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HPLC法同时测定珠芽景天药材中8种黄酮苷类成分的含量
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篇名: HPLC法同时测定珠芽景天药材中8种黄酮苷类成分的含量
TITLE: Simultaneous Determination of 8 Flavonoid Glycosides in Sedum bulbiferum by HPLC
摘要: 目的:建立同时测定珠芽景天药材中8种黄酮苷类成分含量的方法。方法:采用高效液相色谱法测定珠芽景天药材中山柰酚-3-O-β-D-吡喃葡萄糖(-1→2)-α-L-吡喃葡萄糖-7-O-α-L-吡喃鼠李糖苷(KGGR)、山柰酚-3-O-β-D-吡喃葡萄糖-7-O-α-L-吡喃鼠李糖苷(KGR)、槲皮素-3-O-α-L-鼠李糖-7-O-α-L-鼠李糖苷(QRR)、BulbiferumosideⅡ、山柰酚-3-O(-6-香豆酰基)-β-D-葡萄糖(-1→2)-β-D-葡萄糖-7-O-α-L-鼠李糖苷(KcGGR)、山柰酚-3-O-(2-β-D-葡萄糖)-α-L-鼠李糖-7-O-α-L-鼠李糖苷(KGRR)、山柰酚-3-O-α-L-鼠李糖苷-7-O-α-L-鼠李糖苷(KRR)、山柰酚-3-O(-6″-乙酰基-β-D-葡萄糖)-7-O-α-L-鼠李糖苷(KaGR)的含量。色谱柱为WatersCORTECSC18,流动相为乙腈-0.1%磷酸水溶液(梯度洗脱),流速为0.8mL/min,检测波长为254nm,柱温为35℃,进样量为5μL。结果:上述8种成分均达到基线分离,检测进样量的线性范围分别为0.013~0.052、0.005~0.018、0.008~0.031、0.010~0.042、0.009~0.038、0.008~0.030、0.009~0.037、0.032~0.130μg(r均不低于0.9990);检测限分别为0.08、0.14、0.11、0.21、0.42、0.35、0.23、0.28μg/mL,定量限分别为0.25、0.47、0.38、0.69、1.40、1.17、0.77、0.93μg/mL;精密度、重复性、稳定性(24h)试验的RSD均小于3%(n为6或7);平均加样回收率为99.67%~104.20%(RSD为0.17%~1.59%,n=6)。13批样品中,上述8种成分的平均含量分别为0.8938、0.3126、0.4908、0.9649、0.7512、0.5022、0.6062、1.9157mg/g(n=3)。结论:该方法简便、准确、重复性好,可用于同时测定珠芽景天药材中8种黄酮苷类成分的含量。
ABSTRACT: OBJECTIVE:To establish a metho d for sim ultaneous determination of 8 flavonoid glycosides in Sedum bulbiferum . METHODS:HPLC method was adopted to determine the contents of kaempferol- 3-O-β-D-glucopyranoside-(1→2)-α-L-glucopy- ranoside-7-O-α-L-glucopyranoside(KGGR),kaempferol-3-O-β-D-glucopyranosyl-7-O-α-L-rhamnopyranoside(KGR),quercetin-3- O-α-L-rhamnose-7-O-α-L-rhamnoside(QRR),BulbiferumosideⅡ,kaempferol-3-O-(6-coumarinyl)-β-D-glucose-(1→2)-β-D-glu- cose-7-O-α-L-rhamnoside(KcGGR),kaempferol-3-O-(2-β-D-glucose)-α-L-rhamnose-7-O-α-L-rhamnoside(KGRR),kaempferol-3- O-α-L-rhamnoside-7-O-α-L-rhamnoside(KRR),kaempferol-3-O-(6″-acetyl-β-D-glucose)-7-O-α-L-rhamnoside(KaGR)in S. bulbi- ferum. The determination was performed on Waters CORTECS C 18 column with mobile consisted of acetonitrile - 0.1% phosphoric acid water solution (gradient elution )at the flow rate of 0.8 mL/min. The detection wavelength was set at 254 nm,and column temperature was 35 ℃. The sample size was 5 μL. RESULTS:The linear range of 8 constituents were 0.013-0.052,0.005-0.018, 0.008-0.031,0.010-0.042,0.009-0.038,0.008-0.030,0.009-0.037,0.032-0.130 μg,respectively(all r were not less than 0.999 0). The limits of detection were 0.08,0.14,0.11,0.21,0.42,0.35,0.23,0.28 μg/mL,respectively. The limits of quantification were 0.25,0.47,0.38,0.69,1.40,1.17,0.77,0.93 μg/mL,respectively. RSDs of precision ,reproducibility and stability tests (24 h) were all lower than 3%(n=6 or n=7). The average re coveries were 99.67%-104.20%(RSDs=0.17%-1.59%,n=6). Average contents of above 8 constituents in 13 batches of samples were 0.893 8,0.312 6,0.490 8,0.964 9,0.751 2,0.502 2,0.606 2, 1.915 7 mg/g(n=3). CONCLUSIONS : The method is simple, acourate and reproducible , and can be used for simultaneous determination of 8 flavonoid glycosides in 才〔2016〕5677) S. bulbiferum .
期刊: 2020年第31卷第12期
编辑: 吴莹莹,雷艳,姚成芬,马雪,黄勇,李勇军,林昌虎
AUTHORS: WU Yingying ,LEI Yan,YAO Chengfen ,MA Xue,HUANG Yong,LI Yongjun ,LIN Changhu
关键字: 珠芽景天;高效液相色谱法;黄酮苷类成分;含量测定
KEYWORDS: edum bulbiferum ;HPLC;Flavonoid glyco-
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