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高效液相色谱一测多评法同时测定小儿咳嗽宁糖浆中 8 种成分含量
李美玲1,魏谭军1,杨芝芳1,陈飞1,黄爱苹1,唐启荣1,肖成1,罗进芳2(
0
(1. 达州市中西医结合医院,四川达州 635000; 2. 贵州中医药大学,贵阳 550025)
摘要:
目的:建立小儿咳嗽宁糖浆中桑皮苷 A、桑辛素 M、二氢桑色素、黄芩苷、汉黄芩苷、白花前胡甲素、白花前胡乙素及白花前胡 E 素 8 个成分的高效液相色谱一测多评(HPLC-QAMS)定量控制方法。 方法:采用 Ultrasil C18 色谱柱,流动相为乙腈(A)-1 mL/ L 冰醋 酸,流速为 1. 0 mL/ min 进行线性梯度洗脱,检测波长分别为 280 nm(桑皮苷 A、桑辛素 M、二氢桑色素、黄芩苷和汉黄芩苷)和 321 nm(白花前胡甲素、白花前胡乙素和白花前胡 E 素),柱温为 25 ℃ 。 以黄芩苷为参照物,建立其他 7 个成分的相对校正因 子,计算桑皮苷 A、桑辛素 M、二氢桑色素、汉黄芩苷、白花前胡甲素、白花前胡乙素和白花前胡 E 素含量。 结果:桑皮苷 A、桑辛 素 M、二氢桑色素、黄芩苷、汉黄芩苷、白花前胡甲素、白花前胡乙素及白花前胡 E 素分别在 0. 79 ~ 19. 75、0. 56 ~ 14. 00、0. 38 ~ 9. 50、26. 55~663. 75、4. 66~116. 50、5. 87~146. 75、1. 71~ 42. 75 和 2. 39 ~ 59. 75 μg / mL 范围内与峰面积线性关系良好,各组分 低、中、高浓度的平均加样回收率为 96. 83% ~100. 14%,相对标准偏差(RSD)均≤1. 42%(n = 9),HPLC-QAMS 法计算结果与外 标法(ESM)实测结果无明显差异。 结论:HPLC-QAMS 法为小儿咳嗽宁糖浆提供了一个快捷可行的多指标同步质量评价模式。
关键词:  高效液相色谱一测多评法  小儿咳嗽宁糖浆  相对校正因子  含量测定
DOI:10.13407/j.cnki.jpp.1672-108X.2023.12.008
基金项目:
Simultaneous Determination of Eight Kinds of Components in Xiao’er Kesouning Syrup by High-Performance Liquid Chromatography Combined with Quantitative Analysis of Multi-Components by Single-Marker
Li Meiling1 , Wei Tanjun1 , Yang Zhifang1 , Chen Fei1 , Huang Aiping1 , Tang Qirong1 , Xiao Cheng1
(1. Dazhou Integrated TCM & Western Medicine Hospital, Sichuan Dazhou 635000, China; 2. Guizhou University of Traditional Chinese Medicine, Guiyang 550025, China)
Abstract:
Objective: To establish the high-performance liquid chromatography combined with quantitative analysis of multi-components by single-marker (HPLC-QAMS) technology for the quantitative control of 8 kinds of components in Xiao’er Kesouning syrup, including mulberroside A, morusin M, dihydromorin, baicalin, wogonoside, praeruptorin A, praeruptorin B and praeruptorin E. Methods: Ultrasil C18 column was used with the mobile phase of acetonitrile (A) and 1 mL/ L glacial acetic acid. The flow rate was 1. 0 mL/ min with a linear gradient elution, detection wavelengths were set at 280 nm ( mulberroside A, morusin M, dihydromorin, baicalin and wogonoside), and 321 nm (praeruptorin A, praeruptorin B and praeruptorin E), the column temperature was maintained at 25 ℃. Baicalin was used as the reference substance, relative correction factors for the other 7 kinds of components were established to calculate the content of mulberroside A, morusin M, dihydromorin, wogonoside, praeruptorin A, praeruptorin B and praeruptorin E. Results: A good linear relationship with peak area was observed within the range from 0. 79 to 19. 75 μg / mL for mulberroside A, 0. 56 to 14. 00 μg / mL for moracin M, 0. 38 to 9. 50 μg / mL for dihydromorin, 26. 55 to 663. 75 μg / mL for baicalin, 4. 66 to 116. 50 μg / mL for wogonoside, 5. 87 to 146. 75 μg / mL for praeruptorin A, 1. 71 to 42. 75 μg / mL for praeruptorin B and 2. 39 to 59. 75 μg / mL for praeruptorin E, respectively. The average recovery rates for each component at low, medium and high concentrations ranged from 96. 83% to 100. 14%, with relative standard deviation ( RSD) ≤1. 42% ( n = 9). The results obtained by using the HPLC-QAMS technology showed no significant difference from those obtained by using the external standard method (ESM). Conclusion: HPLC-QAMS technology provides a fast and feasible multi-marker simultaneous quality evaluation model for Xiao’er Kesouning syrup.
Key words:  high-performance liquid chromatography combined with quantitative analysis of multi-components by single-marker  Xiao’ er Kesouning syrup  relative correction factor  content determination

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