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[摘要]
目的 建立UPLC法同时测定荷丹片中荷叶碱、补骨脂素、异补骨脂素、丹参酮IIA、丹参素、番泻苷A、番泻苷B、熊果酸8种指标成分的量。方法 采用UPLC法,Acquity UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm),甲醇-乙腈(40∶60,A)-0.1%甲酸水溶液(B)为流动相,体积流量0.6 mL/min,梯度洗脱:0~4.0 min,90% B;4.0~6.0 min,90%~80% B;6.0~9.0 min,80%~70% B;9.0~10.5 min,70%~60% B;10.5~12.0 min,60%~50% B,12.0~16.0 min,50%~10% B;分段变波长测定:0~4.0 min为215 nm,4.0~12.0 min为270 nm,12.0~16.0 min为340 nm;柱温40 ℃;进样量1 μL。分别对线性关系、精密度、重复性、稳定性及加样回收率进行考察。结果 被测定的8种指标成分分别在选定的范围内线性关系良好;精密度良好,RSD均小于3.0%;重复性良好,RSD均小于3.0%;在室温条件下24 h内稳定;平均加样回收率在99.21%~101.91%,RSD均小于3.0%。结论 本方法操作简便,测定结果准确可靠,可用于荷丹片的质量控制。
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[Abstract]
Objective To develop a UPLC method for the simultaneous determination of nuciferine, psoralen, isopsoralen, tanshinone IIA, danshensu, sennoside A, sennoside B, and ursolic acid in Hedan Tablets. Methods The chromatographic separation was achieved on an Acquity UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with methanol-acetonitrile (40∶60, A)-0.1% formic acid (B) as mobile phases at the flow rate of 0.6 mL/min for gradient elution: 0-4.0 min, 90% B; 4.0-6.0 min, 90%-80% B; 6.0-9.0 min, 80%-70% B; 9.0-10.5 min, 70%-60% B; 10.5-12.0 min, 60%-50% B, 12.0-16.0 min, 50%-10% B; Detection with variable wavelength: 0-4.0 min was 215 nm, 4.0-12.0 min was 270 nm, 12.0-16.0 min was 340 nm, and the column temperature was 40 ℃. Its linear relationship, precision, repeatability, stability, and recoveries were investigated. Results The results showed that the eight active components were well separated and showed good linearity. The precision was good and RSD was less than 3.0%. The repeatability was good and RSD was less than 3.0%. The stability was good in 24 h. The average recoveries were between 99.21%-101.91% and RSD was less than 3.0%. Conclusion The method is accurate, sensitive, credible, and repeatable. It could be applied to the quality control of Hedan Tablets.
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