目的 建立一測(cè)多評(píng)法同時(shí)測(cè)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(cè)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(dòng)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(cè)波長(zhǎng)254 nm，柱溫35℃，進(jìn)樣量10 μL，并進(jìn)行專(zhuān)屬性、線性關(guān)系、重復(fù)性、精密度、加樣回收率等方法學(xué)驗(yàn)證；以黃芩苷為內(nèi)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(duì)校正因子，并進(jìn)行含量測(cè)定。采用外標(biāo)法測(cè)定15批小柴胡顆粒中的7個(gè)指標(biāo)性成分對(duì)一測(cè)多評(píng)法的準(zhǔn)確性進(jìn)行驗(yàn)證。結(jié)果 建立的HPLC法方法學(xué)驗(yàn)證結(jié)果符合要求；以黃芩苷為內(nèi)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(duì)于黃芩苷的相對(duì)校正因子分別為0.78、0.52、0.57、1.80、0.82、1.08。一測(cè)多評(píng)法所測(cè)結(jié)果與外標(biāo)法無(wú)顯著性差異。結(jié)論 該方法簡(jiǎn)單、可靠、耐用性良好，可用于小柴胡顆粒的質(zhì)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(guó)家重點(diǎn)研發(fā)計(jì)劃（2018YFC1707300）