提取条件下,平行5次提取叶下珠中丁二酸、原儿茶酸、没食子酸、咖啡酸、阿魏酸的平均含量分别为42.2、103.5、436.2、123.8、67.4 μg/g,相对标准偏差为0.87% ～3.7%,加标回收率为94% ～104%.将该法与常规的微波辅助提取法及回流提取法进行比较,结果表明,微波辅助旋转回流提取法提取效率明显优于其它2种方法.     

何首乌中蒽醌类物质的超声波提取工艺优化

采用超声波辅助法提取何首乌中蒽醌类物质.讨论了甲醇体积分数、提取时间、提取温度、料液比和提取功率5个因素对提取效率的影响;通过正交试验确定了何首乌中蒽醌类物质的最佳提取工艺条件,甲醇体积分数为80%,提取时间为1.0h,提取温度为45℃,料液比为1∶15(g∶mL),提取功率为700W.此条件下蒽醌类物质的最大提取率为1.472 9%.     

Qualitative analysis of multiple compounds in raw and prepared Semen Cassiae coupled with multiple statistical strategies

In China, Semen Cassiae is used clinically to improve eyesight, relieve constipation, and to treat headache and dizziness. Prepared Semen Cassiae is obtained by stir‐frying raw Semen Cassiae until it turned dark brown, micro dilatancy, and overflow aroma. After processing, the therapeutic effects change—the purgation effect is alleviated and the hepatoprotective effect is enhanced. To explore the changes in chemical compositions of Semen Cassiae after processing and clarify the material basis of the changed therapeutic effects, an ultra‐high performance liquid chromatography with quadrupole time‐of‐flight mass spectrometry coupled with automated data analysis software and statistical strategy was developed. As a result, 53 compounds in raw Semen Cassiae and 43 compounds in prepared Semen Cassiae were found, a total of 55 chemical compounds were identified. Principle component analysis and t‐test were processed by Markerview 1.2.1 software. Finally, 39 peaks were found to be the main contributors to the significant difference (p  < 0.05) between raw and prepared Semen Cassiae. Compared with raw Semen Cassiae, 19 peaks showed a higher intensity in prepared Semen Cassiae, while the contents of 20 compounds in prepared Semen Cassiae were lower, most of which belonged to naphthopyrones glycosides and anthraquinone glycosides.     

Quality evaluation of Semen Cassiae (Cassia obtusifolia L.) by using ultra-high performance liquid chromatography coupled with mass spectrometry

A sensitive and reliable ultra-high performance liquid chromatography-electrospray ionization-tandem mass spectrometry has been developed and partially validated to evaluate the quality of Semen Cassiae (Cassia obtusifolia L.) through simultaneous determination of 11 anthraquinones and two naphtha-γ-pyrone compounds. The analysis was achieved on a Poroshell 120 EC-C(18) column (100 mm × 2.1 mm, 2.7 μm; Agilent, Palo Alto, CA, USA) with gradient elution using a mobile phase that consisted of acetonitrile-water (30 mM ammonium acetate) at a flow rate of 0.4 mL/min. For quantitative analysis, all calibration curves showed perfect linear regression (r(2) > 0.99) within the testing range. This method was also validated with respect to precision and accuracy, and was successfully applied to quantify the 13 components in nine batches of Semen Cassiae samples from different areas. The performance of developed method was compared with that of conventional high-performance liquid chromatography method. The significant advantages of the former include high-speed chromatographic separation, four times faster than high-performance liquid chromatography with conventional columns, and great enhancement in sensitivity. This developed method provided a new basis for overall assessment on quality of Semen Cassiae.     

Nine components pharmacokinetic study of rat plasma after oral administration raw and prepared Semen Cassiae in normal and acute liver injury rats

In China, Semen Cassiae has long been used to protect liver, brighten eyes, and relieve constipation. Prepared Semen Cassiae is produced from raw Semen Cassiae by processing, the two forms of Semen Cassiae have different clinical applications. Pathological state is an important factor affecting the efficacy of drugs, the pharmacokinetic behavior of drugs could be significantly changed when people or animal were under different pathological state. To clarify the effect of processing mechanism and pathological state for pharmacokinetic behavior, the pharmacokinetics of nine components of raw and prepared Semen Cassiae under normal and acute liver injury rats were examined. The results showed that the bimodal phenomenon appeared on the plasma concentration‐time profiles of obtusin, emodin, chrysophanol, aloe emodin and rhein. The T_max of aurantio‐obtusin, obtusin, chrysoobtusin, emodin, chrysophanol, aloe emodin, physcion in normal groups administrated prepared Semen Cassiae were shorter than those administrated raw Semen Cassiae. For the AUC_0–t, aurantio‐obtusin, obtusin, chrysoobtusin, chrysophanol, aloe emodin and physcione in model groups administrated prepared Semen Cassiae were significantly higher than other groups, unlike above components, rhein had poor absorption in model groups. The study would be useful for further studies on pharmacokinetics and clinical application of raw and prepared Semen Cassiae.     

生、炒决明子中无机元素的分析测定

为测定生决明子中无机元素水平,探讨其药效物质基础及炒制对其含量的影响,采用原子荧光法和等离子发射光谱法等测定了不同产地、批次的生、炒决明子中重金属及微量元素的含量。结果表明,不同产地的生、炒决明子含有的重金属元素均没有超过食品卫生标准。决明子经过炮制后,无机元素变化情况:硫、钠、铬、钡、锂、镍、锶等元素炮制前后变化不大;钙、钾、镁、锰、锌有益元素的含量略有增高;汞、铅、砷有害元素的含量略有下降。可见决明子饮片药用是安全的,炒制工艺对决明子无机元素含量有一定影响,其特有无机元素的种类和含量对揭示决明子药效的物质基础具有意义。     

A general gas‐assisted three‐liquid‐phase extraction method for separation and concentration of puerarin, 3′‐methoxydaidzin,puerarinxyloside, daidzin and daidzein from puerariae extract

In this work, a general and novel separation technique gas‐assisted three‐liquid‐phase extraction was established and applied in separating and concentrating isoflavonoids from the actual sample of puerariae extract by one step. For the gas‐assisted three‐liquid‐phase extraction method, optimal conditions were selected: polyethylene glycol 2000 and ethyl acetate as the flotation solvent, pH 5, (NH₄)₂SO₄ concentration 350 g/L in aqueous phase, N₂ flow rate 30 mL/min, flotation time 50 min, and flotation twice. Five isoflavonoids compounds puerarin, 3′‐methoxydaidzin, puerarinxyloside, daidzin and daidzein were separated with recoveries of 82, 84, 80, 88 and 89%, respectively. The separated products were purified by preparative high‐performance liquid chromatography, and the purity of the final products was >96%. The established general gas‐assisted three‐liquid‐phase extraction was used to separate anthraquinones from Cassiae Semen under the optimal conditions, and the recoveries were >75%. The experimental results showed that the established gas‐assisted three‐liquid‐phase extraction method is a general technique for separating active compounds from herb extract.     

Dynamic Microwave-assisted Extraction of Flavonoids from Radix Scutellariae

IntroductionRadix Scutellariaeis the root ofScutellaria bai-calensis Georgi(Labiatae), which is widely cultivatedand used as traditional Chinese medicine. It has beendemonstrated to be anti-inflammatory, anti-metamor-phic, antiviral, anti-hot, and live pr…     

GC-MS法测定ABS木塑材料中十溴二苯醚

建立了索氏提取和超声萃取-GC-MS法测定丙烯腈-丁二烯-苯乙烯共聚物(ABS)木塑材料中十溴二苯醚的分析方法。通过正交试验分析提取溶剂、样品质量和提取时间三个因素的显著性,并优化了参数。在优化条件下,索氏提取和超声萃取法的平均回收率均大于80%,精密度均小于10%。经F检验和T检验显著性统计,两种前处理方法的精密度和准确度不存在差异。相对于传统的索氏提取法,超声萃取法具有操作简单、溶剂用量少和省时的特点,可以较好的应用于木塑材料中十溴二苯醚检测。     

紫草中活性成分的非极性溶剂动态微波提取及高效液相色谱法测定

用非极性溶剂动态微波辅助提取,高效液相色谱法测定紫草中的紫草素和β,β′-二甲基丙烯酰紫草素.考察了微波吸收介质类型、提取溶剂种类、提取溶剂流速、微波功率和样品粒度对提取产率的影响,优化提取参数.在优化条件下,将所建立的方法与超声提取和索氏提取相比,所得紫草素和β,β′-二甲基丙烯酰紫草素的产率相差不大,但本文所建立的方法所需提取时间短(5min)、溶剂消耗少(10mL).与极性溶剂动态微波辅助提取相比,提取产率大幅度提高.结果说明,所建立的方法是一种有效的提取中草药中一些活性成分的方法,特别是对于一些在非极性溶剂中有更高溶解度的化合物,此方法更具优势.     

五种十字花科植物中芥子碱的有效提取和高效液相色谱定量分析

本文采用超声,乙醇回流、石油醚脱脂后醇提等提取方法,并通过正交试验,对五种十字花科植物种子白芥子、黄芥子、葶苈子、莱菔子和油菜籽中的芥子碱进行了有效提取,同时采用高效液相色谱法对各种方法得到的提取液进行了定量分析。结果表明:超声提取时间短、提取率高,五种种子中芥子碱的含量分别为5.80mg.g-1、5.13mg.g-1、2.62mg.g-1、2.98mg.g-1和3.31mg.g-1。