摘要
目的建立同时测定舒肝和胃丸中芍药苷、橙皮苷、柚皮苷、欧前胡素与佛手柑内酯5种成分含量的固相萃取-超高效液相色谱(SPE-UPLC)法。方法采用索氏提取法提取样品,用固相萃取(SPE)柱分离后进样测定,色谱柱为Poroshell 120 SB-C18柱(100 mm×4.6 mm,2.7μm),流动相为甲醇(A)-0.1%磷酸溶液(B),梯度洗脱(0~10 min时10%A~40%A,10~15 min时40%A~45%A,15~20 min时45%A~100%A),流速为0.5 m L/min,检测波长分别为230 nm(芍药苷)、283 nm(橙皮苷、柚皮苷)、248 nm(欧前胡素、佛手柑内酯),柱温为30℃,进样量为5μL。结果芍药苷、橙皮苷、柚皮苷、欧前胡素、佛手柑内酯检测的质量浓度线性范围分别为2.180~43.600μg/m L(r=0.9999),2.526~50.520μg/m L(r=0.9999),0.959~19.180μg/m L(r=0.9999),3.493~69.860μg/m L(r=0.9999),4.707~94.140μg/m L(r=0.9998);平均加样回收率分别为92.83%,95.72%,93.36%,94.70%,95.23%,RSD分别为2.27%,2.17%,1.79%,2.38%,2.00%(n=6)。结论该方法重复性好、结果准确,可为舒肝和胃丸的质量控制提供依据。
Objective To establish a solid-phase extraction and ultra-performance liquid chromatography(SPE-UPLC)method for the simultaneous determination of paeoniflorin,hesperidin,naringin,imperatorin and bergapten in Shugan Hewei Pills.Methods The samples were extracted by the Soxhlet extraction method and determined after being separated by the SPE column.The chromatographic column was Poroshell 120 SB-C18 column(100 mm×4.6 mm,2.7μm),the mobile phase was methanol(A)-0.1%phosphoric acid solution(B),with gradient elution(0-10 min,10%A-40%A;10-15 min,40%A-45%A;15-20 min,45%A-100%A),the flow rate was 0.5 m L/min,the detection wavelengths were 230 nm for paeoniflorin,283 nm for hesperidin and naringin,248 nm for imperatorin and bergapten,respectively,the column temperature was 30℃,and the injection volume was 5μL.Results The linear ranges were 2.180-43.600μg/m L for paeoniflorin(r=0.9999),2.526-50.520μg/m L for hesperidin(r=0.9999),0.959-19.180μg/m L for naringin(r=0.9999),3.493-69.860μg/m L for imperatorin(r=0.9999),4.707-94.140μg/m L for bergapten(r=0.9998),respectively.The average recoveries were 92.83%,95.72%,93.36%,94.70%,95.23%,the RSDs were 2.27%,2.17%,1.79%,2.38%,2.00%(n=6).Conclusion The method is reproducible and accurate,which can provide a theoretical basis for the quality control of Shugan Hewei Pills.
作者
梁冬牛
陈峰
郑磊
LIANG Dongniu;CHEN Feng;ZHENG Lei(Shandong Provincial Third Hospital,Ji'nan,Shangdong,China 250031;China Resources Shandong Pharmaceutical Co.,Ltd.,Ji'nan,Shandong,China 250031)
出处
《中国药业》
CAS
2021年第3期53-56,共4页
China Pharmaceuticals
基金
中国药学会精准用药科技传播促进行动2019年重点项目[CMEI2019KPYJ(JZYY)00204]。
关键词
超高效液相色谱法
固相萃取
舒肝和胃丸
芍药苷
橙皮苷
柚皮苷
欧前胡素
佛手柑内酯
含量
ultra-performance liquid chromatography
solid-phase extraction
Shugan Hewei Pills
paeoniflorin
hesperidin
naringin
imperatorin
bergapten
content
