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目的建立HPLC法测定龙胆药材(饮片)中龙胆苦苷和落干酸的方法,提升龙胆药材(饮片)质量标准。方法 Fortis Xi-C18色谱柱(250 mm×4.0 mm,5μm),以乙腈-0.1%磷酸梯度为流动相(0→30 min,8:92→20:80),流速1.0 ml·min-1,检测波长240 nm,柱温25℃。结果龙胆苦苷和落干酸分别在10.02~501.00 mg·L-1和1.01~160.96 mg·L-1内线性关系良好,平均回收率分别为100.2%(RSD为1.51%,n=9)和98.55%(RSD为2.26%,n=9)。所测定39批样品中,坚龙胆中龙胆苦苷含量范围为1.40%~4.82%,落干酸含量范围为0.50%~1.06%;龙胆中龙胆苦苷含量范围为2.35%~4.21%,落干酸含量范围为0.96%~2.76%。结论该方法简单,准确,灵敏,可靠,重现性好,可用于龙胆药材(饮片)质量控制研究。
Objective To establish a method for the determination of gentiopicroside and ascorbic acid in gentian medicinal herbs (Pieces) by HPLC and to improve the quality standards of gentian herbs (Pieces). Methods The mobile phase (0 → 30 min, 8:92 → 20:80) was eluted with a gradient of acetonitrile-0.1% phosphoric acid on a Fortis Xi-C18 column (250 mm × 4.0 mm, 5 μm) Detection wavelength 240 nm, column temperature 25 ℃. Results The linear relationship between gentiopicroside and ascorbic acid was 10.02 ~ 501.00 mg · L-1 and 1.01 ~ 160.96 mg · L-1, respectively. The average recoveries were 100.2% (RSD 1.51%, n = 9) And 98.55% (RSD 2.26%, n = 9). Among the 39 batches of samples tested, the content of gentiopicroside in Gentiana scabra was 1.40% -4.82%, the range of dry acid content was 0.50% ~ 1.06%, and the content of gentiopicroside in Gentiana scabra was 2.35% -4.21 %, Falling acid content range of 0.96% ~ 2.76%. Conclusion The method is simple, accurate, sensitive, reliable, reproducible and can be used for the quality control of gentian medicine (Pieces).