目的 建立一測多評法同時測定小柴胡顆粒中黃芩苷、漢黃芩苷、黃芩素、漢黃芩素、甘草酸、柴胡皂苷B₂、柴胡皂苷B₁的含量。方法 建立高效液相色譜（HPLC）法檢測小柴胡顆粒中黃芩苷、漢黃芩苷、黃芩素、漢黃芩素、甘草酸、柴胡皂苷B₂、柴胡皂苷B₁的含量，色譜柱為Waters XBridge C₁₈柱（150 mm×4.6 mm，3.5 μm），流動相為甲醇（A）-0.1%磷酸溶液（B），梯度洗脫，體積流量0.8 mL/min，檢測波長254 nm，柱溫35℃，進樣量10 μL，并進行專屬性、線性關系、重復性、精密度、加樣回收率等方法學驗證；以黃芩苷為內參物，建立其與漢黃芩苷、黃芩素、漢黃芩素、甘草酸銨、柴胡皂苷B₂和柴胡皂苷B₁的相對校正因子，并進行含量測定。采用外標法測定15批小柴胡顆粒中的7個指標性成分對一測多評法的準確性進行驗證。結果 建立的HPLC法方法學驗證結果符合要求；以黃芩苷為內參物，漢黃芩苷、黃芩素、漢黃芩素、甘草酸銨、柴胡皂苷B₂、柴胡皂苷B₁相對于黃芩苷的相對校正因子分別為0.78、0.52、0.57、1.80、0.82、1.08。一測多評法所測結果與外標法無顯著性差異。結論 該方法簡單、可靠、耐用性良好，可用于小柴胡顆粒的質量控制。

Objective To establish a quantitative analysis of multi-components by single-marker (QAMS) method for the simultaneous determination of baicalin, wogonoside, baicalein, wogonin, glycyrrhizic acid, saikoside B₂, saikoside B₁ in Xiaochaihu Granules. Methods A HPLC method was established for the determination of baicalin, wogonin, baicalein, wogonin, glycyrrhizic acid, saikosaponin B₂ and saikosaponin B₁ in Xiaochaihu granules. The chromatographic column was waters XBridge C₁₈ column (150 mm×4.6 mm, 3.5 μm), The mobile phase was methanol (A)-0.1% phosphoric acid solution (B). The flow rate was 0.8 mL/min, the detection wavelength was 254 nm, the column temperature was 35℃, and the injection volume was 10 μL. The relative correction factors of wogonoside, baicalein, wogonin, ammonium glycyrrhetate, saikosaponin B₂ and saikosaponin B₁ were calculated by using baicalin as an internal reference substance in this study. In order to validate the accuracy, 15 batches of Xiaochaihu Granules were determined and compared by both QAMS and external standard method (ESM). Results The validation results met the requirements. Using baicalin as the internal reference substance, the relative correction factors of wogonoside, baicalein, wogonin, ammonium glycyrrhetate, saikosaponin B₂ and saikosaponin B₁ were 0.78, 0.52, 0.57, 1.80, 0.82, 1.08, respectively. There was no significant difference between QAMS and ESM. Conclusion The simple, reliable and robust QAMS can be used for the quality control of Xiaochaihu Granules.

R284.1

國家重點研發(fā)計劃（2018YFC1707300）