A rapid and efficient method for the identification of antioxidants in the traditional Chinese medicine Polygalae Radix (PR) by HPLC–ESI-Q-TOF-MS/MS is described. The method is based on the hypothesis that upon reaction of antioxidants with 1,1-diphenyl-2-picrylhydrazyl (DPPH), the peak areas of compounds with potential antioxidant activities in the HPLC chromatogram will be significantly reduced in comparison to the untreated sample. The identity confirmation was achieved by Q-TOF-MS/MS technique. With this method, eight components were proposed possessing potent antioxidant activity. They were identified as sibiricose A5, sibiricose A6, sucrose monoester, polygalaxanthone III, tenuifoliside B, 3',6-disinapoylsucrose (DISS), sucrose diester , tenuifoliside C, respectively. DISS was proposed to be the most potent one. The antioxidant activity of DISS was evaluated by DPPH, ABTS radical scavenging assay and ferric-reducing antioxidant power (FRAP) assay in vitro. Vitamin C (Vc) was used as positive control substance. DISS showed moderate DPPH (DISS's IC 50 value was 1024.17 μg/mL, Vc's was 294.68 μg/mL) and ABTS (IC 50 324.13 μg/mL, Vc's was 117.50 μg/mL) free radical scavenging capacity and ferric-reducing antioxidant power. DISS can be used as a new source of natural antioxidant in foods and cosmetics.
Xi Zhou,Huiqin Wu,Xiaolan Huang,Fang Hang,Huitai Luo
This study established a simple and rapid method for simultaneous determination of short-chain chlorinated paraffins (SCCPs) and medium-chain chlorinated paraffins (MCCPs) in human serum by high performance liquid chromatography coupled with electron spray ionization quadrupole time-of-flight mass spectrometry (HPLC-ESI-Q-TOF/MS). A simple pretreatment procedure of protein precipitation by acetonitrile coupled with liquid-liquid extraction by n-hexane was employed for extraction and purification . The purified samples were separated by a PFP chromatographic column. This method could effectively eliminate the matrix effect by lipids and other matrix substances in serum samples with less time and solvent consuming. 76 congener groups of SCCPs and MCCPs with C 10 -C 17 and Cl 5 -Cl 13 were quantified by their [M-H] − ions. Method detection limit (MDL) were 1.0–8.0 ng mL −1 for ∑SCCPs and ∑MCCPs. Recoveries were 98.4 ± 4.42%, 98.8 ± 3.96% and 90.7 ± 2.79% for SCCPs and 93.1 ± 6.67%, 108 ± 1.21% and 90.8 ± 3.78% for MCCPs at spiking concentrations of 20, 50 and 200 ng·mL −1 , respectively. The relative standard deviations (RSDs) of intra- and inter-day variations were 1.41% and 9.84% for SCCPs, and 4.23% and 6.26% for MCCPs. The suitability of the developed method was demonstrated through the application to analysis of SCCPs and MCCPs in human serum samples.
Background Zengye decoction (ZYD) has been widely used in the treatment of type 2 diabetes mellitus (T2DM). Exploring the fate of various components of ZYD in vivo is of considerable significance for pharmacological research and molecular mechanism elaboration. However, the systematic analysis on the metabolic behavior of chemical components of ZYD in T2DM rats has not been reported. Methods To screen and characterize the complex chemical compositions of ZYD, and metabolism fate in plasma, urine, bile, and feces of T2DM rats, the model of T2DM rats was prepared. A rapid procedure using high-performance liquid chromatography coupled with electrospray ionization quadrupole time of flight tandem mass spectrometry (HPLC-ESI-Q-TOF–MS/MS) was established. Data were acquired and analyzed by Agilent MassHunter Workstation Qualitative Analysis software version B.07.00 and PCDL manager B.07.00. Results A total of 80 compounds were identified or tentatively characterized in ZYD, 31 more than previously detected. Besides, 36 prototype components and 49 metabolites of ZYD were found and characterized in T2DM rats, and the proposed fragmentation pathways and possible metabolic behaviors of the main types of compounds were described. Conclusions This study developed the understanding of the composition of ZYD as well as the cleavage rules and metabolic pathways of the prototype compounds. Besides, this study provided abundant data for further research and for study of the metabolism of traditional Chinese medicine prescriptions.
危险品化学品经营许可证（带存储）