猴头菌发酵刺五加后多糖与紫丁香苷的含量变化研究

研究猴头菌发酵刺五加后多糖及紫丁香苷的含量变化,为新药源开发提供理论依据。以蒽酮-硫酸法测定猴头菌发酵刺五加前后多糖的含量,并采用高效液相色谱法对发酵前后紫丁香苷的含量进行检测。结果显示,猴头菌发酵刺五加后多糖的质量分数由发酵前的0.3%提高到0.7%,多糖的含量提高了133%;而刺五加原药材中紫丁香苷的含量为0.0096%,发酵后在紫丁香苷标准峰对应处未出峰,而是在其它位置出现了三个新的谱带。猴头菌发酵刺五加后多糖含量显著提高,可以起到协同或增加猴头菌及刺五加药效的作用;发酵物中紫丁香苷成分未检出,是由于发酵后紫丁香苷在微生物酶的作用下降解转化为其它物质,有利于提高生物利用度,为新药源的开发奠定了基础。     

乳酸杆菌HD11发酵刺五加对紫丁香苷及异嗪皮啶含量的影响

采用高效液相色谱法对刺五加发酵前后紫丁香苷及异嗪皮啶的含量进行检测,研究乳酸杆菌HD11发酵刺五加对紫丁香苷及异嗪皮啶含量的影响。结果表明:刺五加经乳酸杆菌HD11发酵后紫丁香苷含量显著降低,而在其附近位置出现了新物质;乳酸杆菌HD11发酵刺五加根、茎后异嗪皮啶含量分别由发酵前的0.08、0.05mg/g提高到0.14、0.15mg/g。刺五加发酵后紫丁香苷含量降低,是由于紫丁香苷在乳酸杆菌HD11的作用下降解转化为其他物质,而异嗪皮啶含量的提高有利于提高活性成分的利用度。     

LC-MS/MS法同时测定刺五加制剂中紫丁香苷、刺五加苷E和异嗪皮啶的含量

目的建立一种液相色谱-串联四级杆质谱(LC-MS/MS)法同时测定两种刺五加制剂中紫丁香苷、刺五加苷E和异嗪皮啶的含量。方法 LC采用内标法,MS采用电喷雾离子源,多反应监测模式,正负离子同时检测。3种被测成分的监测离子对分别为395.0/232.0(紫丁香苷),765.2/765.2(刺五加苷E),223.0/162.0(异嗪皮啶),内标化合物的监测离子对为431.0/311.1(牡荆苷)。色谱柱为Diamonsil C18色谱柱(4.6 mm×150 mm,5μm),流动相A为甲醇,流动相B为0.1%甲酸溶液,梯度洗脱,流速0.6 mL/min,分析时间12 min。结果刺五加注射液、刺五加片中紫丁香苷、刺五加苷E、异嗪皮啶的线性范围分别为6.00~2000 ng/mL(r=0.9979),6.00~2000 ng/mL(r=0.9951),2.00~600 ng/mL(r=0.9931);刺五加注射液的平均加样回收率(n=9)分别为104.13%,95.16%,102.64%;刺五加片的平均加样回收率(n=9)分别为102.51%,99.60%,99.15%。结论采用LC-MS/MS方法测定刺五加注射液、刺五加片中3个有效成分含量,该方法快速、简便、灵敏度高、专属性好,可作为刺五加制剂的一种质量控制评价方法。     

利用LC-MS对保健酒中七种成分的定性分析研究

分别对神酒、健身酒、海马酒这3种保健酒中是否含有红景天苷、鲁斯可皂苷元、人参皂苷Rb1、腺苷、紫丁香苷、羟基红花黄色素和山奈素这7种成分进行定性研究。用LCMS-8050分别对3种保健酒和7种成分标准品进行分析,并对所得结果进行了比较总结。结果表明,3种保健酒中均检测出红景天苷、人参皂苷Rb1、腺苷和紫丁香苷;3种保健酒中均未检测出鲁斯可皂苷元和山奈素;健身酒和神酒中检测出羟基红花黄色素。     

暴马丁香枝条中紫丁香苷提取工艺的优化及预测模型分析

采用星点设计-效应面法优化暴马丁香枝条中紫丁香苷的超声提取工艺。以乙醇体积分数、超声提取时间、溶媒比为自变量,紫丁香苷提取率为因变量,通过对自变量各水平的多元线性回归及二项式拟合,用岭嵴分析和效应面法优化出最佳的提取工艺,并进行预测分析。确定紫丁香苷最佳提取工艺为:体积分数为54.64%乙醇17.05倍量,超声提取3次,每次提取85.23 min,超声功率为80 W,温度为30℃。最佳工艺验证结果与模型预测值相差1.26%,二项式拟合的相关系数为0.9047,说明二次多项式模型可以较好地描述紫丁香苷提取率与各影响因素之间的关系,可信度大。星点设计-效应面法优化的暴马丁香枝条中紫丁香苷的提取工艺,方法简便,精密度高,质量稳定。因此,该方法可以在实际生产中予以推广使用。     

Ultrasound-Assisted Extraction of Syringin from the Bark of Ilex rotunda Thumb Using Response Surface Methodology

In this work, a rapid extraction method based on ultrasound-assisted extraction (UAE) of syringin from the bark of Ilex rotunda Thumb using response surface methodology (RSM) is described. The syringin was analyzed and quantified by high performance liquid chromatography coupled with UV detection (HPLC-UV). The extraction solvent, extraction temperature and extraction time, the three main factors for UAE, were optimized with Box-Behnken design (BBD) to obtain the highest extraction efficiency. The optimal conditions were the use of a sonication frequency of 40 kHz, 65% methanol as the solvent, an extraction time of 30 min and an extraction temperature of 40 °C. Using these optimal conditions, the experimental values agreed closely with the predicted values. The analysis of variance (ANOVA) indicated a high goodness of model fit and the success of the RSM method for optimizing syringin extraction from the bark of I. rotunda.     

新资源短梗五加及其同属植物根皮中抗疲劳因子的HPLC定量研究

目的：测定新资源短梗五加及糙叶藤五加、红毛五加、刺五加、白毛五加、韩五加、细柱五加、白簕五加等8 种五加属植物根皮中紫丁香苷的含量。方法：采用RP-HPLC 测定紫丁香苷的含量。色谱柱为ODS C18柱,流动相为20% 甲醇溶液,流速为1.0ml/min,检测波长为265nm,柱温35℃。采用正交试验法考察乙醇浓度、提取时间、溶剂用量对提取效果的影响。结果：紫丁香苷在0.0148～0.074mg/ml (r ＝ 0.9999)范围内,进样量与峰面积具有良好的线性关系,回归方程：Y ＝ 15234560X － 7881.767,R2 ＝ 0.9999,平均回收率为98.24%。8 种五加属植物中,糙叶藤五加紫丁香苷含量最高,短梗五加次之。最佳提取工艺为用水做提取剂,料液比1:15、煮沸提取3.5h。结论：本法简便,结果可靠,可用于新资源短梗五加及其同属植物的质量控制。     

超声波法提取刺五加苷B的条件研究

本文采用超声波法提取刺五加苷B,使用正交实验的方法对提取条件进行优化,确定最佳提取条件为料液比为1:20,以水为浸提剂,时间60min.超声功率650W,此条件下刺五加苷的提取率为3.68%.     

Enrichment and Purification of Syringin, Eleutheroside E and Isofraxidin from Acanthopanax senticosus by Macroporous Resin

In order to screen a suitable resin for the preparative simultaneous separation and purification of syringin, eleutheroside E and isofraxidin from Acanthopanax senticosus, the adsorption and desorption properties of 17 widely used commercial macroporous resins were evaluated. According to our results, HPD100C, which adsorbs by the molecular tiers model, was the best macroporous resin, offering higher adsorption and desorption capacities and higher adsorption speed for syringin, eleutheroside E and isofraxidin than other resins. Dynamic adsorption and desorption tests were carried out to optimize the process parameters. The optimal conditions were as follows: for adsorption, processing volume: 24 BV, flow rate: 2 BV/h; for desorption, ethanol-water solution: 60:40 (v/v), eluent volume: 4 BV, flow rate: 3 BV/h. Under the above conditions, the contents of syringin, eleutheroside E and isofraxidin increased 174-fold, 20-fold and 5-fold and their recoveries were 80.93%, 93.97% and 93.79%, respectively.     

高效毛细管电泳法测定刺五加中紫丁香苷的含量

建立刺五加中紫丁香苷的含量的测定方法。采用高效毛细管电泳法,运行缓冲液为15 mmol.L-1磷酸二氢钠-20 mmol.L-1硼砂溶液(pH8.5)。运行电压25 kV;柱温25℃;检测波长254 nm。紫丁香苷在0.012 9～0.258mg.mL-1(r0.999 8)线性关系良好,加样回收率为99.78%,RSD1.09%。方法操作简便,快速,重现性好,适用于刺五加的质量控制。