RP-HPLC测定勒马回胶囊中原儿茶酸的含量

勒马回胶囊是由水蔓菁经加工制成，是由勒马回片经剂改而研制成功的新药，原勒马回片标准收载于卫生部药品标准中药成方制剂第十八册。关于水蔓菁中化学成分的报道较少，目前已有文献报道从中分离出环烯醚萜类和黄酮类化合物，本试验对勒马回胶囊化学成分作了进一步研究，通过DAD检测以及LC／MS联用进行结构确证，在勒马回胶囊中发现了原儿茶酸。现代药理实验表明，原儿茶酸具有增加冠脉流量等生理活性，因此，选择原儿茶酸作为含量测定指标，对控制本制剂的内在质量很有意义。参照文献方法，采用高效液相色谱法测定勒马回胶囊中原儿茶酸的含量，经方法学考察和对3批样品含量测定的结果表明，本法简便、灵敏、准确、重现性好，可作为本品内在质量控制的有效方法。     

高效液相色谱法测定人肝细胞色素P450 3A4转基因细胞中氨氯地平

目的 :研究氨氯地平经人肝细胞色素 P4 5 0 3A4 (CYP3A4 )的代谢 ,建立反相高效液相色谱的测定人肝转基因细胞 CYP3A4酶 S9孵育液中氨氯地平浓度的方法。方法 :与人肝转基因细胞提取的 S9上清液孵育之后的样品 ,用 3倍量的甲醇沉淀后离心 ,取上清液用 0 .4 5μm微孔滤膜滤过后进样。采用 Hypersil C18柱 ,以乙腈 -磷酸盐缓冲液 (4 5∶ 5 5 ,v/ v,p H4 .5 )为流动相 ,普萘洛尔为内标 ,在 2 5 0 nm波长处测定。结果 :氨氯地平浓度在 0 .2～ 30 .0μg/ ml范围内线性关系良好 ,r=0 .9993,方法平均回收率为 (98.2± 2 .4 ) % (n=5 ) ,日内和日间相对标准偏差(RSD)均小于 10 % ,检测限为 2 0 ng/ ml,定量限为 0 .2 μg/ ml(回收率为 10 4 .0 % ,RSD为 11.4 % ,n=5 )。结论 :建立的反相高效液相色谱方法简便、准确 ,可用于研究氨氯地平在人肝 CYP3A4转基因细胞中的代谢。     

Extraction of organic acids by ion-pair extraction with tri-n-octylamine - VIII. Identification of synthetic dyes in pharmaceutical preparations

Synthetic dyes were extracted from syrups, oral suspensions, tablets, gelatin capsules, suppositories and granules by ion-pair formation with tri-n-octylamine (TnOA) and back-extracted with perchlorate ions. Identification was performed by TLC on cellulose layers and by reversed phase ion-pair HPLC.     

Analysis of neomycins A, B and C by high-performance liquid chromatography with post-column reaction detection

The analysis of the antibiotics neomycins A, B and C was investigated. The separation of the components was studied using reversed-phase and reversed-phase ion-pair chromatography. The optimum separation was obtained utilizing a Lichrosorb RP-2 column with a mobile phase consisting of 75 mg/l sodium dodecyl sulphate, 0.5M Na2SO4 and 0.015 M sodium acetate buffer at pH 7.0. Using this mobile phase, baseline separation was obtained for all three compounds in approximately 20 min. Detection was via post-column derivatization of the analytes with ortho-phthalaldehyde in the presence of mercaptoethanol to form fluorescent iso-indole products. This system is applied to the analysis of a number of formulated products containing neomycin.     

The influence of bile salts on the absorption in vitro and in vivo of propranolol

The lipophilicity of propranolol is increased by some bile salts which form ion-pairs. In the presence of taurodeoxycholate, the logarithm of the apparent partition coefficient (log P) of propranolol is increased. Moreover, the apparent diffusion constants in vitro of propranolol as ion-pairs at pH 3.0–6.0 are about 5–6 times higher than those of propranolol alone.

The area under the curve values of plasma concentration—time profiles of propranolol, following its oral administration to rabbits together with taurodeoxycholate, are about 1.4 times higher than those after administration of propranolol alone. Moreover, after the admistration of propranolol with taurodeoxycholate the plasma concentration rises more rapidly, with a point of inflection between 0.5 and 1.5 h, than after administration of propranolol alone.

Taurodeoxycholate does not modify the first-pass effect of propranolol in rabbits following intravenous and intraportal administration. The absorption of an oral dose of propranolol in the presence of taurodeoxycholate increases from 70% to 100%, due to the higher lipophilicity of the ion-pair. The plasma concentration—time curves suggest the hypothesis that greater absorption of the ion-pair occurs mainly in the upper region of the gastrointestinal tract.     

RP—HPLC测定清眩丸中欧前胡素的含量

目的：建立反相高效液相色谱测定清眩丸中欧前胡素含量的方法。方法：采用乙醇做溶剂,水浴加热回流提取。ＬＵＮＡ－Ｃ１８色谱柱分离测定,流动相为乙腈－水（５３∶４７）,流速１ｍＬ·ｍｉｎ－１,检测波长３００ｎｍ。结果：欧前胡素与其相邻峰的分离度是１５,理论板数按欧前胡素峰计算是１６１５５,欧前胡素对照品线性范围是１４６２～４８７５μｇ·ｍＬ－１,加样平均回收率９８０％。结论：用本文方法测定清眩丸中欧前胡素的含量,操作简便,结果准确。     

血栓素B2的高效液相荧光测定及刺五加提取物的抗血小板作用

本文在Turk及Wintersteiger荧光衍生实验的基础上,建立了反相HPLC法测定血小板TXB₂含量的方法.血小板TXB₂用Sep-PakC₁₈提取,在冠醚和碳酸钾存在下,BrMmc与TXB₂的羧基反应生成BrMmc-TXB₂。然后经Zorbax-ODS柱(250mm×4.6mm,5μm)分离,测定荧光强度(E×345,Em405)。流动相为乙腈:水:磷酸(60:40:0.1V/V),流速1ml/min.BrMmc-TXB₂的分离在20min内完成。TXB₂的含量用外标法定量,检测限15ng。体外实验刺五加提取物(0.275～2.2mg/mlPRP)对AA、ADP诱导的家兔血小板聚集有明显的抑制作用,并能抑制AA诱导的血小板TXB₂的生成。静脉注射(120mg/kg)对AA、ADP诱导的聚集也有抑制作用。     

细辛脑片剂的生物利用度

目的 :比较两种不同生产工艺的细辛脑片剂生物利用度。方法 :18名健康志愿者单剂量随机交叉口服不同生产工艺的片剂 1和片剂 2 16 0mg ,及静脉注射细辛脑针剂 16mg后 ,用反相高效液相色谱法测定细辛脑血清浓度 ,对AUC0～∞ ,Cmax和Tmax3个参数进行等效性检验。结果 :片剂 1和片剂 2的绝对生物利用度分别为 (5 .4± 1.6 ) %和 (9.7± 2 .5 ) % ,片剂 2对片剂 1的相对生物利用度为 (181.9± 15 .2 ) %。结论 :经生产工艺改造后的片剂 2生物利用度比原生产工艺片剂 1提高81.9% ,但是 ,细辛脑片剂的绝对生物利用度仍很低。