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高效液相色谱-超滤法测定常氧及缺氧大鼠血浆中毛蕊花糖苷的蛋白结合率 被引量:1
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作者 王维刚 王芃 +5 位作者 李晓琳 王俊丽 刘天龙 陈升富 李茂星 阳志强 《中药新药与临床药理》 CAS CSCD 北大核心 2021年第12期1839-1844,共6页
目的建立毛蕊花糖苷血浆蛋白结合率的测定方法,比较常氧及缺氧大鼠血浆中毛蕊花糖苷蛋白结合率的异同。方法将大鼠置于低压低氧动物实验舱中,于海拨7 500 m下缺氧暴露3 d制备缺氧大鼠模型。采用超滤法处理样品,结合高效液相色谱(HPLC)... 目的建立毛蕊花糖苷血浆蛋白结合率的测定方法,比较常氧及缺氧大鼠血浆中毛蕊花糖苷蛋白结合率的异同。方法将大鼠置于低压低氧动物实验舱中,于海拨7 500 m下缺氧暴露3 d制备缺氧大鼠模型。采用超滤法处理样品,结合高效液相色谱(HPLC)法测定常氧及缺氧大鼠血浆中毛蕊花糖苷游离型药物浓度(Cf)和总药物浓度(Ct),并考察超滤膜非特异性结合率(NSB),对Cf进行矫正后,计算血浆蛋白结合率。结果大鼠血浆中毛蕊花糖苷浓度为3、6、12μg·mL^(-1)时,毛蕊花糖苷与常氧大鼠血浆的蛋白结合率分别为(62.02±8.51)%、(60.17±5.59)%和(62.60±3.77)%;与缺氧大鼠血浆的蛋白结合率分别为(32.79±4.20)%、(33.16±1.74)%和(32.72±2.20)%,两者比较差异有统计学意义(P<0.05)。结论毛蕊花糖苷与常氧大鼠血浆蛋白属于中强度结合,且在研究的浓度范围内,不具浓度依赖性,而毛蕊花糖苷与缺氧大鼠血浆蛋白结合强度明显低于常氧大鼠血浆。 展开更多
关键词 毛蕊花糖苷 高效液相-超滤 常氧 缺氧 血浆蛋白结合率 大鼠
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金芪降糖片与牛血清白蛋白结合作用的超滤-色谱联用技术研究 被引量:3
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作者 夏娜 邓雁如 +2 位作者 金华 丁菲菲 曹颖 《时珍国医国药》 CAS CSCD 北大核心 2013年第8期1804-1807,共4页
目的研究金芪降糖片中成分与牛血清白蛋白(BSA)的结合作用。方法采用超滤法与高效液相色谱联用技术对金芪降糖片、金银花、黄连药材中成分与BSA的结合率进行测定;考察pH值对金芪降糖片、金银花、黄连药材与BSA结合作用的影响。结果金芪... 目的研究金芪降糖片中成分与牛血清白蛋白(BSA)的结合作用。方法采用超滤法与高效液相色谱联用技术对金芪降糖片、金银花、黄连药材中成分与BSA的结合率进行测定;考察pH值对金芪降糖片、金银花、黄连药材与BSA结合作用的影响。结果金芪降糖片中9种成分新绿原酸、隐绿原酸、绿原酸、咖啡酸、表小檗碱、黄连碱、盐酸药根碱、盐酸巴马汀及盐酸小檗碱与BSA结合作用明显;有机酸与生物碱成分与BSA结合存在置换作用。结论金芪降糖片中成分与牛血清白蛋白有较强的结合。该研究为研究药物在体内的药动学、药效学及临床用药提供了实验依据。 展开更多
关键词 金芪降糖片 牛血清白蛋白 结合率 超滤-高效液相色谱
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藏药材诃子中3种α-葡萄糖苷酶抑制剂的分离与鉴定 被引量:7
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作者 马家麟 陈涛 +2 位作者 谭亮 王环 李玉林 《天然产物研究与开发》 CAS CSCD 北大核心 2020年第8期1357-1362,1356,共7页
通过超滤-高效液相色谱法筛选诃子提取物中具有α-葡萄糖苷酶抑制活性的化合物,采用大孔吸附树脂和半制备高效液相色谱对其进行富集和分离制备,1H NMR和13C NMR鉴定其化学结构,最后采用以4-硝基酚-α-D-吡喃葡萄糖苷(pNPG)为底物的酶抑... 通过超滤-高效液相色谱法筛选诃子提取物中具有α-葡萄糖苷酶抑制活性的化合物,采用大孔吸附树脂和半制备高效液相色谱对其进行富集和分离制备,1H NMR和13C NMR鉴定其化学结构,最后采用以4-硝基酚-α-D-吡喃葡萄糖苷(pNPG)为底物的酶抑制剂筛选模型检测目标化合物的活性。结果显示:诃子提取物中含有的3个主要成分具有潜在的α-葡萄糖苷酶抑制活性;经筛选,AB-8大孔树脂对目标化合物富集效果最好,富集后目标化合物的峰面积比分别达到29.6%、40.3%和21.9%;由半制备高效液相色谱对目标化合物进一步纯化后,得到纯度分别为96.6%、98.1%和96.4%的化合物1(27 mg)、2(35 mg)和3(22 mg);经1H NMR和13C NMR鉴定得出3个化合物分别为诃黎勒酸、诃子酸、鞣花酸;活性测试结果表明,3个化合物均具有良好的α-葡萄糖苷酶抑制作用,其中诃黎勒酸(IC50=39.2±0.7 mg/L)和诃子酸(IC50=35.8±0.4 mg/L)抑制活性大于阳性对照阿卡波糖(IC50=41.2±0.6 mg/L)。本试验为开发诃子中的α-葡萄糖苷酶抑制剂提供了科学依据。 展开更多
关键词 诃子 Α-葡萄糖苷酶抑制剂 超滤-高效液相色谱 分离 鉴定
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Ultrafiltration of Shiitake Polyphenol with Ultrasound Enhancement
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作者 Defang SHI Hong GAO +3 位作者 Xiuzhi FAN De YANG Shujing XUE Wei CHENG 《Agricultural Science & Technology》 CAS 2015年第10期2243-2246,共4页
Ultrafiltration (UF) experiments were subjected to the concentration of Shi- itake polyphenol(SP) with ultrasound (US) enhancement, by which the effects of the main parameters such as ultrasonic power, transmemb... Ultrafiltration (UF) experiments were subjected to the concentration of Shi- itake polyphenol(SP) with ultrasound (US) enhancement, by which the effects of the main parameters such as ultrasonic power, transmembrane pressure, temperature and axial flow-rate on the membrane fluxes were analyzed, and then the SP of the ultrafiltrate after follow-up resin adsorption by HPLC was investigated. The results in- dicated that US could significantly enhance the membrane fluxes. The optimal con- ditions obtained was as follows: 0.60 W/cm2 US power, axial flow-rate of 80 L/h, operation temperature 30 ~C, transmembrane pressure 0.10 MPa. US increased the absorption capacity of the absorbent resin during the following stage. The HPLC analysis also showed that catechins were purified to some extent as the ultrafiltrate was treated by US and macroporous resin, indicating the technology of US en- hancement coupled with UF showed the potential for concentration and purification of SP by absorbent resins. 展开更多
关键词 SHIITAKE ULTRAFILTRATION ULTRASOUND
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Development of a simple and rapid method to measure the free fraction of lamotrigine in plasma using HPLC:applications for therapeutic drug monitoring 被引量:1
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作者 Huanxin Wang Yaxin Sun +3 位作者 Shansen Xu Tong Lu Yanan Chen Limei Zhao 《Journal of Chinese Pharmaceutical Sciences》 CAS CSCD 2018年第12期832-839,共8页
Lamotrigine (LTG) is a widely used antiepileptic drug (AED) for the treatment of new-onset, as well as refractory epilepsy. Due to the narrow treatment window and large individual variability in the pharmacokinetics a... Lamotrigine (LTG) is a widely used antiepileptic drug (AED) for the treatment of new-onset, as well as refractory epilepsy. Due to the narrow treatment window and large individual variability in the pharmacokinetics and pharmacodynamics of LTG, therapeutic drug monitoring (TDM) is necessary in clinical practice to guide dose adjustments. Individual differences and drug combinations can also affect protein binding rate, which further affects the unbound concentration of LTG. The unbound fraction is more closely related to adverse reactions and therapeutic efficacy than total concentration. Therefore, it may be more meaningful to determine the unbound LTG concentration in plasma than the total concentration.Unbound LTG in plasma was extracted by ultrafiltration. High-performance liquid chromatography (HPLC) was used to measure unbound LTG concentration. This method was validated by studies of its selectivity, linearity, lower limit of quantification (LLOQ), accuracy, precision, recovery, and stability.The method was validated over a linear range of 0.2 to 10.0 μg·mL–1, and its LLOQ was 0.2 μg·mL–1. The method’s relative standard deviations (RSDs) for intra-day and inter-day precision were less than 15%, and its accuracy (RE) was ±4.69%. The recoveries of unbound LTG at three different concentrations satisfied the requirements for the analysis of biological samples, and no significant degradation of LTG was observed under different storage conditions.A simple HPLC method showed good performance when used to measure unbound LTG concentration. This method might be used to study the relationship between unboundLTG concentrations and its effectiveness according to TDM. 展开更多
关键词 LAMOTRIGINE Unbound concentration ULTRAFILTRATION HPLC Therapeutic drug monitoring
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