HPLC法同时测定珠芽景天药材中8种黄酮苷类成分的含量  

Simultaneous Determination of 8 Flavonoid Glycosides in Sedum bulbiferum by HPLC

作　　者：吴莹莹 雷艳 姚成芬 马雪[1] 黄勇[3] 李勇军[1] 林昌虎[1] WU Yingying;LEI Yan;YAO Chengfen;MA Xue;HUANG Yong;LI Yongjun;LIN Changhu(Engineering Research Center for the Development and Application of Ethnic Medicine and TCM/State Key Laboratory of Functions and Applications of Medicinal Plants,Guizhou Medical University,Guiyang 550004,China;School of Pharmacy,Guizhou Medical University,Guiyang 550004,China;Guizhou Provincial Key Laboratory of Pharmaceutics,Guizhou Medical University,Guiyang 550004,China)

机构地区：[1]贵州医科大学民族药与中药开发应用教育部工程研究中心/省部共建药用植物功效与利用国家重点实验室,贵阳550004 [2]贵州医科大学药学院,贵阳550004 [3]贵州医科大学贵州省药物制剂重点实验室,贵阳550004

出　　处：《中国药房》2020年第12期1436-1439,共4页China Pharmacy

基　　金：国家自然科学基金资助项目(No.U1812403);中央引导地方科技发展专项资金项目(No.黔科中引地〔2018〕4006);贵州省科技计划项目(No.黔科合平台人才〔2016〕5613,No.黔科合平台人才〔2016〕5677)。

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Waters CORTECS C18,流动相为乙腈-0.1%磷酸水溶液(梯度洗脱),流速为0.8 mL/min,检测波长为254 nm,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(24 h)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、1.9157 mg/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。OBJECTIVE:To establish a method for simultaneous 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-glucopyranoside-7-O-α-L-glucopyranoside(KGGR),kaempferol-3-O-β-D-glucopyranosyl-7-O-α-L-rhamnopyrano side(KGR),quercetin-3-O-α-L-rhamno se-7-O-α-L-rhamnoside(QRR),Bulbiferumo side Ⅱ,kaempferol-3-O-(6-coumarinyl)-β-D-glucose-(1→2)-β-D-glucose-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 C18 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 than0.999 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 recoveries 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 9,0.7512,0.502 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 S.bulbiferum.

关 键 词：珠芽景天 高效液相色谱法 黄酮苷类成分 含量测定 

分 类 号：R917[医药卫生—药物分析学]