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目的建立HPLC波长切换联合梯度洗脱法同时测定参苏宣肺丸中咖啡酸、迷迭香酸、3’-羟基葛根素、葛根素、3’-甲氧基葛根素、大豆苷的含量。方法采用ZOBAX SB-C18色谱柱(4.6 mm×250 mm,5μm);流动相A为甲醇-乙腈(1∶1),流动相B为0.1%冰醋酸溶液,进行梯度洗脱;流速为1.0 m L·min?1;咖啡酸和迷迭香酸的检测波长为320 nm,3’-羟基葛根素、葛根素、3’-甲氧基葛根素和大豆苷的检测波长为250 nm;进样量为20μL。结果咖啡酸、迷迭香酸、3’-羟基葛根素、葛根素、3’-甲氧基葛根素、大豆苷的浓度与峰面积分别在2.32~46.40μg·m L?1(r=0.999 8)、3.06~61.20μg·m L?1(r=0.999 5)、4.45~89.00μg·m L?1(r=0.999 9)、14.48~289.60μg·m L?1(r=0.999 9)、4.86~97.20μg·m L?1(r=0.999 7)、3.69~73.80μg·m L?1(r=0.999 6)内具有较好的线性关系,平均加样回收率和相应的RSD分别为99.0%(1.6%),97.5%(0.6%),99.3%(0.9%),98.6%(1.3%),97.6%(1.3%),97.0%(0.9%)。结论方法操作准确、简便,可用于参苏宣肺丸的质量控制。
OBJECTIVE To establish simultaneous determination of caffeic acid, rosmarinic acid, 3’-hydroxy puerarin, puerarin, 3’-methoxy puerarin and daidzin in Shensu Xuanfei Pills by HPLC wavelength shift combined with gradient elution. Methods The mobile phase A was methanol-acetonitrile (1: 1) and the mobile phase B was 0.1% acetic acid in acetic acid. The gradient elution was performed on a ZOBAX SB-C18 column (4.6 mm × 250 mm, 5 μm) L · min -1; the detection wavelength of caffeic acid and rosmarinic acid was 320 nm; the detection wavelength of 3’-hydroxy puerarin, puerarin, 3’-methoxy puerarin and daidzin was 250 nm; The amount is 20 μL. Results The concentrations and peak areas of caffeic acid, rosmarinic acid, 3’-hydroxy puerarin, puerarin, 3’-methoxy puerarin and daidzin were between 2.32 and 46.40 μg · m L -1 (R = 0.999 5), 4.45-89.00 μg · m L -1 (r = 0.999 9), 14.48-289.60 μg · m L -1 (r = 0.999 9) , 4.86 ~ 97.20μg · m L · 1 (r = 0.999 7) and 3.69 ~ 73.80μg · m L · 1 (r = 0.999 6) respectively. The average recovery and the corresponding RSD were respectively Were 99.0% (1.6%), 97.5% (0.6%), 99.3% (0.9%), 98.6% (1.3%), 97.6% (1.3%), 97.0% (0.9%). Conclusion The method is accurate and easy to operate and can be used for the quality control of Shen-Su Xuan-Fei Wan.