HPLC法同时测定青娥丸中7种成分的含量  

Simultaneous Determination of 7 Kinds of Components in Qing'e Pills by HPLC

作　　者：王向锋[1] 黄小为 刘明霞 朱玉青 

机构地区：[1]郯城县第一人民医院,山东临沂276100 [2]山东罗欣药业集团股份有限公司,山东临沂276017

出　　处：《中国药房》2017年第33期4728-4731,共4页China Pharmacy

摘　　要：目的:建立同时测定青娥丸中补骨脂素、异补骨脂素、佛手柑内酯、欧前胡素、三甲基补骨脂素、新补骨脂异黄酮、补骨脂二氢黄酮含量的方法。方法:采用高效液相色谱法。色谱柱为Kinetex-C_(18),流动相为甲醇-0.1%乙酸溶液(梯度洗脱),流速为1.0mL/min,检测波长为248 nm,柱温为30℃,进样量为20μL。结果:补骨脂素、异补骨脂素、佛手柑内酯、欧前胡素、三甲基补骨脂素、新补骨脂异黄酮、补骨脂二氢黄酮检测质量浓度线性范围分别为1.012~101.2μg/mL(r=0.999 9)、1.007~100.7μg/mL(r=0.999 7)、1.010~101.0μg/mL(r=0.999 9)、1.021~102.1μg/mL(r=0.999 9)、1.002~100.2μg/mL(r=0.999 6)、1.008~100.8μg/mL(r=0.999 9)、1.025~102.5μg/mL(r=0.999 8);定量限分别为0.15、0.15、0.30、0.30、0.15、0.30、0.30μg/mL,检测限分别为0.05、0.05、0.10、0.10、0.05、0.10、0.10μg/mL;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为95.3%~99.6%(RSD=1.9%,n=6)、96.1%~99.3%(RSD=1.2%,n=6)、95.2%~98.4%(RSD=1.4%,n=6)、95.4%~99.2%(RSD=1.5%,n=6)、96.1%~99.3%(RSD=1.5%,n=6)、95.6%~98.9%(RSD=1.4%,n=6)、95.2%~99.6%(RSD=1.6%,n=6)。结论:该方法简便、结果准确,适用于青娥丸中7种成分含量的同时测定。OBJECTIVE： To develop a method for simultaneous determination of psoralen, isopsoralen, bergapten, imperato- rin, trimethylpsorale, neobavaisoflavone and bavachin in Qing＇e pills. METHODS： HPLC method was adopted. The separation was performed on Kinetex-C18 column with mobile phase consisted of methanol-0.1% glacial acetic （gradient elution） at the flow rate of 1.0 mL/min. The detection wavelength was set at 248 mn. The column temperature was 30℃. The sample size was 20μL. RESULTS： The linear ranges were 1.012-101.2 μg/mL for psoralen （r=0.999 9）, 1.007-100.7μg/mL for isopsoralen （r=0.999 7）, 1.010-101.0μg/mL for bergapten （r=0.999 9）, 1.021-102.1μg/mL for imperatorin （r=0.999 9）, 1.002-100.2 μg/mL for trimethyl- psorale （r=0.999 6）, 1.008-100.8 gg/mL for neobavaisoflavone （r=0.999 9）, 1.025-102.5 μg/mL for bavachin （r=0.999 8）,respectively. The limits of quantitation were 0.15, 0.15, 0.30, 0.30, 0.15, 0.30, 0.30μg/mL, and the limits of detection were 0.05, 0.05, 0.10, 0.10, 0.05, 0.10, 0.10μg/mL, respectively. RSDs of precision, stability and reproducibility tests were lower than 2.0%. The recoveries were 95.3%-99.6% （RSD=1.9% ,n=6）, 96.1%-99.3% （RSD=1.2% ,n=6）, 95.2%-98.4% （RSD= 1.4%, n=6）, 95.4% -99.2% （RSD=1.5%, n=6）, 96.1% -99.3% （RSD=1.5%, n=6）, 95.6% -98.9% （RSD=1.4%, n=6）, 95.2%-99.6% （RSD= 1.6%,n= 6）, respectively. CONCLUSIONS： The method is simple and accurate, can be used for simultaneous determination of 7 kinds of components in Qing＇ e pills.

关 键 词：高效液相色谱法 青娥丸 含量 补骨脂素 异补骨脂素 佛手柑内酯 欧前胡素 三甲基补骨脂素 新补骨脂异黄酮 补骨 脂二氢黄酮 

分 类 号：R927.2[医药卫生—药学]