Lanxin Luo,Yan Cui,Shuting Zhang,Lingxi Li,Yuanyuan Li,Peiyu Zhou,Baoshan Sun
To develop an efficient method for large preparation of various individual polyphenols from white grape skins (Fernão Pires; Vitis vinifera ) by preparative high-speed counter-current chromatography (HSCCC) and preparative-HPLC, an optimized preparative HSCCC condition with two-phase solvent system composed of Hex-EtOAc-H 2 O (1:50:50, v/v) was used to separate grape skin polyphenols into various fractions. Both the tail-head and head-tail elution modes were used with a flow rate of 3.0 ml/min and a rotary speed of 950 rpm. Afterwards, a preparative-HPLC separation was applied to isolate individual polyphenols in each of the fractions from HSCCC. Total of 7 fractions (Fraction A to G) were obtained from grape skin extract by HSCCC. After preparative-HPLC isolation, fifteen individual compounds were obtained, most of which presented high yields and purity (all over 90%). The HSCCC method followed with preparative-HPLC appeared to be convenient and economical, constituting an efficient strategy for the isolation of grape skin polyphenols.
Stemonae Radix shows multiple pharmacological effects, mainly due to the alkaloid of tuberostemonine contained in it. An online SPE-HPLC method was fabricated by combining the solid-phase extraction (SPE) cartridge with a C18 analytical column through high-performance liquid chromatography (HPLC) system, which was used for the quantitative determination of tuberostemonine from Stemonae Radix extract and plasma. The SPE cartridge shows excellent matrix removal ability and specific selectivity for the tuberostemonine. The methodology validation confirms its good accuracy with the spiked recovery of 100.6%∼101.7%, a good repeatability with the relative standard deviations of 0.3%∼0.7% ( t R ) and 5.8%∼7.7% ( A ). Furthermore, the proposed monolithic SPE cartridge was used for the preparative separation and purification of tuberostemonine from Stemonae Radix, which was carried out on a semi-preparative HPLC instrument, with a high yield of 1.08 mg g −1 obtained. These results show that the present monolithic cartridge is an outstanding SPE adsorbent for the extraction, separation, enrichment and purification of tuberostemonine from Stemonae Radix, which can be extended to the analysis of similar alkaloids from complex samples.
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