动态轴向压缩色谱法制备高纯度芍药苷

本文建立动态轴向压缩色谱法分离制备高纯度芍药苷的方法。白芍提取物采用90%乙醇经MCI柱洗脱除杂富集后,采用动态轴向压缩色谱柱分离,以Daisogel C_(18),10μm为填料,甲醇-水系统为洗脱剂,对芍药苷进行纯化。运用HPLC对芍药苷进行含量测定。制备所得芍药苷纯度达96.14%。该方法操作简便、快速、高效,为制备高纯度的芍药苷提供了一条新途径。     

HPLC测定当归芍药散中的芍药苷和芍药内酯苷的含量

目的:建立同时测定当归芍药散中芍药苷和芍药内酯苷含量的方法。方法:采用全波长HPLC,COSMOSIL 5C_(18)-MS-Ⅱ柱(4.6×250mm,5μm),流动相:0.1%H_3PO_4溶液-乙腈(体积比86∶14),检测波长为230nm,柱温为30℃,流速为1mL·min~(-1)。结果:芍药苷和芍药内酯苷分别在7.24～36.20μg·mL~(-1),4.08～20.40μg·mL~(-1)线性关系良好,平均回收率分别为99.00%,96.80%。结论:该法简便、准确、灵敏、重现性好,可用于当归芍药散中芍药苷和芍药内酯苷的同时测定。     

HPLC法测定芍药花瓣中紫云英苷的含量

建立芍药花瓣中紫云英苷含量的检测方法。采用HPLC法测定芍药花瓣中紫云英苷的含量,色谱柱为InertsilODS-3,流动相为乙腈-0. 1%磷酸梯度洗脱,检测波长347nm。紫云英苷在0. 05～0. 75μg范围内线性良好,r=0. 9997,平均回收率分别为98. 07%(n=6)。建立的方法简便可行,专属性强,可以用于芍药花瓣的质量研究。     

回生口服液中主要成分的鉴别研究

回生口服液作为一种抗癌新药,为了更好的保证回生口服液的质量,采用薄层色谱法对处方中起主要作用的大黄素、大黄酚、丁香酚、吴茱萸、盐酸水苏碱、人生皂苷Re、芍药苷进行定性鉴别。同时,采用HPLC法对主要成分大黄素及大黄酚进行了定量测定。由此建立的定性定量方法简便、准确,可作为回生口服液质量控制的方法。     

高效液相色谱法测定消炎利胆冲剂中芍药苷的含量

采用超声法提取消炎利胆冲剂中的芍药苷,建立了高效液相色谱法测定芍药苷含量的方法。采用Agilent ZORBAX SB-C18色谱柱(250mm×4.6mm,5μm),柱温26℃,流动相为0.2%磷酸溶液-甲醇(58∶42,体积比),流速1.0mL·min-1,检测波长230nm。结果表明:在2.016~336μg·mL-1的范围内芍药苷浓度与峰面积呈良好的线性关系,平均回收率为100.42%,RSD为0.97%。该方法简便、准确、重复性好,可用于消炎利胆冲剂中有效成分芍药苷的含量测定。     

HPLC法测定宫炎康颗粒中芍药苷的含量

建立了宫炎康颗粒中芍药苷的含量测定方法。采用反相高效液相色谱法,YMC pack ODS-A C18色谱柱（150 mm×4.6 mm,5μm）;乙腈-0.1%磷酸溶液（12.5∶87.5）为流动相;检测波长为230 nm,流速1.0 mL·min-1。结果表明：芍药苷在0.222－2.220μg范围内与峰面积呈良好线性关系,r=0.9999,芍药苷平均加样回收率为99.19%,RSD为0.56%,精密度、稳定性良好。本方法可靠性高,分离度、准确性、重复性好,适用于宫炎康颗粒中芍药苷的含量测定。     

高效液相色谱法测定亳芍中芍药苷的含量研究

建立亳芍中芍药苷含量的HPLC测定方法。方法:采用岛津VP-ODS C18色谱柱(5μm,250mm×4.6mm),流动相为0.1%磷酸溶液-乙腈(80∶20,V/V),流速为1.0mL/min,检测波长为230nm,柱温为室温。结果:在0.028mg/mL～0.142mg/mL范围内芍药苷的量与其峰面积呈良好的线性关系,平均加样回收率为98.3%。结论:采用HPLC测定亳芍中芍药苷的含量简便、准确、选择性好,可用于亳芍中芍药苷的含量测定。     

HPLC测定达原饮中的芍药苷和黄芩苷的含量

目的:建立同时测定达原饮中芍药苷和黄芩苷含量的方法。方法:采用双波长HPLC,Aglient ZORBAX SB-C_(18)柱(4.6×250mm,5μm);流动相:0.2%H3PO4溶液-甲醇(体积比50∶50);检测波长分别为230nm(芍药苷)和280nm(黄芩苷);柱温为30℃;流速为1m L·min~(-1)。结果:芍药苷和黄芩苷分别在9.69~155.04μg·m L~(-1),18.66~298.56μg·m L~(-1)线性关系良好,平均回收率分别为99.03%,98.98%,RSD分别为1.95%,1.67%。结论:该法简便、准确、灵敏、重现性好,可用于达原饮中芍药苷和黄芩苷含量的同时测定。     

芍药苷及芍药内酯苷在超临界CO_2中无限稀释扩散系数的测定与计算

在温度308.15~328.15 K,压力10~18 MPa,运用Taylor峰扩展法测定了芍药苷及芍药内酯苷在超临界CO_2中无限稀释扩散系数,两组分的扩散系数均随温度升高而增大,随压力升高而减小,随改性剂乙醇含量的增加而减小,并建立了芍药苷与芍药内酯苷的扩散系数与超临界CO_2的密度关联方程。分别采用修正的Wilke-Chang、Lusis-Ratcliff、Hayduck-Minhas模型和Dymond-Hildbrand-Batschinski(DHB)模型预测了芍药苷及芍药内酯苷在夹带乙醇的超临界CO_2中的三元扩散系数,与实验测定值对比表明,DHB模型的预测效果最好,对芍药苷及芍药内酯苷的平均绝对偏差分别为3.11%和4.96%。     

HPLC法测定归芍护肝颗粒中芍药苷的含量

建立测定归芍护肝颗粒中芍药苷含量的方法。采用HPLC-UV法,Aglient ZORBAX SB-C18柱(4.6×250 mm,5μm);流动相为乙腈-0.1%磷酸溶液(14:86,v/v)为流动相;检测波长为230 nm;柱温为30℃;流速为1 m L/min。芍药苷在10~100μg/m L范围内线性关系良好,平均回收率为98.79%,RSD分别为0.92%。该法简便、准确、灵敏、重现性好,可用于归芍护肝颗粒中芍药苷含量的测定。     

巯嘌呤口服混悬液有关物质的HPLC法测定

建立了HPLC法测定巯嘌呤口服混悬液中的有关物质,以加校正因子的自身对照法定量。采用Uitimate Phenyl-Ether色谱柱,以0.04%甲酸∶甲醇为流动相,等度洗脱,检测波长260 nm。计算有关物质的相对校正因子(RCF),以此计算有关物质含量,并与对照品法测定结果比较,以验证方法的准确性。结果主成分巯嘌呤与相邻杂质,以及各杂质之间均分离良好,RCF法与对照品法测定结果无显著性差异。已知杂质2、3的相对保留时间分别为0.56和4.33,相对校正因子分别为0.16和0.23,2和3的平均加样回收率为104.2%和95.3%,RSD为3.2%和2.9%。本方法重复性好、灵敏度高,适用于巯嘌呤口服混悬液中有关物质的分析。     

Enhanced hypoglycemic effect of biotin-modified liposomes loading insulin: effect of formulation variables,intracellular trafficking,and cytotoxicity

Peroral protein/peptide delivery has been one of the most challenging, but encouraging topics in pharmaceutics. This article was intended to explore the potential of biotin-modified liposomes (BLPs) as oral insulin delivery carriers. By incorporating biotin-DSPE into the lipid bilayer, we prepared BLPs using reverse evaporation/sonication method. We investigated hypoglycemic effects in normal rats after oral administration of BLPs, and the possible absorption mechanism by a series of in vitro tests. The relative pharmacological bioavailability of BLPs was up to 11.04% that was as much as 5.28 folds of conventional liposomes (CLPs). The results showed that the enhanced oral absorption of insulin mainly attributed to biotin ligand-mediated endocytosis. The results provided proof of BLPs as effective carriers for oral insulin delivery.     

Oral HPV Infection and Sexuality: A Cross-Sectional Study in Women

Human Papillomavirus (HPV) is the main risk factor for cervical cancers and is associated with close to 36% of oropharyngeal cancers. There is increasing evidence that oral HPV transmission is related to sexual behavior but to our knowledge studies that involve women who have sex with women have not been performed. We examined the prevalence of oral HPV according to sexual behavior among a population-based sample of 118 women and have made some inferences of possible predictors of oral HPV infection. Women were categorized as heterosexual (history of vaginal sex and/or oral sex with males only, n = 75), bisexual (history of vaginal sex and oral sex with females, n = 32) and other (no history of vaginal sex but oral sex with females [homosexuals], virgins and women with incomplete sexual exposure data, n = 11) The prevalence of oral HPV infection was 12/118 (10.2%) for the overall study population and was not significantly different between heterosexual and bisexual women (10.7% (8/75) vs. 12.5% (4/32), p = 0.784). There was no oral HPV detected among homosexual women, virgins or among women where sexual exposure was unknown. Never smokers were more likely to be oral HPV+ compared to former smokers (Adjusted Odds Ratio (Adj OR) = 0.1, 95% CI, 0.0-1.1) and there was no difference in risk between never smokers and current smokers (Adj OR = 0.7, 95% CI, 0.1-4.6). Twenty-five percent (3/12) of oral HPV+ women had a history of HPV and/or genital warts compared to 9% (10/106) of oral HPV-women (p = 0.104). For the women with a history of vaginal sex (n = 110), oral HPV status was statistically significantly different according to oral sex exposure (p = 0.039). A higher proportion of oral HPV-positive women reported that they had no history of oral sex exposure compared to oral HPV-negative women (4/12, 33% vs. 7/98, 8%). The prevalence of cervical HPV infection did not vary between heterosexuals and bisexuals (35.7% (25/70) vs. 35.5% (11/31), p-value 0.411) and for all other women the cervical HPV prevalence was significantly lower (11.1%, 1/9). Our study suggests that smoking and sexual behavior involving males rather than female partners may be possible predictors of oral HPV infection in women. Further studies with larger sample size are needed to confirm these findings.     

液相色谱-串联质谱法测定人血浆中左旋氨氯地平

建立一种快速灵敏的液相色谱-串联质谱方法测定人血浆中左旋氨氯地平。分析样品经液-液萃取后,通过Zorbax SB C18柱进入质谱,内标为尼莫地平。标准曲线的线性范围0．05～20ng／mL,日内日间精密度小于7．4％,准确度在±1．1％之间,该方法成功应用于22名健康受试者口服5mg左旋氨氯地平的药动学研究。     

高效液相色谱法同时测定口腔护理用品中3种抗菌药物

建立高效液相色谱（ HPLC）同时测定口腔护理用品中3种抗菌药物含量的分析方法。试样经甲醇水溶液超声提取后,以甲醇-磷酸盐缓冲溶液为流动相,经C18柱分离后进行HPLC检测。3种药物在2.0mg/L-100mg/L范围内呈良好的线性关系,线性相关系数均大于0.999。20、40、100 mg/kg 3个浓度加标水平的平均回收率为97.2%-103.7%,相对标准偏差（RSD,n=6）为1.28%-2.36%,检出限为2.5 mg/kg-5.0mg/kg。该方法灵敏度高、重现性好、定量准确。     

Novel preparation of PLGA/HP55 nanoparticles for oral insulin delivery

The aim of the present study was to develop the PLGA/HP55 nanoparticles with improved hypoglycemic effect for oral insulin delivery. The insulin-loaded PLGA/HP55 nanoparticles were produced by a modified multiple emulsion solvent evaporation method. The physicochemical characteristics, in vitro release of insulin, and in vivo efficacy in diabetic rats of the nanoparticles were evaluated. The insulin encapsulation efficiency was up to 94%, and insulin was released in a pH-dependent manner under simulated gastrointestinal conditions. When administered orally (50 IU/kg) to diabetic rats, the nanoparticles can decrease rapidly the blood glucose level with a maximal effect between 1 and 8 h. The relative bioavailability compared with subcutaneous injection (5 IU/kg) in diabetic rats was 11.3% ± 1.05%. This effect may be explained by the fast release of insulin in the upper intestine, where it is better absorbed by the high gradient concentration of insulin than other regions. These results show that the PLGA/HP55 nanoparticles developed in the study might be employed as a potential method for oral insulin delivery.     

基于正交试验的桔梗多糖口服液的研制

桔梗具有丰富的药理和保健功能。采用超声辅助法提取桔梗多糖,通过正交试验得到最优化配方为桔梗多糖0.6%、白砂糖3%、蜂蜜3%、柠檬酸0.1%,复合稳定剂配方为:瓜尔豆胶0.06%、CMC-Na 0.06%、黄原胶为0.07%,添加0.02%的山梨酸钾,得到的桔梗多糖口服液为淡黄色澄清液体,味道酸甜适口,口感圆润,各项质量指标均符合相应的标准。     

Rapid and Sensitive Determination of Timosaponin AIII in Rat Plasma by LC-MS/MS and Its Pharmacokinetic Application

A rapid sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for determination of timosaponin AIII (TA-III) in rat plasma, using ginsenoside Re as an internal standard (IS). TA-III and the IS were detected in MRM mode with a negative ionization electrospray mass spectrometer. The calibration curves were linear over the concentration ranges from 11.14 to 1114 ng/mL and the lower limit of quantification (LLOQ) was 11.14 ng/mL. Intra-day and inter-day precisions (RSD) were within 10%, and accuracy ranged from 6.4% to 9.1%. The extraction recovery at three concentrations ranged from 92.3% to 95.5%. The validated method was successfully applied to monitor the concentrations of TA-III in rat plasma after intragastric administration. The best fit pharmacokinetic model to estimate the pharmacokinetic parameters was a single compartment model with weight of 1/x² for oral administration groups of rats for TA-III.     

载胰岛素壳聚糖微球口服降血糖作用的研究

为了研制一种生物利用度高且具有缓释作用的口服胰岛素制剂,采用静电液滴工艺制备载胰岛素壳聚糖-海藻酸钙微球,以四氧嘧啶为诱导剂建立糖尿病小鼠模型,采用葡萄糖氧化酶法测定小鼠血糖含量,对载药微球的口服药效学进行评价。结果表明:载胰岛素微球平均粒径48μm,药物包封率94.1%,胰岛素相对活性71.7%;药效学研究表明,口服高(4.8 IU/kg)、中(3.6 IU/kg)、低(2.4 IU/kg)3种剂量胰岛素微球,糖尿病小鼠相对血糖值口服6 h时降至最低,分别为42.69%,59.8%,76.13%,药理相对生物利用度为41.20%,37.76%,35.81%。口服载胰岛素壳聚糖-海藻酸钠微球具有降血糖作用和显著的缓释作用,药理相对生物利用度高。