AIMTo reinvestigate the chemical constituents of the ethanolic extract of Meconopsis quintuplinervia Regel which is a traditional Tibetan medicine used for treatments of hepatitis, tuberculosis etc..

METHODSThe compounds were enriched by column chromatography techniques over silica gel, macro porous resin and Sephadex LH-20 absorbents, and finally purified by reverse phase preparative HPLC methods with isocratic mobile phase systems of methanol-H2O-acetic acid (500:500:1) and acetonitrile-H2O-acetic acid (200:800:1). Structural determination of the pure compounds were based on extensive analyses of modern spectroscopic methods including IR, MS, HRMS, 1D- and 2D-NMR spectra.

RESULTSThree alkaloids were obtained and their structures were elucidated as norsanguinarine (I), O-methylflavinantine (II) and 6-methoxy-17-methyl-2, 3-[methylenebis (oxy)]-morphin-5-en-7-one (III).

CONCLUSIONNorsanguinarine (I) was isolated from genus Meconopsis for the first time, and 6-methoxy-17-methyl-2,3-[methylenebis(oxy)]-morphin-5-en-7-one (III) is a new alkaloid named as meconoquintupline.

Alkaloids ; chemistry ; isolation & purification ; Medicine, Tibetan Traditional ; Molecular Conformation ; Molecular Structure ; Morphinans ; chemistry ; isolation & purification ; Morphine Derivatives ; chemistry ; isolation & purification ; Papaveraceae ; chemistry ; Plants, Medicinal ; chemistry

OBJECTIVE: To develop a specific, sensitive, reproducible SPE-HPLC method for the determination of 37 drugs in whole blood. METHODS: With the doxapram as internal standard, Oasis column was used to extract drugs from whole blood. Two kinds of mobile phases were used in this study. Separations were achieved by a LiChrospher 100 RP-C18 (250 mm x 4.0 mm x 5 microm) column kept at 50 degrees C, the DAD detector was set at 230 nm and 250 nm. RESULTS: The limit of detection were 1-30 ng/mL. The method showed excellent linearity and the linear correlation coefficient was > or =0.997 98. The relative standard deviation for between-day and within-day assay were <10%. CONCLUSION The method is effective, simple, reliable and has been used in real cases.
Chromatography, High Pressure Liquid/methods* ; Doxapram/isolation & purification* ; Doxepin/isolation & purification* ; Estazolam/isolation & purification* ; Forensic Medicine ; Humans ; Morphine/isolation & purification* ; Papaverine/isolation & purification* ; Pharmaceutical Preparations/isolation & purification* ; Prazosin/isolation & purification* ; Procaine/isolation & purification* ; Reproducibility of Results ; Sensitivity and Specificity ; Solid Phase Extraction/methods* ; Solvents/chemistry*

The paper is to establish a method for simultaneous determination of 5 kinds of alkaloids in ephedra and poppy which are in Kechuanning tablets. Solid-phase extraction (SPE) was adopted in pretreatment, and a UPLC method with 2 different wavelengths had been developed: 210 nm for the detection of morphine, codeine phosphate, ephedrine hydrochloride and pseudoephedrine hydrochloride, and 251 nm for papaverine hydrochloride. The column used was Acquity UPLC BEH C18 (100 mm x 2.1 mm ID, 1.7 microm) with linear gradient elution using acetonitrile and 0.1% phosphoric acid. The flow rate was 0.4 mL.min-1, and the column temperature was 30 degrees C. The linear response range was 0.375 0 - 12.50 microg.mL-1 for morphine, 0.064 32 - 2.144 microg.mL-1 for codeine phosphate, 0.030 06 - 1.002 microg.mL-1 for papaverine hydrochloride, 1.126 - 37.52 microg.mL-1 for ephedrine hydrochloride, 0.287 8 - 9.592 microg.mL-1 for pseudoephedrine hydrochloride (r = 0.999 7). The average recoveries of these compounds were 99.26%, 100.6%, 95.29%, 100.1% and 97.48%, respectively. This is a more reasonable and credible method of quality control for Kechuanning tablets.
Alkaloids ; analysis ; Chromatography, High Pressure Liquid ; Codeine ; analysis ; Drugs, Chinese Herbal ; administration & dosage ; chemistry ; isolation & purification ; Ephedra ; chemistry ; Ephedrine ; analysis ; Morphine ; analysis ; Papaver ; chemistry ; Papaverine ; analysis ; Plants, Medicinal ; chemistry ; Pseudoephedrine ; analysis ; Quality Control ; Solid Phase Extraction ; Tablets