正交试验法优选延胡索中延胡索乙素提取工艺

摘 要 目的：优选延胡索中延胡索乙素的最佳提取工艺。方法: 选用L9（34）正交试验设计,以提取物中延胡索乙素的含量为指标,考察乙醇浓度、乙醇用量、提取温度和提取时间对提取效果的影响。结果: 最佳提取工艺为按料液比1∶10（g·ml^-1）加入浓度为60%的乙醇溶液,以80 °C为提取温度,加热回流提取3 次,每次1 h。结论: 优选得到提取工艺稳定、合理、可行、操作简单,能耗低,较大限度地提高了延胡索的综合利用率。     

延胡索乙素的制备方法研究

目的 寻找制备延胡索乙素的高效方法.方法 采用先从黄藤中提取巴马汀、再还原成延胡索乙素的的方法制备,所得产品经核磁共振鉴定.结果 制备得到的延胡索乙素纯度超过97％.结论 黄藤中巴马汀经硼氢化钠还原后可制备成高纯度的延胡索乙素.     

响应曲面法优化延胡索中延胡索乙素的提取工艺

目的以延胡索乙素为指标成分对中药延胡索的提取工艺进行优化,以利于工业化生产。方法采用响应曲面法对提取工艺进行优化,通过考察乙醇体积分数、提取时间、溶媒用量及其交互作用对中药延胡索中延胡索乙素提取率的影响。模拟得出了延胡索乙素的提取回归方程,确定了延胡索乙素的最佳提取条件。结果优化得到的最佳工艺参数:乙醇体积分数为87.16%,提取时间为105.13 min,液料比为1∶7.13。在该工艺条件下,提取物中延胡索乙素的含量质量分数为0.183%。结论该提取工艺对延胡索提取物中的延胡索乙素提取优化效果显著,方法稳定、可行。     

HPLC法测定延胡索中延胡索乙素的含量

目的:对延胡索中的延胡索乙素进行含量测定。方法:采用HPLC法,以C₁₈-ODS为色谱柱,甲醇 0.1%磷酸(用三乙胺调pH至6.0)( 60∶40)为流动相,检测波长为280nm。结果:延胡索乙素的量在0.257～2.056μg范围内线性良好,回收率为99.03% ,RSD为0.51%。结论:该方法简便、可靠,适合延胡索的质量控制。     

延胡索和左旋延胡索乙素的条件性位置偏爱效应

目的:观察延胡索和左旋延胡索乙素(l-THP)是否具有精神依赖性。方法:80只大鼠随机分为延胡索高、中、低剂量组,l-THP高、中、低剂量组,生理盐水对照组,吗啡组。前6组大鼠每天分别灌胃(ig)延胡索生药0.5、1.0、2.0g·kg-1,l-THP1.0、2.0、4.0mg·kg-1,吗啡组每天皮下注射(sc)吗啡(10mg·kg-1),生理盐水对照组给予等体积生理盐水,进行条件性位置偏爱(conditioned place preference,CPP)训练,时间10d。结果:高、中、低剂量延胡索和l-THP组大鼠在伴药箱中的停留时间均无明显延长,且同一组大鼠在伴药箱中的停留时间与训练前比,差异也无显著性,未形成CPP;而吗啡组对伴药箱明显形成CPP。结论:延胡索和l-THP不具有精神依赖性,无成瘾性。     

延胡索及其制剂复方镇痛丸中延胡索乙素的薄层扫描法测定

延胡索及其制剂复方镇痛丸中延胡索乙素的薄层扫描法测定深圳市药品检验所５１８０２６熊英，邬晓鸥复方镇痛丸是由延胡索、香附、苍术等１５味药材制成的复方制剂，用于治疗各种癌症引起的疼痛，延胡索是其中的君药。关于延胡索药材中延胡索乙素的含量测定，有容量法、分...     

薄层扫描法测定痛经宁贴剂中延胡索乙素的含量

采用薄层扫描法,对痛经宁中延胡索的有效成分延胡索乙素进行含量测定,回收率为96.97％,RSD为0.90％。     

薄层扫描法测定乳泰囊中延胡索乙素含量

采用薄层扫描法,以酸提碱沉法提取样品中的生物碱,用1％NaOH硅胶G薄层板,石油醚－乙酸乙酯（2：17）为展开剂分离各类生物碱,用CS－9000型薄层扫描仪,在λs=278nm,λR=360nm处用双波长反射锯齿形扫描不, 定乳泰胶囊中延胡索乙素的含量。平均回收率99．5％（n=4),RSD=5.8%。     

RP-HPLC法测定元胡饮片中延胡索乙素的含量

<正>延胡索为罂粟科植物延胡索(Corydalis yanhusuo W.T.Wang)的干燥块茎,又称"元胡";功效活血,行气,镇痛,用于胸胁、脘腹疼痛,胸痹心痛,经闭痛经,产后瘀阻,跌扑肿痛。元胡饮片常用醋制延胡索,目的是引药入经增强其镇痛功     

延胡索醋炙前后饮片和煎剂中延胡索乙素的含量比较

目的 比较延胡索醋炙前后饮片和煎剂中延胡索乙素的含量变化.方法 采用高效液相色谱法,对延胡索醋炙前后饮片和煎剂中延胡索乙素的含量进行测定.结果 延胡索醋炙后,饮片中延胡索乙素含量降低3.70%,但在煎剂中延胡索乙素的含量提高18.18%.结论 醋炙对于延胡索饮片中延胡索乙素的含量影响较小,但可以明显增加其在煎剂中的溶出.     

介质研磨法制备他达拉非纳米混悬液研究

目的:采用介质研磨法制备他达拉非纳米混悬液,以提高他达拉非的溶出度和生物利用度。方法:以粒径、多分散指数(PDI)、Zeta电位和物理稳定性为评价指标,优化处方和工艺参数;采用扫描电镜(SEM)、X-射线粉末衍射法(XRPD)、差示扫描量热法(DSC)对样品进行表征,HPLC法测定他达拉非纳米混悬液体外溶出度,UPLC-MS/MS法检测大鼠中他达拉非的血药浓度。结果:他达拉非纳米混悬液最优处方为他达拉非质量分数2%、HPC 1%和SDS 0.1%;最优工艺为粒径0.1 mm氧化锆珠,转速3 000 r·min^-1,研磨时间30 min。制备的他达拉非纳米混悬液PDI为0.173±0.013,Zeta电位为(－22.6±0.4) mV,纳米颗粒为棒状结晶,粒径为(218.2±1.3) nm,分布均匀,晶型稳定;体外溶出度10 min内达到99%,大鼠体内生物利用度为原料药的4.01倍,在室温条件下放置6个月稳定性良好。结论:介质研磨法制备他达拉非纳米混悬液方法简单,产品稳定性好,能显著提高他达拉非溶出度和生物利用度。     

Preparation and storage stability of rutin nanosuspensions

Formulations of the rutin nanosuspensions have been prepared by high pressure homogenization (HPH). A Micron LAB 40 was used for HPH to obtain rutin nanosuspensions. Photon correlation spectroscopy (PCS) and laser diffraction were employed to analyze the particle size. Morphology of the particles was analyzed by light microscopy. The HPH technique produced rutin nanosuspensions having PCS size average of 547–912 nm and zeta potential range about ?30 mV in water. Aqueous rutin nanosuspension stabilized by SDS and Tween 80 were stable over 12 months. The nanosuspensions produced via HPH not only could prevent large particle size and particle growth, but also protect the drugs from chemically degradation. The molecules of the surface stabilizer are able to shield the chemical compound. The crystalline structure in a nanoparticulate sized formulation results in improved drug chemical-stability.     

番荔素纳米混悬剂的制备及其抗肿瘤作用研究

目的 制备高载药量番荔素纳米混悬剂（ACGs-NSPs）,并研究其对小鼠乳腺癌4T1移植肿瘤的生长抑制作用,为强效抗肿瘤药物ACGs的临床应用提供可用注射剂型。方法 番荔素、TPGS、SPC（质量比7:5:2）采用超声-沉淀法制备ACGs-NSPs,并用动态光散射法测定ACGs-NSPs的粒径,透射电镜观察其形态;稳定剂TPGS、SPC组成比例对ACGs-NSPs的溶血性考察;透析法考察其体外释放;采用MTT比色法评价ACGs-NSPs对4T1细胞细胞毒性;建立4T1乳腺癌皮下小鼠肿瘤模型,以紫杉醇注射液（PTX）为阳性对照,考察不同剂量ACGs-NSps静脉注射给药对4T1肿瘤的抗肿瘤药效。结果 ACGs-NSPs为表面光滑的球形,平均粒径为(129.03±1.03）nm,多分散指数PDI为0.134±0.03,zeta为（-17.7±0.16）mV,HPLC法测得番荔素线性回归方程为Y=0.157 2 X-0.363 2（R²=0.999）,在5~200 μg/mL范围内显性关系良好,载药量高达（45.03±0.72）%;体外释放较为缓慢;MTT试验中,ACGs-NSPs对4T1乳腺癌的细胞毒性显著强于游离药物（IC⁵⁰,3.221 μg/mL vs 4.464 μg/mL,P<0.05）;4T1荷瘤小鼠的药效学实验中,ACGs-NSPs表现出剂量相关性的抑瘤作用,高、中、低剂量组（0.4、0.2、0.1 mg/kg）抑瘤率分别为76.09%、74.34%、42.03%;但高剂量组小鼠有死亡（3/10）。结论 成功制备高载药量的ACGs-NSPs,且其对4T1乳腺癌有显著的抑制作用;从药效和小鼠存活率来看,0.2 mg/kg为合适的给药剂量。     

Enhancement of oral bioavailability of quercetin by metabolic inhibitory nanosuspensions compared to conventional nanosuspensions

Quercetin-loaded nanosuspensions (Que-NSps) added metabolic inhibitors were evaluated as drug delivery system to promote the oral bioavailability of quercetin. Que-NSps were prepared respectively using d-alpha tocopherol acid polyethylene glycol succinate (TPGS) or Soybean Lecithin (SPC) as stabilizer. On the basis, Piperine (Pip) or sodium oleate (SO) was, respectively, encapsulated in Que-NSps as phase II metabolic inhibitors. The resulting Que-NSps all displayed a mean particle size of about 200 nm and drug loading content was in the range of 22.3–27.8%. The release of quercetin from Que-NSps was slow and sustained. After oral administration of 50 mg/kg different Que-NSps, the levels of free quercetin in plasma were significantly promoted, the concentration of quercetin metabolites (isorhamnetin and quercetin 3-O-β-d-Glucuronide) were decreased. The absolute bioavailability was, respectively 15.55%, 6.93%, 12.38%, and 23.58% for TPGS-Que-NSps, TPGS-SO-Que-NSps, SPC-Que-NSps, and SPC-Pip-Que-NSps, and 3.61% for quercetin water suspension. SPC-Pip-Que-NSps turned out to an ideal nanocarrier combined nano drug delivery system together with metabolic inhibitor to promote oral absorption of quercetin.     

夫西地酸纳米混悬剂原位凝胶的制备与评价

目的制备夫西地酸纳米混悬剂原位凝胶并评价其质量。方法采用反溶剂沉淀-超声法制备夫西地酸纳米混悬剂,并通过单因素实验考察了纳米混悬剂的处方和制备工艺;以泊洛沙姆作为凝胶基质将夫西地酸纳米混悬剂制备成原位凝胶,并以泊洛沙姆407 (P407)与泊洛沙姆188 (P188)的质量浓度作为考察因素,以凝胶化温度作为评价指标,采用星点设计-效应面法优化原位凝胶处方,得到满足凝胶化温度范围的设计空间;评价了夫西地酸纳米混悬剂的外观形态、粒径分布和Zeta电位等理化性质;比较了夫西地酸原料药、夫西地酸纳米混悬剂以及原位凝胶的体外药物释放行为。结果制备的夫西地酸纳米混悬剂平均粒径为335.7±34.5 nm,多分散性指数(PdI)为0.216±0.015,Zeta电位为-9.4±0.8 mV;扫描电镜下显示夫西地酸纳米混悬剂呈球形或近球形分布;通过实验优化得到夫西地酸纳米混悬剂原位凝胶的设计空间,在设计空间内任取一点:P407的质量浓度为22.0 mg·mL~(-1),P188的质量浓度为6.0 mg·mL~(-1),凝胶温度为34.0℃;夫西地酸纳米混悬剂与原料药相比释药速度及程度显著提高,1 h内药物累积释放完全,而原位凝胶可减慢夫西地酸纳米混悬剂的释药速率。结论将夫西地酸制备成纳米混悬剂,可提高药物溶解度,改善药物释放速度,进一步制备成原位凝胶有望提高药物的治疗效果。     

HPLC法测定延胡索中延胡索乙素的含量

目的：对延胡索中的延胡索乙素进行含量测定。方法：采用ＨＰＬＣ法,以１８－ＯＤＳ为色谱柱,甲醇－０．１％磷酸（用三乙胺调ＰＨ至６．０）（６０：４０）为流动相,检测波长为２８０ｎｍ。结果：延胡索乙素的量在０．２５７－２．０５６μｇ范围内线性良好,回收率为９９．０３％,ＲＳＤ为０．５１％,结论：该方法简便、可靠,适合延胡索的质量控制。     

HPLC法测定胃安颗粒中延胡索乙素的含量

目的建立胃安颗粒中延胡索乙素的含量测定方法.方法采用高效液相色谱法测定胃安颗粒中延胡索乙素的含量.色谱柱:Hypersil C18柱(4.6mm×250mm,5μm);流动相:甲醇-0.1%磷酸溶液(55∶45);流速:1mL·min-1;柱温:室温;检测波长:280nm.结果延胡索乙素在0.193～0.965μg范围内,进样量与峰面积呈良好的线性关系(r=0.9992),平均回收率为96.59%,RSD=1.99%.结论本法准确、专属性强、重现性好,可作为胃安颗粒中延胡索乙素的含量测定方法.     

HPLC测定痛经软膏中延胡索乙素的含量

目的测定痛经软膏中延胡索乙素的含量。方法采用HPLC法,色谱柱为ODS柱,流动相为pH7.4磷酸盐缓冲液-甲醇(40:60),流速1.0 m l.m in-1,柱温35℃,检测波长280 nm。结果精密度和稳定性均良好;线性范围0.0448~0.2240mg.m l-1(r=0.9999),平均回收率99.2%;分离度符合要求。结论所建方法简便、专属、重复性好。     

高效液相色谱法测定抗乳腺小叶增生合剂中延胡索乙素的含量

目的建立HPLC法测定抗乳腺小叶增生合剂中延胡索乙素的含量。方法采用VP-ODS柱（4．6mm×250mm。5μm）为分析柱。以甲辞．0．1％磷酸溶液（三乙胺调pH值至6．0）（55：45）为流动相,流速1．0mL·min-1,检测波长为280nm．柱温：30℃。结果延胡索乙素的浓度在9．84～98．4μg·mL-1范围内线性关系良好（r=0．9999）．平均回收率为99．57％,RSD为1．30％（n=6）。结论HPLC法操作简便,快速,结果可靠。可用于抗乳腺小叶增生合剂的质量控制。     

Preparation and evaluation of nanosuspensions for enhancing the dissolution of poorly soluble drugs

Poorly water-soluble compounds are difficult to develop as drug products using conventional formulation techniques and are frequently abandoned early in discovery. In the present study, the melt emulsification method traditionally used to prepare solid lipid nanoparticles was adapted to produce drug nanosuspensions. The method was evaluated in comparison with the well known solvent diffusion process for ibuprofen as a model drug. Control of the preparation variables (stabilizers, drug content, homogenization procedure and cooling conditions) allowed formation of nanosuspensions with diameters less than 100 nm. The major advantage of the melt emulsification method over the solvent diffusion method is the avoidance of organic solvents during production, although the mean particle size is slightly greater. The combination of Tween 80 and PVP K25 as stabilizers yields nanosuspensions with the smallest average particle size. The formulation of ibuprofen as a nanosuspension, either in the form of lyophilized powder or granules, was very successful in enhancing dissolution rate, more than 65% of the drug being dissolved in the first 10 min compared to less than 15% of the micronized drug. The increase in in vitro dissolution rate may favourably affect bioavailability and improve safety for the patient by decreasing gastric irritancy.