Optimization of Extraction Process of Clerodendrum philippinum Schauer var. simplex Mlodenke Total Flavonoids(CPTF) by Central Composite Design-Response Surface Methodology

[Objectives] The research aimed to optimize extraction process of Clerodendrum philippinum Schauer var. simplex Mlodenke total flavonoids( CPTF),and provide reference for its development and utilization. [Methods] Based on single-factor test,ethanol concentration,extraction temperature and extraction time were taken as independent variables,and total flavonoids yield was taken as dependent variable. The test was conducted according to central composite design principle. Multivariate linear regression and binomial equation fitting of the result were conducted,and extraction process of CPTF was optimized by using response surface methodology. [Results]The optimal extraction process of CPTF was as below: ethanol concentration 54. 76%,extraction temperature 83. 92℃,extraction time 102. 64 min,solid-liquid ratio 1:20,extraction for twice. [Conclusions] The extraction process of CPTF by central composite design-response surface methodology was simple and feasible,with reliable prediction result,which was suitable for industrial production.

Optimization of Extraction Process of Total Flavonoids from Akebia trifoliata (Thunb.) Koidz. by Central Composite Design-Response Surface Methodology

[Objectives]To optimize extraction process of total flavonoids from Akebia trifoliata( Thunb.) Koidz.,so as to provide references for development and use of Akebia trifoliata( Thunb.) Koidz. [Methods]The extraction rate of total flavonoids of Akebia trifoliata( Thunb.)Koidz. was taken as observation indicator. On the basis of single factor experiment,central composite design( CCD) was used to evaluate the effects of the extraction temperature,extraction time,and ethanol concentration on the extraction process. Multiple linear regression and binomial fitting were used,and response surface methodology( RSM) was used to select the optimum extraction process. [Results] The optimum extraction process conditions for total flavonoids of Akebia trifoliata( Thunb.) Koidz. was extraction temperature: 83. 92 ℃; extraction time:96. 47 min; ethanol concentration: 63. 92%; extraction times: two times; solid to liquid ratio: 1 ∶ 20; extraction rate of total flavonoids:4. 55%. [Conclusions] The central composite design-response surface methodology( CCD-RSM) is simple,convenient,and feasible for extraction of total flavonoids from Akebia trifoliata( Thunb.) Koidz.,and the prediction results are reliable.

Optimization and characterization of nimesulide bilayer tablets by response surface methodology

The objectives of this present investigation were to develop and formulate nimesulide bilayer tablets by using different polymer combinations and fillers, to optimize the formulations for different drug release variables by orthogonal design and central composite design-surface methodology and to evaluate drug release pattern of the optimized product. The bilayer tablet containing a fast release layer（FRL） and a sustained release layer（SRL） provided an initial burst release of nimesulide, followed by the sustained release for a period of time. The optimal formulation obtained was as follows：（I） the formulation of FRL： nimesulide, 50 mg; lactose, 92 mg; starch, 22 mg; CCMC-Na, 14 mg; PVP K30, 1 mg; micronized silica gel, 1 mg; magnesium stearate, 0.9 mg; and iron oxide red, 0.1 mg; and（II） the formulation of SRL： nimesulide, 150 mg; HPMC K100LV, 26 mg; HPMC K4M, 33 mg; lactose, 54 mg; PVP K30, 1 mg; micronized silica gel, 1 mg; and magnesium stearate, 0.9 mg. According to the optimal formulation, the biphasic type of release was identified. The in vitro drug dissolution from the bilayer tablets was sustained for about 16 h after releasing 15% of drug in the first 10 min. The developed nimesulide bilayer tablets with improved efficacy can perform therapeutically better than the conventional tablets.

直肠用美沙拉嗪温敏凝胶的制备及质量评价

目的 制备一种具有缓释和保留性能,用于直肠给药的美沙拉嗪温敏凝胶(MZ-Gel)。方法 以胶凝温度为评价指标,采用星点设计-响应面法对泊洛沙姆407和泊洛沙姆188的用量进行优化。以Franz扩散池法进一步考察体外释药行为,得到最佳处方并对其进行质量评价。结果 MZ-Gel优化处方为P407 22.56%,P188 3.34%,胶凝温度为(32.8±0.3)℃;MZ-Gel的体外释药符合一级动力学特征,具有缓释效果;胶凝时间平均值为38.3 s,pH平均值为4.07,膨胀系数平均值为4.81%,持水率平均值为99.78%;红外表征表明,美沙拉嗪的加入并没有破坏温敏凝胶结构。结论 此方法制备工艺简单,性质稳定且具有良好的体外释药特征。

星点设计-效应面法优化赪桐根总黄酮提取工艺及含量测定

目的研究赪桐根中总黄酮提取工艺的优化及含量测定,为赪桐药材的资源开发利用提供理论和实验基础。方法以赪桐根中总黄酮的含量为考察指标,通过单因素试验考察复合酶的用量、酶解温度、酶解时间等因素对赪桐根总黄酮含量的影响。在单因素试验的基础上,再采用星点设计-效应面法考察复合酶的用量、酶解温度、酶解时间3个自变量之间相互作用对提取赪桐根中总黄酮含量的影响。通过对以上3个自变量各水平的多元线性回归及二项式拟合,用星点设计-效应面法选取最佳的提取工艺,并进行预测分析。同时,采用星点设计-效应面法优化赪桐总黄酮得到的最佳提取工艺制备不同产地赪桐根的供试样品,经显色后,以芦丁做对照,在波长为500 nm下测定吸光度。结果赪桐根总黄酮最佳提取工艺为酶的用量是0.35%,酶解温度为62℃,酶解时间为125.7 min。在此优化条件下,总黄酮含量的预测值为10.37 mg/g。总黄酮含量测定结果说明不同产地的赪桐根中的总黄酮含量有较大的差异。结论采用星点设计-效应面法优化复合酶酶解赪桐根总黄酮提取工艺条件合理、稳定可行,操作简便、快捷,为测定赪桐根中总黄酮的提取工艺提供科学依据。不同产地药材因生长环境、湿度、阳光、温度等因素对赪桐根中总黄酮含量有较大的影响。

星点设计-效应面法优化五味黄连洗液的水提工艺研究

目的优化五味黄连洗液的提取工艺。方法以加水倍数、提取时间为主要考察因素,以栀子苷、黄芩苷、黄连碱、盐酸小檗碱和干浸膏得率的综合评分为评价指标,采用星点设计-响应面法结合单因素法优化提取工艺,并进行验证试验。结果最优提取工艺为浸泡40 min,13倍水,提取2次,每次提取132 min。验证试验实测值与预测值的偏差为3.63%。结论星点设计-效应面法可用于五味黄连洗液提取工艺的优化,所建模型预测性好,所得工艺稳定可靠。

八角茴香精油的超临界萃取工艺研究

采用超临界CO;萃取八角茴香精油,利用单因素试验及响应面法对工艺进行优化,优化后的工艺条件为萃取温度37℃,萃取压力17 MPa,CO;流量25 L/h,萃取时间95 min,在此条件下,八角茴香精油平均收率为9.1%。通过试验验证,响应曲面分析法适用于超临界CO;萃取八角茴香精油的工艺研究,有效减少了试验次数,降低了试验成本。

星点设计响应面法优化纳米结构脂质载体载辛伐他汀的研究

目的利用星点设计响应面法优化制备纳米结构脂质载体载辛伐他汀的最佳制备条件。方法 采用星点设计响应面法,以乳剂的平均粒径、多分散指数和zeta电位为评价指标,考察处方中自变量OA浓度、P188浓度和微射流次数对制剂的影响,预测出最优制备条件。结果 优选出的最佳制备条件:OA浓度为40%(wt%),P188浓度为0.4%(w/v%),微射流机循环次数为4次。依据最佳制备条件完成纳米结构脂质载体载辛伐他汀的制备,平均粒径为174.7 nm,包封率94.1%,实际载药量18.2。结论 星点设计响应面分析法所建立的模型能较好地用于纳米结构脂质载体载辛伐他汀的处方优化,纳米结构脂质载体可以很好地实现SV包裹。

星点设计-效应面法优化蒿甲醚自微乳释药系统

目的研究蒿甲醚自微乳释药系统(SMEDDS)的制备优化及体外评价。方法通过溶解度实验、伪三元相图的绘制及星点设计-效应面法,以粒径、Zeta电位和平衡溶解度为指标,筛选最优处方,并对蒿甲醚自微乳的理化性质和体外释药进行评价。结果蒿甲醚自微乳最优处方为:Cremophor RH40为39.29%、Transcutol HP为35.71%、MCT为25%;其平均粒径为24.52 nm,Zeta电位为-10.10 m V,平衡溶解度>88 mg/g。结论应用星点设计-效应面优化法得到蒿甲醚SMEDDS的最优处方,显著提高蒿甲醚的溶解度和体外溶出度。

微波水解-液相色谱-原子荧光光谱法测定硒蛋白中的硒代氨基酸

针对酶解法测定硒代氨基酸操作复杂,时间长,水解不完全且水解产物不稳定等问题,建立一种微波水解-液相色谱-原子荧光光谱仪测定硒蛋白中硒代氨基酸的方法。样品经HCl(6 mol/L)微波水解后,调节pH值至7.5,采用阴离子色谱柱,pH=6.0的(NH_(4))_(2)HPO_(4)(40 mmol/L)溶液为流动相,流速0.6 mL/min,等度洗脱12 min的条件对硒代胱氨酸(SeCys_(2))、甲基-硒代半胱氨酸(MeSeCys)和硒代蛋氨酸(SeMet)进行分离,用原子荧光光谱仪测定其含量。微波水解条件采用星点设计-响应面法进行优化,优选最佳水解条件为:称样量20 mg,水解温度150℃,水解时间40 min。SeCys_(2)、MeSeCys和SeMet均在0~100 ng浓度范围内呈线性关系,相关系数均大于0.999,检出限分别为0.07、0.03和0.14 mg/kg,RSD分别为5.6%、4.6%、3.7%(n=6)。用来测定硒代氨基酸,耗时短,成本低,水解完全,操作简单,水解产物稳定,能够科学评价硒蛋白中硒代氨基酸的组成,对硒蛋白产品的质量控制和溯源提供了科学方法,值得推广应用。

星点设计-响应面法优化黄芪多糖提取工艺实验研究

建立黄芪多糖最佳提取工艺。通过单因素试验与正交设计试验,应用Box-Behnken中心组合试验设计和响应面(RSM)分析法,以黄芪多糖得率为响应值,回归分析黄芪多糖提取的影响因素,优选黄芪多糖提取工艺。结果表明正交设计与响应面法优化结果接近,所得黄芪多糖的最佳提取条件为:提取时间40min,水提取温度100℃,液料比(mL/g)40∶1。此方法对黄芪多糖提取条件的优化合理可行,为简化黄芪多糖提取工艺以及提高黄芪多糖得率提供了依据,且预测性良好。

Characterization of stereostructure by X-ray and technology of extracting in combination hydrolysis in situ of acankoreanogenin from leaves of Acanthopanax gracilistylus W.W.Smith

To study the stereostructure by X-ray and the technology of extracting acankoreanogenin from the leaves of Acanthopanax graeilistylus W. W. Smith （AGS）, the crystal structure was measured with a Bruker APEX-Ⅱ area-detector diffractometer instrument and the technology of extracting in combination hydrolysis in situ （ECHS） was compared with these of traditional methods. The crystal belongs to the monoclinic system, space group P2b with unit cell parameters： a=（8.3652±0.0006） nm, b=（24.721±0.002） nm, and c=（14.5587±0.0011） nm, α=90°, β=97.850 （4） °, γ=90 °, V=2982.51 nm3, Dc= 1.179 mg/m3, and the molecular number （Z） of elementary structures was 2. The comparisons show that the extraction rate of acankoreanogenin with ECHS methods is much higher than that of traditional methods. Then, central composite design-response surface methodology （CCD-RSM） was adopted for optimizing the extraction rate of ECHS methods. The optimized values of extraction parameters are as follows： for the for extraction process of acid hydrolysis are that extraction time 110.8 min, solvent-herb ratio 11.5 and acid content 5.25%; the best extraction process of basic hydrolysis are that extract time 120 min, solvent-herb ratio 8.7 and the alkali content 8.79%. Finally, the extracts were purified with decolorizing carbon after alkali solution and acid-isolation and purity of acankoreanogenin was 98.7%.

星点设计-效应面法优化酒制巴戟天的炮制工艺

目的以水晶兰苷为指标建立酒制巴戟天最佳炮制工艺。方法采用星点设计-效应面法以辅料黄酒用量、润药时间为考察因素,水晶兰苷的含量变化为评价指标,优化酒蒸巴戟天的炮制工艺。结果星点设计-效应面法优化酒制巴戟天的最佳炮制工艺为:辅料黄酒用量为10%(g/g)、浸润时间为1 h,蒸透,干燥。结论以黄酒用量、浸润时间为考察因素,水晶兰苷为评价指标的响应面法能够用于优化酒蒸巴戟天的最佳炮制工艺。

辛烯基琥珀酸淀粉钠黄连素颗粒剂的制备

使用辛烯基琥珀酸淀粉钠为掩味剂对黄连素进行颗粒剂制备,以溶出度为指标,采用星点设计―响应面法对黄连素颗粒剂制备工艺进行优化。实验结果表明,颗粒剂最佳制备工艺为辛烯基琥珀酸淀粉钠与黄连素投料比为0.94∶1(g/g),制粒温度为33.6℃,干燥时间为150.33 min。在此条件下,黄连素颗粒溶出度为86.92%,与预测值相近。三个因素对黄连素颗粒剂溶出度值的影响依次是:投料比>干燥时间>制粒温度。制备得到的黄连素颗粒剂干燥,色泽一致,味微苦,无结块等现象,粒度范围在355±15μm。研究可为黄连素颗粒剂在临床上的应用奠定基础。