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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 Δ
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吴莹莹 1,2* ,雷 艳 ,姚成芬 ,马 雪 ,黄 勇 ,李勇军 ,林昌虎 (1.贵州医科大学民族药与中药开发应用
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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)
中图分类号 R917 文献标志码 A 文章编号 1001-0408(2020)12-1436-04
DOI 10.6039/j.issn.1001-0408.2020.12.06
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 5 μL。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、0.032~0.130 μg(r均不低于0.999 0);检测限分别为0.08、0.14、0.11、0.21、
0.42、0.35、0.23、0.28 μg/mL,定量限分别为0.25、0.47、0.38、0.69、1.40、1.17、0.77、0.93 μg/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0.893 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)。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。
关键词 珠芽景天;高效液相色谱法;黄酮苷类成分;含量测定
Simultaneous Determination of 8 Flavonoid Glycosides in Sedum bulbiferum by HPLC
WU Yingying 1,2 ,LEI Yan 1,2 ,YAO Chengfen 1,2 ,MA Xue ,HUANG Yong ,LI Yongjun ,LIN Changhu (1.
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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;2. School of Pharmacy,Guizhou Medical University,Guiyang 550004,China;3. Guizhou Provincial
Key Laboratory of Pharmaceutics,Guizhou Medical University,Guiyang 550004,China)
ABSTRACT 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-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 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 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 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 9,0.751 2,0.502 2,0.606 2,
1.915 7 mg/g (n=3). CONCLUSIONS: The method is
Δ 基金项目:国家自然科学基金资助项目(No.U1812403);中央
simple, acourate and reproducible, and can be used for
引导地方科技发展专项资金项目(No.黔科中引地〔2018〕4006);贵州
simultaneous determination of 8 flavonoid glycosides in
省科技计划项目(No.黔科合平台人才〔2016〕5613,No.黔科合平台人
S. bulbiferum.
才〔2016〕5677)
*硕士研究生。研究方向:药效物质基础。E-mail:2458460478@qq. KEYWORDS Sedum bulbiferum; HPLC; Flavonoid glyco-
com sides;Content determination
# 通信作者:教授,博士生导师。研究方向:中药资源可持续利用
及其物质基础。E-mail:linchh026@126.com
·1436 · China Pharmacy 2020 Vol. 31 No. 12 中国药房 2020年第31卷第12期