ABSTRACT
OBJECTIVE： To establish a method for simultaneous determination of 4 triglyceride anti-tumor components in Coix lacryma seed oil. METHODS： HPLC-ELSD was adopted. The determination was performed on Inertsil ODS-3 C18 column with mobile phase consisted of acetonitrile-isopropanol （57 ∶ 43， V/V） at the flow rate of 1.0 mL/min. The column temperature was 30 ℃， and the sample size was 10 μL. Evaporative light scattering detector was used， the drift tube temperature was 70 ℃， and the gas flow rate was 2 L/min. Using glycerol trioleateas internal standard， relative correction factors （RCF） of linolein trilinolein， 1，2-linoleic acid-3-palmitic acid glyceride and 1-palmitic acid-2-oleic acid-3-linoleic acid glyceride were calculated respectively. The contents of above 3 components in C. lacryma seed oil were calculated by RCF. The contents of 4 components in C. lacryma seed oil were determined by external standard. The results of content determination by quatitative analysis of multi-components by single marker （QAMS） were compared with external standard method. RESULTS： The linear ranges were 0.15-4.50 μg for linolein trilinolein， 0.15-4.50 μg for 1，2-linoleic acid-3-palmitate， 0.35-10.50 μg for 1-palmitic acid-2-oleic acid-3-linoleic acid glyceride， 0.35-10.50 μg for glycerol trioleate （r≥0.999 5）. The limits of quantification were 0.13， 0.06， 0.07， 0.12 μg. The limits of detection were 0.04， 0.02， 0.02， 0.03 μg， respectively. RSDs of precision， stability， and repeatability tests were less than 2.0％（n＝6）. The average recoveries were 95.43％-102.67％（RSD＜2.0％， n＝6）. Average RCFs of linolein trilinolein， 1，2- linoleic acid-3-palmitic acid glyceride and 1-palmitic acid-2- oleic acid-3-linoleic acid glyceride were 0.31， 0.88， and 1.21， respectively. RCFs reproducibility was perfect under different experiment conditions. There was no significant difference in results of content determination between QAMS and external standard method （P＞0.05）. CONCLUSIONS： The method is simple， rapid， accurate and reliable. It is used for simultaneous determination of linolein trilinolein， 1， 2-linoleic acid-3-palmitate， 1-palmitic acid-2-oleic acid-3-linoleic acid glyceride and glycerol trioleateas in C. lacryma seed oil.
ABSTRACT
Objective: To establish the method of simultaneous determination of contents of honokiol, magnolol and piperitylmagnolol in Cortex Magnoliae Officinalis from different regions, which could provide evidence for the quality control evaluation of Cortex Magnoliae Officinalis. Methods: The quantitative analysis was performed with a column of Waters Acquity UPLC BEH-Cl8 (2.1 mm×50 mm, 1.7 μm) by UPLC-PDA, and eluted with a mobile phase of 0.2％formic acid solution (A)-methanol (B) in a gradient mode (0-2 min, 65％-65％ B; 2-3 min, 65％-75％ B; 3-5 min, 75％-84％ B; 5-9 min, 84％-90％ B) under a flow rate of 0.5 mL·min-1. The column temperature was set at 35℃, and the detection wavelength was 294 nm and the injection volume was 1 μL. Results: The 3 lignan components were completely separated and could be separated well from other components. The honokiol, magnolol and piperitylmagnolol showed a good linear relationship with chromatographic peak area in range of 20.3-406.0, 15.2-304.0, 5.6-112.0 ng, respectively.The average recoveries were 91.75％, 93.86％, 95.15％ with the RSDs were 1.75％, 1.88％, 1.91％ (n = 9), respectively.Conclusion: Contents of the 3 constituents from different place were significantly different and this method is simple and effective, which can be used to quality control of Cortex Magnoliae Officinalis.