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机构地区:[1]新乡医学院第一附属医院药剂科,河南卫辉453100 [2]遂成药业股份有限公司,河南新郑451150
出 处:《中南药学》2016年第7期752-755,共4页Central South Pharmacy
摘 要:目的建立高效液相色谱波长切换法同时测定仙蟾片中补骨脂素、异补骨脂素、双去甲氧基姜黄素、去甲氧基姜黄素和姜黄素含量。方法采用Zorbax Eclipse C18色谱柱(4.6 mm×250 mm,5μm),以乙腈(A)-0.6%冰醋酸溶液(B)为流动相,进行梯度洗脱(0~13 min,32.0%A;13~24min,32.0%→45.0%A;24~47 min,45.0%→58.0%A;47~55 min,58.0%→32.0%A),流速0.8m L·min-1,波长切换法检测(0~24 min,246 nm,补骨脂素和异补骨脂素;24~55 min,420 nm,双去甲氧基姜黄素、去甲氧基姜黄素和姜黄素),进样量为20μL。结果补骨脂素、异补骨脂素、双去甲氧基姜黄素、去甲氧基姜黄素和姜黄素5种成分的线性范围分别为18.15~363.00μg·m L-1(r=0.9998)、17.13~342.60μg·m L-1(r=0.9992)、4.85~97.00μg·m L-1(r=0.9999)、5.75~115.00μg·m L-1(r=0.9995)、4.92~98.40μg·m L-1(r=0.9996);平均加样回收率及相应的RSD分别为98.6%(1.6%)、99.1%(1.3%)、97.8%(1.6%)、97.0%(1.1%)、98.9%(1.5%)。结论本文建立的高效液相色谱波长切换法同时测定仙蟾片中的5种成分,样品处理方法简便,方法专属性强,测定结果准确,重复性好,稳定性好,可作为仙蟾片全面可靠的质量控制方法。Objective To develop an HPLC with wavelength switching method to determine the content of psoralen, isopsoralen, bisdemethoxycurcumin, demethoxycurcumin and curcumin in Xianchan tablet simultaneously. Methods Zorbax Eclipse C18(4.6 mm×250 mm, 5 μm) chromatographic column was adopted; the mobile phase was acetonitrile(A)-0.6% glacial acetic acid solution(B) with gradient elution(0- 13 min, 32.0%A; 13- 24 min, 32.0% → 45.0%A; 24- 47 min, 45.0% → 58.0%A; 47- 55 min, 58.0% → 32.0%A) at the flow rate of 0.8 m L·min-1, and the detection wavelength was 246 nm(0- 24 min, psoralen and isopsoralen), and 420 nm(24-55 min, bisdemethoxycurcumin, demethoxycurcumin and curcumin). The injection volumn was 20 μL. Results The linearity of psoralen, isopsoralen, bisdemethoxycurcumin, demethoxycurcumin and curcumin was respectively 18.15- 363.00 μg·m L-1(r = 0.9998), 17.13- 342.60 μg·m L-1(r = 0.9992), 4.85- 97.00 μg·m L-1(r = 0.9999), 5.75- 115.00 μg·m L-1(r = 0.9995), and 4.92- 98.40 μg·m L-1(r = 0.9996). The average recoveries and RSDs were 98.6%(1.6%), 99.1%(1.3%), 97.8%(1.6%), 97.0%(1.1%), and 98.9%(1.5%), respectively. Conclusion The HPLC with wavelength switching method has successfully simultaneously determined the 5 components in Xianchan tablets. The sample processing method is simple, specific and the measurement is accurate, repeatabile, stabile. The method is helpful for the quality control of Xianchan tablet.
关 键 词:仙蟾片 补骨脂素 异补骨脂素 双去甲氧基姜黄素 去甲氧基姜黄素 姜黄素 波长切换法
分 类 号:R917[医药卫生—药物分析学]
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