论文部分内容阅读
目的建立应用小粒径色谱柱快速测定红景天(蔷薇红景天)提取物中红景天苷、酪醇和络赛维的HPLC方法。方法色谱柱为HALO C18(150 mm×4.6 mm,2.7μm);流动相为乙腈(A)-0.1%甲酸水溶液(B),梯度洗脱:0～5 min,7%～15%A;5～8 min,15%～18%A;8～20 min,18%～30%A;20～25 min,30%～40%A;25～30 min,40%～55%A;体积流量0.6 mL/min;柱温30℃;检测波长280 nm;进样量5μL。结果红景天苷、酪醇、络赛维15 min内达到分离,峰形尖锐对称,线性范围分别为0.41～106.00、0.42～108.00、0.38～98.00μg/mL,平均加样回收率分别为99.29%、98.82%、98.33%。采用所建立的方法测定不同来源红景天提取物的多种成分,结果表明单一采用红景天苷作为质量控制指标,9批样品的差异度较小(RSD=7.95%),如果将酪醇或络赛维引入质量评价体系,则红景天提取物各批次间就存在较大的差异(酪醇,RSD=24.42%;络赛维,RSD=50.55%);但是,同一单位提供的样品间的差异度较小。结论建立的HPLC-小粒径色谱柱法高效、准确,经济,精密度好,灵敏度高,可用于红景天提取物中的红景天苷、酪醇和络赛维的同时快速测定;引入多成分的测定方法,可以评价不同厂家提取物质量的差异,并筛选出导致质量差异的成分,为提取物的工艺优化提供参考。
OBJECTIVE To establish a rapid HPLC method for the determination of salidroside, tyrosol and sildenafil from the extracts of Rhodiola rosea with small particle size columns. Methods The column was HALO C18 (150 mm × 4.6 mm, 2.7 μm). The mobile phase consisted of acetonitrile (A) -0.1% formic acid in water (B) with gradient elution: 0-5 min and 7-15% A; 8 to 20 min, 18 to 30% A; 20 to 25 min, 30 to 40% A; 25 to 30 min, 40 to 55% A; volume flow rate 0.6 mL / min; column temperature 30 ℃; detection wavelength 280 nm; injection volume 5μL. Results Salidroside, tyrosol and sildenafil were separated within 15 min. The peak shape was sharp and symmetrical. The linear range was 0.41 ~ 106.00,0.42 ~ 108.00,0.38 ~ 98.00 μg / mL, and the average recoveries were 99.29 %, 98.82%, 98.33%. The results showed that using salidroside alone as a quality control index, the difference of 9 batches of samples was small (RSD = 7.95%). If the tyrosol (RSD = 24.42%; RSD = RSD = 50.55%); however, the same unit provided that there was a big difference between batches of Rhodiola rosea extract The difference between samples is small. Conclusion The established HPLC-small particle size column method is efficient, accurate, economical, accurate and sensitive. It can be used for simultaneous determination of salidroside, tyrosol and sildenafil in Rhodiola extract. Determination of ingredients, can evaluate the differences in the quality of extracts from different manufacturers, and filter out the ingredients that lead to differences in quality, extract for the process to provide a reference.