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目的:建立快速溶剂萃取(ASE)及HPLC测定决明子中大黄酚和橙黄决明素的分析方法。方法:利用正交试验对ASE350快速溶剂萃取系统进行提取方法的研究,采用HPLC法同时测定决明子中大黄酚和橙黄决明素的含量。色谱柱为ACE Excel C_(18)-PFP柱(75 mm×2.1 mm,2.5μm),流动相为乙腈-0.1%磷酸溶液梯度洗脱,流速为0.4 ml·min~(-1),检测波长为284 nm,柱温为40℃。结果:采用甲醇为萃取溶剂、萃取温度为120℃、静态萃取时间为5 min以及循环萃取3次的方法最优,可以很好地提取决明子中大黄酚和橙黄决明素,耗时仅为药典提取方法的1/9。大黄酚和橙黄决明素线性范围为0.73~58.57μg·ml~(-1)(r=0.999 7)和1.09~87.29μg·ml~(-1)(r=0.999 6),平均回收率分别为102.7%(RSD=0.8%)和98.2%(RSD=1.5%)。结论:该方法能简便、快速、准确的测定决明子中的大黄酚和橙黄决明素。
OBJECTIVE: To establish a rapid solvent extraction (ASE) and HPLC method for the determination of chrysophanol and rhubarb in cassia seed. Methods: The extraction method of ASE350 rapid solvent extraction system was studied by orthogonal test. Simultaneously, the content of chrysophanol and orange yellow cassia seed in Cassia seed was determined by HPLC. The column was ACE Excel C_ (18) -PFP column (75 mm × 2.1 mm, 2.5 μm). The mobile phase consisted of acetonitrile-0.1% phosphoric acid solution with a gradient of 0.4 ml · min -1. The detection wavelength 284 nm, column temperature 40 ℃. Results: The best extraction method was using methanol as extracting solvent, extraction temperature of 120 ℃, static extraction time of 5 min and cyclic extraction of 3 times, which could extract chrysophanol and orange yellow cassia seed in cassia seed, consuming only Pharmacopoeia Extraction method of 1/9. The linear range was 0.73 ~ 58.57μg · ml -1 (r = 0.999 7) and 1.09 ~ 87.29μg · ml -1 (r = 0.999 6) for chrysophanol and orange. The average recoveries were 102.7% (RSD = 0.8%) and 98.2% (RSD = 1.5%). Conclusion: The method can be simple, rapid and accurate determination of cassia seed and cassia toxoid Cassia.