目的: 建立1种快速准确检测复方丹参片中5个三萜皂苷类成分的固相萃取净化-高效液相色谱的方法,为复方丹参片中三七项质量评价提供参考。方法: 样品经70%甲醇水超声提取,经过聚苯乙烯包覆硅胶键合C18固相萃取柱净化后,采用Chrom Core 300 C18色谱柱(100 mm×3.0 mm,3 μm)进行分离,以乙腈-0.1%磷酸水溶液为流动相进行梯度洗脱,紫外检测波长为203 nm检测。结果: 所建方法可以使干扰成分大幅减少,三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1和人参皂苷Rd 5个三萜皂苷类成分能够有效分离,分析时间缩短为20 min,并分别在5.0~100.0、20.0~400.0、5.0~100.0、20.0~400.0、20.0~400.0 μg·mL-1浓度范围内具有良好的线性关系,相关系数(r≥0.999 9)。方法的重复性良好(RSD≤1.0%),平均回收率为94.4%~98.2%(RSD≤1.4%,n=6),满足定量分析要求。结论: 该方法快速灵敏,耐用性好,回收率和重复性良好,可作为复方丹参片三萜皂苷类成分评价的依据。
Objective: To establish a rapid and accurate assay method using solid phase extraction (SPE) and HPLC for simultaneously determining five triterpene glycosides in Fufang Danshen tablets. Methods: The sample was extracted with 70% methanol and purified with polystyrene coated silica bonding C18 SPE cartridge. A gradient elution with acetonitrile and 0.1% phosphoric acid was performed on ChromCore 300 C18 (100 mm×3.0 mm, 3 μm) at wavelength of 203 nm. Results: The target compounds in Fufang Danshen tablets, i.e. notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ginsenoside Rd were simultaneously detected without interference within an analytical time of 20 min. All calibration curves showed good linear regression (r>0.999 9) within ranges of 5.0-100.0, 20.0-400.0, 5.0-100.0, 20.0-400.0, 20.0-400.0 and 20.0-400.0 μg·mL-1, respectively. The established method showed good repeatability (RSD≤1.0%) and good recovery (ranging from 94.4% to 98.2%, RSD≤1.4%, n=6). Conclusion: The method is reliable for the quantification of four triterpene glycosides in Fufang Danshen tablets.
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