Separation of three anthraquinone glycosides including two isomers by preparative high‐performance liquid chromatography and high‐speed countercurrent chromatography from<i>Rheum tanguticum</i>Maxim. ex Balf

Aqueous two‐phase flotation followed by preparative high‐performance liquid chromatography was used to separate four flavonol glycosides from Solanum rostratum Dunal. In the aqueous two‐phase flotation section, the effects of sublation solvent, solution pH, (NH4)2SO4 concentration in aqueous solution, cosolvent, N2 flow rate, flotation time, and volumes of the polyethylene glycol phase on the recovery were investigated in detail, and the optimal conditions were selected: 50 wt% polyethylene glycol 1000 ethanol solvent as the flotation solvent, pH 4, 350 g/L of (NH4)2SO4 concentration in aqueous phase, 40 mL/min of N2 flow rate, 30 min of flotation time, 10.0 mL of flotation solvent volume, and two times. After aqueous two‐phase flotation concentration, the flotation products were purified by preparative high‐performance liquid chromatography. The purities of the final products A and B were 98.1 and 99.0%. Product B was the mixture of three compounds based on the analysis of high‐performance liquid chromatography at the temperature of 10°C, while product A was hyperoside after the identification by nuclear magnetic resonance. Astragalin, 3’‐O‐methylquercetin 3‐O‐β‐d‐galactopyranoside, and 3’‐O‐methylquercetin 3‐O‐β‐d‐glucopyranoside were obtained with the purity of 93.8, 97.1, and 99.2%, respectively, after the further separation of product B using preparative high‐performance liquid chromatography.

Section: Introductionmentioning

confidence: 99%

Separation of four flavonol glycosides from Solanum rostratum Dunal using aqueous two‐phase flotation followed by preparative high‐performance liquid chromatography

Lin

Shao

et al. 2016

“…Aloe‐emodin‐1‐ O ‐β‐ d ‐glucoside ( 37 ), aloe‐emodin‐8‐ O ‐β‐ d ‐glucoside ( 50 ), emodin‐1‐ O ‐β‐ d ‐glucoside ( 62 ) and emodin‐8‐ O ‐β‐ d ‐glucoside ( 70 ) were identified comparing with the retention times in the literature . Likewise, compound 61 and 64 were identified as chrysophanol‐1‐ O ‐β‐ d ‐glucoside and chrysophanol‐8‐ O ‐β‐ d ‐glucoside accordingly .…”

Section: Resultsmentioning

confidence: 98%

Chemical profiling and quantification of ShenKang injection, a systematic quality control strategy using ultra high performance liquid chromatography with Q Exactive hybrid quadrupole orbitrap high‐resolution accurate mass spectrometry

Zuo

Sun

et al. 2017

ShenKang injection is traditional Chinese medicine used to treat chronic renal failure in China. It is a compound preparation that consists of four herbs: Rhubarb, Salvia miltiorrhiza, Safflower and Radix Astragali. We developed an ultra high pressure liquid chromatography coupled with Q Exactive hybrid quadrupole-orbitrap high resolution accurate mass spectrometry tandem mass spectrometry method to analyze its chemical compositions, and a total of 90 compounds were identified from ShenKang injection. Among them, 19 major compounds were unambiguously detected by comparing with reference standards. Meanwhile, 13 representative compounds selected as quality control markers were simultaneously quantified in ShenKang injection samples. Chromatographic separation was accomplished on a Waters ACQUITY HPLC® HSS C column using gradient elution. The method was validated with respect to linearity, sensitivity, accuracy and precision, reproducibility and stability. And the validated method was successfully applied for simultaneous determination of 13 bioactive compounds in ShenKang injection from ten batches of samples by liquid chromatography with mass spectrometry. The results were analyzed by principal components analysis method, and three compounds had a significant relationship with the quality control of ShenKang injection. This research established a rapid and reliable method for the integrating quality control, including qualitation and quantification of ShenKang injection.

“…An appropriate two‐phase solvent system could be achieved through the measurement of partition coefficient. In general, the solvent system should satisfy these rules : (1) form a stable two‐phase solvent system, (2) the sample should not be decomposed and denatured, (3) solubility of samples should be high enough, (4) the sample should have suitable partition coefficient ( K ) in the solvent system, and (5) the setting time of the two‐phase solvent system should be less than 30 s and the retention of the stationary phase should be over 40%.…”

Section: Resultsmentioning

confidence: 99%

Isolation and purification of alkaloids from lotus leaves by ionic‐liquid‐modified high‐speed countercurrent chromatography

Xie

Fang

et al. 2017

An effective high-speed countercurrent chromatography method was successfully established by using ionic liquids as the modifier of the two-phase solvent system. Adding a small amount of ionic liquids significantly shortens the separation time and improves the separation efficiency. The conditions of ionic-liquid-modified high-speed countercurrent chromatography including solvent systems, types and content of added ionic liquids, and ionic liquids posttreatment were investigated. The established method was successfully applied to separate alkaloids from lotus leaves using a two-phase solvent system composed of petroleum ether/ethyl acetate/methanol/water/[C mim][BF ] (1:5:1:5:0.15, v/v/v/v/v). Four alkaloids pronuciferine (1.7 mg), N-nornuciferine (4.3 mg), nuciferine (3.1 mg), and roemerine (2.1 mg) were obtained with the purities of 90.53, 92.25, 99.86, and 98.63%, respectively, from 100 mg crude extract of lotus leaves. The results indicated that the ionic-liquid-modified high-speed countercurrent chromatography method was suitable for alkaloid separation from lotus leaves and would be a promising method for the separation of alkaloids from other natural products.