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HPLC波长切换法同时测定经典名方槐花散中5种成分的含量 Δ
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向泽栋 ,薛 晴 ,于海涛 ,孙志强 ,李 震 ,刘菊妍 ,张加余 ,高 鹏 ,代 龙 (1.山东中医药大学药学院,
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济南 250355;2.山东禹泽药康产业技术研究院有限公司,山东 德州 251200;3.广州医药集团有限公司技质
部,广州 510130;4.滨州医学院药学院,山东 烟台 264003)
中图分类号 R917 文献标志码 A 文章编号 1001-0408(2021)16-1964-05
DOI 10.6039/j.issn.1001-0408.2021.16.08
摘 要 目的:建立同时测定经典名方槐花散中芦丁、柚皮苷、新橙皮苷、槲皮素和胡薄荷酮等5种成分含量的方法。方法:采用
高效液相色谱波长切换法。色谱柱为Cosmosil C18,流动相为乙腈-0.05%磷酸溶液(梯度洗脱),检测波长依次为257 nm(芦丁)、
283 nm(柚皮苷、新橙皮苷)、254 nm(槲皮素)、252 nm(胡薄荷酮),流速为1.0 mL/min,柱温为30 ℃,进样量为10 μL。结果:芦丁、
柚皮苷、新橙皮苷、槲皮素、胡薄荷酮检测质量浓度的线性范围分别为 21.7~2 170、46~4 600、22.3~2 230、0.96~96、2.7~270
μg/mL(r均大于0.999);精密度、稳定性(24 h)、重复性试验的RSD均小于2%(n=6);平均加样回收率分别为100.70%、99.31%、
101.10%、100.03%、99.63%(RSD 均小于 2%,n=9)。3 批槐花散样品中,上述 5 种成分的含量分别为 20.055~22.615、25.557~
27.806、11.428~13.250、0.350~0.478、2.372~4.011 mg/g。结论:所建含量测定方法操作简便、结果准确、重复性好,可用于槐花散
中5种成分的同时测定。
关键词 槐花散;高效液相色谱波长切换法;芦丁;柚皮苷;新橙皮苷;槲皮素;胡薄荷酮;含量测定
Simultaneous Determination of 5 Components in the Classical Formula Huaihua San by HPLC Wavelength
Switching Method
XIANG Zedong ,XUE Qing ,YU Haitao ,SUN Zhiqiang ,LI Zhen ,LIU Juyan ,ZHANG Jiayu ,GAO Peng ,
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DAI Long(1. College of Pharmacy,Shandong University of TCM,Jinan 250355,China;2. Shandong Yuze
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Institute of Pharmaceutical and Health Industry Technology,Shandong Dezhou 251200,China;3. Technology
and Quality Department,Guangzhou Pharmaceutical Group Co.,Ltd,Guangzhou 510130,China;4. School of
Pharmacy,Binzhou Medical University,Shandong Yantai 264003,China)
ABSTRACT OBJECTIVE:To develop a method for simultaneous determination of 5 components in classical formula Huaihua
san,including rutin,naringin,neohesperidin,quercetin and pulegone. METHODS:HPLC wavelength switching method was
adopted. The determination was performed on Cosmosil C18 column with mobile phase consisted of acetonitrile-0.05% phosphoric
acid solution(gradient elution)at the flow rate of 1.0 mL/min. The detection wavelengths were set at 257 nm for rutin,283 nm for
naringin and neohesperidin,254 nm for quercetin,252 nm for pulegone,respectively. The column temperature was set at 30 ℃,
and sample size was 10 μL. RESULTS:The linear range was 21.7-2 170 μg/mL for rutin,46-4 600 μg/mL for naringin,22.3-
2 230 μg/mL for neohesperidin,0.96-96 μg/mL for quercetin,2.7-270 μg/mL for pulegone(all r>0.999),respectively. RSDs of
precision,stability(24 h)and reproducibility tests were all lower than 2%(n=6). Average recoveries were 100.70%,99.31%,
101.10% ,100.03% and 99.63%(all RSD<2% ,n=9). Among 3 batches of Huaihua san samples,the contents of above 5
components were 20.055-22.615,25.557-27.806,11.428-13.250,0.350-0.478,2.372-4.011 mg/g,respectively. CONCLUSIONS:
Established method is simple,accurate and reproducible,and could be used for the simultaneous determination of 5 components in
Huaihua san.
KEYWORDS Huaihua san;HPLC wavelength switching method;Rutin;Naringin;Neohesperidin;Quercetin;Pulegone;
Content determination
Δ 基金项目:国家“重大新药创制”科技重大专项课题(No.2018- 槐花散始载于宋代许叔微所著的《普济本事方》,是
[1]
ZX09721004) 治疗肠风脏毒的经典方 。该方为《古代经典名方目录
*硕士研究生。研究方向:中药新药质量控制与评价。电话:
(第一批)》第 34 方,具有清肠凉血止血、疏风行气的功
0531-89628200。E-mail:1014137130@qq.com
效,主治风热湿毒、壅遏肠道、损伤血络证,常用于溃疡
# 通信作者:教授,硕士生导师,硕士。研究方向:新药和新制剂
[2]
研发。电话:0531-89628200。E-mail:2665275709@qq.com 性结肠炎的临床治疗 。槐花散由槐花(炒)、侧柏叶(烂
·1964 · China Pharmacy 2021 Vol. 32 No. 16 中国药房 2021年第32卷第16期