高效毛细管胶束电泳测定血浆卡马西平浓度

目的　建立高效毛细管胶束电泳测定血浆中卡马西平浓度方法。方法　取 1mL血浆经蛋白酶处理后 ,碱性条件下用三氯甲烷提取 ,氮气吹干后 ,以电泳缓冲液溶解残渣 ,采用毛细管胶束电泳测定。电泳条件 :电泳缓冲液为 15mmol·L-1磷酸盐溶液 (pH9.4 )含SDS 2 5mmol·L-1,分离温度 2 0℃ ,分离电压 2 5kV ,检测波长 2 0 0nm ,压力进样 5s。结果　本法在 1～ 5 0μg·mL-1范围内呈良好线性和重现性 ,方法的最低测定浓度 0 .5 μg·mL-1。结论　本法有简便、快速、灵敏、干扰少的特点 ,是测定血浆中卡马西平浓度的理想方法之一     

关附壬素在Caco-2细胞上的摄取特性研究

目的:研究关附壬素在Caco-2细胞上的摄取特性.方法:采用液相色谱质谱联用(LC-MS)测定法,COSMOSIL C18柱(150 mm×2.0mm,5μm),流动相:乙腈-水(含0.2％冰乙酸)30∶70,流速0.2 mL· min-1,电喷雾离子化(ES1)方式,采用选择性离子检测法,检测离子为正离子,关附壬素的选择性离子:[M+H],m/z 388.考察了温度、药物浓度、时间和pH对关附壬素在Caco-2细胞上摄取的影响.结果:关附壬素在0.2～50.0μmol·L-1内呈良好的线性关系(r=0.9967),最低定量限为0.2 μmol·L-1.关附壬素在Caco-2细胞上的摄取具有一定的浓度、时间和pH依赖性.结论:该方法灵敏、操作简单,选择性强,关附壬素在Caco-2细胞上摄取良好,其摄取表现为被动扩散.     

高效液相色谱法测定新止咳合剂中儿茶素的含量

目的:建立高效液相色谱法测定新止咳合剂中儿茶素含量的方法。方法:采用Dikma钻石C18色谱柱(4.6mm×250mm,5μm);流动相为乙睛—0.2%磷酸溶液(8∶92);检测波长为280nm,流速为1.0ml/min,柱温为35℃。结果:儿茶素进样量在0.0425~4.25μg(r=0.99999)范围内与峰面积线性关系良好,平均加样回收率为99.05%,RSD=0.72%(n=9)。结论:本法简便、快速、专属性强、重现性好;可作为新止咳合剂的质量控制方法。     

生物分配胶束色谱法预测中药制剂消炎利胆片膜通透性的研究

目的:基于生物分配胶束色谱法进行复杂中药制剂消炎利胆片的分离和膜通透性预测。方法:考察了生物分配胶束色谱的保留因子与药物膜通透性的相关性,以非离子型表面活性剂Brij 35作为流动相,模拟生物体内环境,得到各受试药物的保留因子Log k,与膜通透性参数(口服吸收率、Log Papp、Log BB)数据进行相关分析得出定量保留-膜通透性(QRPR)模型。结果:预测了消炎利胆片10个主要保留成分的透膜吸收情况。结论:生物分配胶束色谱可以用于中药复杂成分的分离,以及预测药物主成分的透膜吸收活性。     

工业色谱法纯化山银花中绿原酸的工艺研究

目的 探索工业色谱法纯化山银花中绿原酸的最优工艺参数。方法 以绿原酸的转移率为评价指标,以山银花水提液过大孔树脂后的20%乙醇洗脱液为原料液,采用单因素及响应面设计试验,对采用工业色谱纯化山银花中绿原酸工艺中的原料液浓缩程度、固定相类型、流动相乙醇浓度、乙醇流速、进样量等主要工艺参数进行优化,确定了最优工业色谱纯化山银花中绿原酸的工艺条件。结果 工业色谱纯化山银花中绿原酸的最优工艺条件：以60℃,-0.1 MPa为浓缩条件,将原料液浓缩至原体积的0.166 7（1/6）,工业色谱UV检测波长为230 nm,以PIPO-02色谱填料为固定相,以18.54%乙醇作为流动相,流速为14.57 mL·min^-1,进样量为13.15 mg。该工艺绿原酸的平均转移率为95.49%,RSD=1.91%,绿原酸产品纯度为97.45%,RSD=3.30%。结论 经过工艺优化与验证,创立了一条工业色谱纯化山银花中绿原酸工艺路线,该工艺制备的绿原酸产品纯度>97%,绿原酸转移率高,工艺简单、无毒,溶剂易于回收,适合于山银花中绿原酸纯化的工业化生产。     

乳状液膜法提取青霉素非稳态传质数学模型的研究

在“渐进前沿模型”的基础上 ,建立并推导了乳状液膜法提取青霉素的非稳态传质数学模型。实验条件下乳状液膜法提取青霉素的过程属扩散控制 ,其阻力主要来源于膜相。青霉素在膜相中的扩散是提取过程的速控步骤     

Disposition and oxidative metabolism of phenylbutazone in man

Summary The absorption and elimination of orally administered¹⁴C-phenylbutazone and the role of oxidation in its metabolism have been studied. The main routes of excretion of¹⁴C-phenylbutazone and its metabolites were investigated in 3 patients with rheumatoid arthritis, and in 1 patient with a T-tube in the common bile duct. Up to 9 days after an oral dose of¹⁴C-phenylbutazone 600 mg (30 µCi) 63% of the radioactivity was found in the urine and 14% had appeared in the faeces. The cumulative excretion of radioactivity in bile amounted to 9.5% of the dose in 4 days. Only 1% of the radioactivity in the urine and bile was due to unchanged phenylbutazone. The role of oxidative metabolism of phenylbutazone in healthy human subjects was studied by gas chromatography. In 3 subjects given a single dose of phenylbutazone 600 mg, only 8.3% of the dose was excreted in urine as oxidized metabolites after 5 days. However, in 5 patients who had taken phenylbutazone for more than 5 weeks, these metabolites accounted for 23.4% of the dose. These results suggest that oxidative metabolism becomes more important after continued administration of the drug. After a single dose of phenylbutazone, the side-chain oxidized metabolite (II) was the major free derivative excreted in urine, but the ring oxidized metabolite, oxyphenbutazone (I), was much more important than the former in plasma. However, after prolonged treatment there was little difference between the concentration of the two metabolites in plasma. This finding suggests that side-chain oxidation is increased relative to ring oxidation on prolonged treatment with phenylbutazone. A third derivative containing hydroxyl groups both in the phenyl ring and in the side-chain (metabolite III) was found in urine in experiments with phenylbutazone, but in only one out of 3 volunteers given repeated doses of oxyphenbutazone.     

当归补血汤相状态的研究

目的:研究当归补血汤提取液的相状态。方法:通过HPLC检测阿魏酸、HPLC-ELSD检测黄芪甲苷、紫外分光光度法检测总多糖、双缩脲法检测蛋白质,并以激光衍射法检测粒径和粒径分布,结合光学现象,描述当归补血汤的相状态。结果:可以测得当归补血汤中阿魏酸、黄芪甲苷、总多糖和蛋白质的含量,提取液中分散相质点的粒径主要分布于50～100 nm和1 000 nm以上,并可以观察到明显的丁达尔现象。结论:当归补血汤含有以均相状态存在的真溶液和非均相状态存在的胶体溶液、混悬液或乳浊液,为混合分散体系。     

蓝芩口服液治疗病毒性上呼吸道感染发热疗效观察

目的观察蓝芩口服液治疗病毒性上呼吸道感染发热的治疗效果。方法130例病毒性上呼吸道感染发热患者,其中包括甲型H1N1流感确诊病例20例,疑似病例8例,临床诊断病例41例,予蓝芩口服液治疗3d,随访1d,观察退热效果和退热时间。结果治疗后,4h内退热39例（30．0％）,72h退热118例（90．8％）,平均退热时间为（23．7±14．9）h。结论蓝芩口服液治疗病毒性上呼吸道感染发热疗效确切。