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Objective::To establish an LC-MS/MS method for the determination of alcohol-soluble components and water-soluble components in Arnebiae Radix(L-shikonin, β, β′-dimethylacrylshikonin, β-acetoxy-isovalerylshikonin, lithospermic acid, caffeic acid, rosmarinic acid), for the purpose of quality control of the herb. Method::Chromatographic separation was carried out at 35 ℃ on Agilent ZORBAX SB C18 (4.6 mm×50 mm, 1.8 μm), with 0.1% formic acid acetonitrile (A)-0.1% formic acid solution (B) as the mobile phase for gradient elution (0-3 min, 5%-95%A; 3-7 min, 95%A; 7-7.01 min, 95%-5%A; 7.01-8.5 min, 5%A). The flow rate was 0.2 mL·min-1, and the injection volume was 5 μL. In a negative ionization mode, MRM scanning mode was adopted for quantification. Result::The calibration curves of L-shikonin, β, β′-dimethylacrylshikonin, β-acetoxy-isovalerylshikonin, lithospermic acid, caffeic acid, rosmarinic acid showed a good linearity, and the linear ranges of the above six compounds were 10.12-1 012 μg·L-1(r=0.998 1), 10.88-1 088 μg·L-1(r=0.991 2), 10.08-806.4 μg·L-1(r=0.997 6), 20.32-1 016 μg·L-1(r=0.996 6), 10.37-1 037 μg·L-1(r=0.999 6), 10.26-1 026 μg·L-1(r=0.997 8), respectively. The average recoveries of the analysts were 95.8%(RSD 3.2%), 103.5%(RSD 2.3%), 105.3%(RSD 2.1%), 96.1%(RSD 3.3%), 98.9%(RSD 2.7%), 100.8%(RSD 3.4%). The contents of six components in 13 batches of samples showed significant differences. Conclusion::The established method is feasible and simple, and provides a basis for comprehensive quality evaluation of Arnebiae Radix.
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Objective To study the preparation and properties of alkalized shikonin liposome.Methods Alkalized shikonin was purified from extracts of radix lithospermi with an alkali solution and acid formulation, and then the alkalized shikonin liposome was prepared by ethanol injection.The morphology, particle size and Zeta potential were determined, and the encapsulation efficiency and the in vitro release property were investigated.The content of L-shikonin was also measured by High Performance Liquid Chromatography.Results Alkalized shikonin liposome presented even sphere and normal distribution with particle size of 104.2nm.The Zeta potential was-14.8mV.L-shikonin was linear in the range of 5-50mg/L with the correlation coefficient 0.999 9.The encapsulation efficiency was 43.67％.The final release rate was 65.82％.Conclusion Alkalized shikonin liposome was prepared successfully with good entrapment efficiency and in vitro release property.
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OBJECTIVE:To establish a method for the content determination of L-shikonin in Zilian liniment and evaluate the uncertainty by 2 calculation methods. METHODS:HPLC was performed on the column of Waters C18 with mobile phase of metha-nol-0.025 mol/L phosphate(85:15,V/V)at flow rate of 1.0 ml/min,the detection wavelength was 516 nm,column temperature was room temperature,and the injection volume was 10 μl. Quantitative analysis was conducted for the process and procedures calculat-ed by standard curve method and external standard method,and the uncertainty was evaluated. RESULTS:The linear range of L-shi-konin was 4.024-80.48μg/ml;RSDs of precision,stability and reproducibility test were lower than 2.0%;recovery was 88.5%-93.1%(RSD=2.0%,n=6). Standard curve method was used to determine the content,and the expanded uncertainty was 0.70 μg/ml;ex-ternal standard method was used to determine the content,and the expanded uncertainty was 0.30 μg/ml. CONCLUSIONS:Stan-dard curve method is more economical,more convenient and lower uncertainty in the content determination of L-shikonin in Zilian liniment.
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OBJECTIVE:To establish a method for content determination of the total naphthoquinone in oil/water emul?sion of shikonin by ultraviolet spectrophotometry.METHODS:The content of the total naphthoquinone was counted in L-shikonin,methanol was used as solvent and the wavelength was set at516nm.RESULTS:The concentration of L-shikonin had good linear correlation with absorbance in the range of8.32～41.60?g/ml(r=1.0000,n=5),the average recovery was98.6%(RSD=0.53%).CONCLUSIONS:The present method is simple,precise and replicable resulting in high recovery and accuracy,it can be used to determine the content of total naphthoquinone in oil/water emulsion of shikonin.