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Objective To determine 10 components in Shiliang tea by high performance liquid chromatography-quantitative analysis of multi-components with a single-marker(HPLC-QAMS),and to evaluate its comprehensive quality by multivariate statistical analysis and entropy-technique for order preference by similarity to ideal solution(E-TOPSIS).Methods The determination was performed on COSMOSIL ?5 C18-MS-Ⅱ column(250 mm×4.6 mm,5 μm)with mobile phase consisted of acetonitrile-0.1％ phosphoric acid solution and gradient elution at the flow rate of 1.0 mL·min-1,and the detection wavelength was set at 360 nm and 222 nm.The contents of scopolin,scopoletin,isofraxidin,rutoside,kaempferol-3-O-rutinoside,astragalin,scoparone,quercetin,kaempferol and mcalycanthine in 18 batches of Shiliang tea were calculated according to QAMS using rutoside as internal reference.The content data of 18 batches of Shiliang tea were analyzed chemometrically using statistical software;the quality of Shiliang tea was evaluated comprehensively using E-TOPSIS method.Results Good separation was obtained for all 10 components and showed good linearity with peak area in their respective scopes(r>0.999 0).The average recovery rates were 96.98％ -100.12％ (RSD<2.0％ ,n=9).The average relative correction factors for rutoside and the other 9 components were 2.115 7,2.592 4,0.553 1,0.897 6,0.780 7,1.159 3,0.693 6,1.458 3 and 0.6017(RSD<2.0％ ,n=6),and there was no significant difference between the contents obtained by QAMS and external standard method for each component.The results of multivariate statistical analysis showed that the cumulative variance contribution rate of the 2 principal components was 83.886％ ,and the variable importance in the projection value greater than 1 were kaempferol-3-O-rutinoside,rutoside and astragalin.The results of E-TOPSIS showed that the euclidean closeness of the optimal solution was between 0.180 4 and 0.739 4.Conclusion The method established is simple,accurate,economical and practical,which can fully reflect the quality difference of Shiliang tea and better control the quality of this variety.
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Objective To synthesize and analyze sodium 18F-fluoroacetate (FAC) and its precursor ethyl O-mesylglycolate (EOMG). Methods EOMG was synthesized using modified method. Its chemical purity was checked by HPLC and its structure was elucidated on the basis of spectral analyses. Final product of 18F-FAC was synthesized based on general nucleophilic reactions module Explora GN using EOMG as a precursor. Liquid chromatography Explora LC was applied to get rid of its chemical impurities.Then HPLC and radio-thin layer chromatography were used to assay its radiochemical purity, chemical purity and specific activity. Results EOMG was synthesized and identified. Its yield was 70% and its chemical purity was 97.0% (calculated by chromatographic peak area). The radiochemical purity of 18F-FAC was more than 98%, and its specific activity was 236. 5 MBq/μmol. Conclusion This synthetic method for 18F-FAC and its precursor can be defined as effective and highly quality-controlled.
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Objective To evaluate 18F-N- succinimidyl -4-fluorobenzoate (SFB)-Annexin B1 in detectingin vitro andin vivo apoptosis. Methods Anti-Fas antibody was used to induce apoptosis in Jurkat cells. Apoptosis in Jurkat cells was confirmed by flow cytometer (FCM). Unilateral renal ischemia/reperfusion injury was induced by transient (45 min) ligation of the renal artery in the rabbit. The rabbit was then administrated with 18F-SFB-Annexin B1 intravenously 24 h later and then imaged by PET/CT at 10,30,60,90,120 and 240 min postinjection. Apoptosis in kidney was confirmed by terminal deoxynucleotidyl transferase mediated dUTP biotin nick end labeling (TUNEL) assay and HE staining. Results The apoptosis rate induced by anti-Fas antibody was 25.98%(120 min) while that in the control group was only 1.81%. The uptake of 18F-SFB-Annexin B1in apoptosis group was greater than that in the control group. PET/CT images at 240 min showed higher uptake in the ligated kidney than the non-ligated kidney. TUNEL assay and HE staining confirmed great amount apoptotic cells in the ligated kidney. Conclusion 18 F-SFB-Annexin B1may be potentially useful in detecting apoptosis both in vitro and in vivo.