2023 年第 5 期 第 18 卷

复元胶囊质量标准与药理作用及临床意义

Quality standard, pharmacological action and clinical significance of Fuyuan capsule

作者：周凤盈1王殿奎1张玉2孙琛1耿春辉1

英文作者：Zhou Fengying1， Wang Diankui1， Zhang Yu2， Sun Chen1， Geng Chunhui1

单位：1河北省衡水市综合检验检测中心，衡水053000；2河北省衡水市药品不良反应监测中心，衡水053000

英文单位：1Hengshui City Comprehensive Inspection and Testing Center Hebei Province Hengshui 053000， China; 2Hengshui City Adverse Drug Reaction Monitoring Center Hengshui 053000 China

关键词：复元胶囊；薄层色谱法；高效液相色谱法

英文关键词：Fuyuancapsule;Thin-layerchromatography;High-performanceliquidchromatography

• 摘要：

• 目的 探讨复元胶囊部分成分的定性鉴别方法及4种主要活性成分含量测定方法的准确性。方法 采用薄层色谱法对复元胶囊中的人参、黄芪、熟地黄、淫羊藿进行定性鉴别。采用高效液相色谱法在同一色谱条件下同时测定复元胶囊中主要活性成分2,3,5,4′-四羟基二苯乙烯-2-O-β-D-葡萄糖苷、3,6′-二芥子酰基蔗糖、淫羊藿苷、丹酚酸B的含量；色谱柱为Waters Symmetry C18柱(250 mm×4.6 mm，5 μm)，柱温为 30 ℃；流动相为乙腈-0.1%磷酸，梯度洗脱，检测波长为320 nm，进样量为10 μl，流速为1.0 ml/min。结果  薄层色谱法鉴别人参、黄芪、熟地黄、淫羊藿的特征斑点清晰，分离度好且阴性对照无干扰。含量测定中4个主要活性组分的线性范围分别为：2,3,5,4′-四羟基二苯乙烯-2-O-β-D-葡萄糖苷4.84～48.40 μg/ml(r=0.999 8)、3,6′-二芥子酰基蔗糖1.11～11.12 μg/ml(r=0.999 1)、丹酚酸B 1.84～18.36 μg/ml(r=0.999 2)、淫羊藿苷1.45～14.50 μg/ml(r=0.999 9)，平均加样回收率分别为94.34%、94.70%、95.38%、92.76%，相对标准偏差分别为1.09%、1.03%、0.92%、0.88%(n=6)。检测限分别为0.153 0、0.032 5、0.055 2、0.043 3 μg/ml；定量限分别为0.509，0.108，0.184，0.144 μg/ml；精密度试验、重复性试验、稳定性试验均良好，相对标准偏差均小于2.0%（n=6）。结论   采用薄层色谱法可以对复元胶囊组方中人参、黄芪、熟地黄、淫羊藿进行定性鉴别。在检测波长为320 nm的条件下，以乙腈-0.1%磷酸溶液作为流动相进行梯度洗脱，复元胶囊4种主要活性成分检测的方法准确可靠、灵敏度高、稳定性和重复性良好，操作简单。

• Objective  To explore the qualitative identification Methods  of some components of Fuyuan capsules and the accuracy of the content determination Methods  of four main active components. Methods Thin-layer chromatography (TLC) was used to qualitatively identify ginseng, Astragalus, Rehmannia glutinosa, and Epimedium in Fuyuan capsules. The high-performance liquid chromatography was used to simultaneously determine contents of the main active ingredients of 2,3,5,4′-tetrahydroxystilbene-2-O-β-D-glucoside, 3,6′-dierucanoyl sucrose, icariin and salvianolic acid B in Fuyuan capsules under the same chromatographic conditions. The chromatographic column was Waters Symmetry C18 column (250 mm×4.6 mm, 5 μm), the column temperature was 30 ℃, the mobile phase was acetonitrile-0.1% phosphoric acid, gradient elution, the detection wavelength was 320 nm, the injection volume was 10 μl, and the flow rate was 1.0 ml/min. ResultsThe characteristic spots of ginseng, Astragalus, Rehmannia glutinosa and Epimedium were clear by TLC, with good separation and no interference in negative control. The linear ranges of the four main active components in the content determination were respectively 2,3,5,4′-tetrahydroxystilbene-2-O-β-D-glucoside 4.84-48.40 μg/ml(r=0.999 8), 3,6′-dierucanoyl sucrose 1.11-11.12 μg/ml(r=0.999 1), salvianolic acid B 1.84-18.36 μg/ml(r=0.999 2), and icariin 1.45-14.50 μg/ml (r=0.999 9). The average recovery rates of sample addition were respectively 94.34%, 94.70%, 95.38%, and 92.76%, and the relative standard deviations were respectively 1.09%, 1.03%, 0.92%, and 0.88% (n=6). The limits of detection were 0.153 0, 0.032 5, 0.055 2, and 0.043 3 μg/ml, the limits of quantification were 0.509, 0.108, 0.184, and 0.144 μg/ml, the precision test, repeatability test, and stability test were all good, and the relative standard deviations were all less than 2.0%（n=6）. Conclusions The TLC can be used to qualitatively identify ginseng, Astragalus, Rehmannia glutinosa, and Epimedium in Fuyuan capsules. At the detection wavelength of 320 nm, acetonitrile-0.1% phosphoric acid solution is used as the mobile phase for gradient elution. The method for the detection of the four main active components of Fuyuan capsules is accurate, reliable, sensitive, stable and reproducible, and easy to operate.