ABSTRACT
OBJECTIVE：To analyze the mass spectrometry fragmentation regularity of bicyclol ，bifendate and schisandrin C ， and to identify the impurities of bicyclol raw material. METHODS ：UHPLC-ESI-Q-TOF-MS method was adopted. Using electrospray ionization source ，in positive ion mode ，the excimer ion and characteristic fragments of bicyclol ，bifendate and schisandrin C were analyzed by means of TOF-MS. According to the mass change of fragments ，the possible fragmentation pathways were speculated ，and the fragmentation regularity were analyzed and summarized. Bicyclol raw material sample was first separated by liquid chromatography to find the impurity peaks in it ，and then the impurity peaks were analyzed by mass spectrometer；the impurity identification was conducted by combining with the fragmentation regularity. RESULTS ：The 3 compounds all produced [M+H] + excimer ion in the positive ion mode. After collision-induced dissociation ，the C-O bond ，the simple rupture of the C-C bond and the ring-opening cleavage of the oxygen ring occurred ；with the loss of neutral fragments ， mainly CH 2O，supplemented by CO 2，CO and CHO ，the dissociation was concentrated in the middle and high quality regions. C-C and C-O bonds of 3 compounds were simply broken only in the branched chain structure and/or oxygen ring structure ，but the structure of the biphenyl parent nucleus remained unchanged. Among them ，the bicyclol contained a benzyl alcohol structure ，so under acidic mobile phase conditions ，it would exist stably in the form of [M+H －H2O]+. Because schisandrin C contained 8-membered ring structure，ring opening first occurred under collision voltage ，and then neutral fragment loss occurred. The secondary mass spectra of impurity in bicyclol raw material were consistent with the mass spectra fragmentation of secondary fragments of bifendate. CONCLUSIONS：The study summarized mass spectrometry fragmentation regularity of 3 schisandrin derivatives. The impurity in bicyclol raw material may be bifendate.
ABSTRACT
Aim To investigate the effects of schisandrin C on arterial inflammation and atherosclerosis of ApoE-/-mice fed with high-fat diet. Methods ApoE-/-mice were divided into high fat diet group (HFD) and high fat diet group + schisandrin group (HFD + Sch C). High fat diet and Sch C were given at the same time. After 12 weeks, mice were executed and arterial tissues were collected. RT-q PCR and Western blot were respectively used to detect the expressions of IL-6, TNF-α, ICAM-1, β-actin and the phosphorylation and expression of IκB-α in arteries. Oil red O staining and biochemical kit were respectively used to detect the lipid changes in aortic root and the blood lipid levels. Results Compared with HFD group, the area of atherosclerotic plaque in HFD + Sch C was reduced (P < 0. 05), but Sch C did not affect blood lipid levels. Compared with HFD group, the mRNA expression of TNF-α, IL-6 and ICAM-1 and the phosphorylation of IκB-α of arterial tissue in HFD + Sch Cgroup decreased (P < 0. 05). Conclusions Sch C could effectively alleviate atherosclerosis induced by high-fat diet in ApoE-/-mice, accompanied by alleviation of arterial inflammation.
ABSTRACT
Objective: To establish an RP-HPLC method for determining the contents of deoxyschizandrin, schisandrin b, schisandrin c, and ursolic acid in Baogan Pill, and to provide the quality guarantee for Baogan Pill. Methods: Agilent Zorbax SB-C18 (150 mm × 46 mm, 5 μm) column was used. Acetonitrile and 0.1% phosphoric acid water solution was used as mobile phase, the volume flow was at 1.0 mL/min; Ultraviolent wavelength was 210 nm; Column temperature was at 30℃, and injection volume was 10 μL. Results: The lowest detection limits in deoxyschizandrin, schisandrin b, schisandrin c, and ursolic acid respectively were 0.016, 0.019, 0.020, and 0.025 mg/L, the linear ranges respectively were 3.906-250.000, 5.323-340.000, 3.225-205.000, and 5.323-340.000 mg/L. The average recoveries of deoxyschizandrin, schisandrin b, schisandrin c, and ursolic acid in Baogan Pill respectively were 100.79%, 101.09%, 101.26%, and 101.16%; The precision RSD values were 1.76%, 1.69%, 1.80%, and 1.86%, respectively; The repeatability RSD values were 1.77%, 1.66% 1.49% and 1.56%, respectively; The stability RSD values were 1.61%, 1.39%, 1.60%, and 1.56%, respectively. The average amounts of deoxyschizandrin, schisandrin b, schisandrin c, and ursolic acid in the selected samples per pill were 0.444, 1.066, 0.3125, 1.068μg, respectively. Conclusion: The method is believable for determining the contents of deoxyschizandrin, schisandrin b, schisandrin c, and ursolic acid with good simplicity, sensibility, repeatability, and recovery rate.