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1.
J Chromatogr Sci ; 58(7): 591-599, 2020 Jul 24.
Article in English | MEDLINE | ID: mdl-32537638

ABSTRACT

Microemulsion eluents have been found to have excellent potential uses in high-performance liquid chromatography (HPLC). Here, a novel, environmentally benign and simple method using concentration/flow-rate double-gradient elution using a microemulsion eluent was used to separate water- and fat-soluble vitamins simultaneously and rapidly. Preliminary screening experiments were performed to determine the optimum column type, surfactant concentration, co-surfactant to surfactant ratio, oil, mobile phase pH and microemulsion concentration. The resolution and analysis time were simultaneously optimized using concentration/flow-rate double-gradient elution. The optimized method simultaneously separated water- and fat-soluble vitamins using a Venusil ASB C8 column and a combination of isocratic and linear gradient elution modes using a microemulsion mobile phase (solvent A) consisting of 3.5% (w/w) sodium dodecyl sulfate, 10.5% (w/w) n-butanol, 0.8% (w/w) n-octanol and 85.2% (w/w) water and water (solvent B) at pH 2.50. The optimum detection wavelength was 283 nm. The method was validated and used to analyze a solid pharmaceutical sample.


Subject(s)
Chromatography, High Pressure Liquid/methods , Emulsions/chemistry , Vitamins/analysis , Vitamins/isolation & purification , 1-Butanol/chemistry , Hydrogen-Ion Concentration , Limit of Detection , Linear Models , Reproducibility of Results , Sodium Dodecyl Sulfate/chemistry , Solubility , Vitamins/chemistry , Water/chemistry
2.
Article in English | MEDLINE | ID: mdl-28985481

ABSTRACT

In this study, we analyzed danshen (Salvia miltiorrhiza) constituents using biopartitioning and microemulsion high-performance liquid chromatography (MELC). The quantitative retention-activity relationships (QRARs) of the constituents were established to model their pharmacokinetic (PK) parameters and chromatographic retention data, and generate their biological effectiveness fingerprints. A high-performance liquid chromatography (HPLC) method was established to determine the abundance of the extracted danshen constituents, such as sodium danshensu, rosmarinic acid, salvianolic acid B, protocatechuic aldehyde, cryptotanshinone, and tanshinone IIA. And another HPLC protocol was established to determine the abundance of those constituents in rat plasma samples. An experimental model was built in Sprague Dawley (SD) rats, and calculated the corresponding PK parameterst with 3P97 software package. Thirty-five model drugs were selected to test the PK parameter prediction capacities of the various MELC systems and to optimize the chromatographic protocols. QRARs and generated PK fingerprints were established. The test included water/oil-soluble danshen constituents and the prediction capacity of the regression model was validated. The results showed that the model had good predictability.


Subject(s)
Chromatography, High Pressure Liquid/methods , Drugs, Chinese Herbal/chemistry , Drugs, Chinese Herbal/pharmacokinetics , Salvia miltiorrhiza/chemistry , Abietanes/blood , Abietanes/chemistry , Abietanes/pharmacokinetics , Animals , Area Under Curve , Benzofurans/blood , Benzofurans/chemistry , Benzofurans/pharmacokinetics , Cinnamates/blood , Cinnamates/chemistry , Cinnamates/pharmacokinetics , Depsides/blood , Depsides/chemistry , Depsides/pharmacokinetics , Emulsions/chemistry , Male , Rats , Rats, Sprague-Dawley , Reproducibility of Results , Surface-Active Agents/chemistry , Rosmarinic Acid
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