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建立甘草酸发酵液中甘草酸及其发酵产物乌拉尔甘草皂苷乙、3-O-β-D-葡萄糖醛酸-24-OH-18β-甘草次酸、单葡萄糖醛酸甘草次酸、18α-单葡萄糖醛酸甘草次酸和甘草次酸的RP-HPLC含量测定方法,为单葡萄糖醛酸甘草次酸的生产工艺研究及产品质量控制提供方法学基础。采用Kromasil C18(250 mm×4.6 mm,5μm)色谱柱,以甲醇(B)-1%乙酸溶液(A)为流动相进行梯度洗脱:0 min,63%B;40 min,66%B;50 min,75%B;70 min,90%B;80 min,90%B。体积流速:1.0 mL/min;进样量:10μL;柱温:25℃;检测波长:254 nm。甘草酸、乌拉尔甘草皂苷乙、3-O-β-D-葡萄糖醛酸-24-OH-18β-甘草次酸、单葡萄糖醛酸甘草次酸、18α-单葡萄糖醛酸甘草次酸和甘草次酸的线性范围分别为11.25~180.0μg/mL(r=0.9986);3.031~96.99μg/mL(r=0.9978);2.595~83.00μg/mL(r=0.9999);62.50~2000μg/mL(r=0.9999);11.25~180.0μg/mL(r=0.9980);1.560~50.00μg/mL(r=0.9992);平均回收率(n=9)分别为98.3%,101.2%,98.4%,101.9%,101.7%,97.42%,RSD分别为2.5%,1.4%,0.96%,2.8%,0.73%,0.32%。
Glycyrrhizic acid and its fermentation products were isolated from glycyrrhizic acid fermented broth and identified as Ural glycyrrhizin B, 3-O-β-D-glucuronic acid-24-OH-18β-glycyrrhetinic acid, glycyrrhetinic acid mono-glucuronide, 18α- RP-HPLC method for the determination of glucuronide glycyrrhetinic acid and glycyrrhetinic acid provides the methodological basis for the research of the production technology and product quality control of glycyrrhetinic acid monoglycuronic acid. The gradient elution was carried out on a Kromasil C18 (250 mm × 4.6 mm, 5 μm) column with a mobile phase of methanol (B) -1% acetic acid (A): 0 min, 63% B; 40 min, 66% B; 50 min, 75% B; 70 min, 90% B; 80 min, 90% B. Volume flow rate: 1.0 mL / min; injection volume: 10 μL; column temperature: 25 ° C; detection wavelength: 254 nm. Glycyrrhizic acid, Ural glycyrrhizin B, 3-O-β-D-glucuronic acid-24-OH-18β-glycyrrhetinic acid, monoglycuronic glycyrrhetinic acid, 18α-monoglucuronic glycyrrhetinic acid, The linear ranges of acid were 11.25-180.0μg / mL (r = 0.9986), 3.031-96.99μg / mL (r = 0.9978), 2.595-83.00μg / mL (r = 0.9999), 62.50-2000μg / mL 0.9999); 11.25-180.0μg / mL (r = 0.9980); 1.560-50.00μg / mL (r = 0.9992); the average recoveries were 98.3%, 101.2%, 98.4%, 101.9% and 101.7 %, 97.42%, RSD respectively 2.5%, 1.4%, 0.96%, 2.8%, 0.73%, 0.32%.