目的 建立HPLC法測定通便寧片中咖啡酸、兒茶素、表兒茶素、芹菜素-6,8-二-C-葡萄糖苷、異鼠李素-3-O-β-龍膽二糖苷、番瀉苷B、番瀉苷A、丁內未利葡萄糖苷，結合化學計量學綜合評價產品質量。方法 采用Discovery C₁₈色譜柱（250 mm×4.6 mm，5μm），流動相0.3%冰醋酸–乙腈，梯度洗脫；檢測波長為325 nm（0～13 min檢測咖啡酸）、270 nm（13～55 min檢測兒茶素、表兒茶素、芹菜素-6,8-二-C-葡萄糖苷、異鼠李素-3-O-β-龍膽二糖苷、番瀉苷B、番瀉苷A和丁內未利葡萄糖苷）；柱溫30℃；體積流量1.0 mL/min；進樣量10 μL。運用聚類分析（CA）、主成分分析（PCA）、正交偏最小二乘判別分析法（OPLS-DA）對測定結果進行綜合分析。結果 咖啡酸、兒茶素、表兒茶素、芹菜素-6,8-二-C-葡萄糖苷、異鼠李素-3-O-β-龍膽二糖苷、番瀉苷B、番瀉苷A、丁內未利葡萄糖苷分別在0.49～12.25、0.36～9.00、1.08～27.00、4.15～103.75、39.47～986.75、43.71～1092.75、29.20～730.00、8.57～214.25 μg/mL線性關系良好，平均回收率分別為96.99%、97.28%、98.01%、99.33%、100.03%、99.74%、100.10%、98.85%，RSD值分別為1.43%、0.89%、1.55%、0.72%、0.58%、0.66%、0.82%、1.31%。12批通便寧片樣品可聚為3類，不同的生產周期呈現(xiàn)一定的差異性；番瀉苷B、異鼠李素-3-O-β-龍膽二糖苷和番瀉苷A是影響通便寧片產品質量的主要潛在標志物。結論 所建立的方法簡單可行，結合化學計量學可用于通便寧片質量的綜合評價，可為通便寧片的質量標準提升提供參考。

Objective To establish an HPLC method to determine the contents of caffeic acid, catechin, epicatechin, 6,8-di-C- glucosylapigenin, isorhamnetin 3-O-gentiobioside, sennoside B, sennoside A, and tinnevellin glucoside in Tongbianning Tablets, and to comprehensively evaluate quality by chemometrics analysis. Methods The separation was carried out on Discovery C₁₈column (250 mm×4.6 mm, 5 μm). The mobile phase was 0.3% glacial acetic acid-acetonitrile with gradient elution. The detection wavelength was set at 325 nm (0-13 min for caffeic acid) and 270 nm (13-55 min for catechin, epicatechin, 6,8-di-C- glucosylapigenin, isorhamnetin 3-O-gentiobioside, sennoside B, sennoside A, and tinnevellin glucoside). The column temperature was 30℃, the volume flow was 1.0 mL/min, and the injection volume was 10 μL. The results were comprehensively analyzed by using cluster analysis (CA), principal component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA). Results Caffeic acid,catechin, epicatechin, 6,8-di-C-glucosylapigenin, isorhamnetin 3-O-gentiobioside, sennoside B, sennoside A, and tinnevellin glucoside showed good linear relationships within the ranges of 0.49 -12.25, 0.36 -9.00, 1.08-27.00, 4.15-103.75, 39.47-986.75, 43.71-1 092.75, 29.20-730.00, and 8.57-214.25 μg/mL, whose average recoveries were 96.99%, 97.28%, 98.01%, 99.33%, 100.03%, 99.74%, 100.10%, and 98.85% with RSD values of 1.43%, 0.89%, 1.55%, 0.72%, 0.58%, 0.66%, 0.82%, and 1.31%, respectively. 12 Batches of Tongbianning Tablets could be clustered into three categories, and different production cycles show certain differences. Sennoside B, isorhamnetin 3-O-gentiobioside, and sennoside A were the main potential markers affecting the quality of Tongbianning Tablets. Conclusion The established method is simple and feasible, and can be used combined with chemometrics method for the comprehensive evaluation of the quality of Tongbianning Tablets, and can provide a reference for the improvement of the quality standard of Tongbianning Tablets.

R286

安徽省教育廳高校優(yōu)秀拔尖人才培育項目(gxyq2021265)