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    HPLC-ELSD法同时测定桔梗中5种皂苷含量

    2016-03-03 中国测试岳 虹, 陈芙蓉, 王梦丽, 谢红英, 冯亚男, 徐小平
    摘  要:建立高效液相色谱法同时测定桔梗药材中去芹糖桔梗皂苷E、桔梗皂苷E、桔梗皂苷D3、去芹糖桔梗皂苷D、桔梗皂苷D的方法。色谱柱为ODS 250 mm×4.6 mm×5 μm,流动相A为乙腈-0.2%甲酸,流动相B为水,采用梯度洗脱(0~15 min,20%~22%A;15~60 min,22%A;60~65 min,22%~30%A;65~70 min,30%~20%A)。供试品经50%甲醇(ν/ν)超声提取30 min,过滤蒸干后以50%甲醇(ν/ν)定容至5 mL容量瓶中;漂移管温度为75 ℃,氮气流量为2.5 L/min。去芹糖桔梗皂苷E、桔梗皂苷E、桔梗皂苷D3、去芹糖桔梗皂苷D、桔梗皂苷D分别在0.64~6.4 μg、1.22~12.2 μg、1.08~10.8 μg、0.74~7.4 μg,1.7~17 μg范围内组分浓度与峰面积线性关系良好;药材中5种成分的平均加标回收率分别为101.1%、99.9%、100.4%、100.7%和101.6%;RSD均<5%。该方法简便、准确,分离效果好,可用于桔梗药材的质量控制。
    关键词:桔梗;桔梗皂苷;HPLC-ELSD;梯度洗脱
    文献标志码:A       文章编号:1674-5124(2016)01-0049-04
    Simultaneous determination of the content of 5 Platycosides in Platycodon radix
    YUE Hong, CHEN Furong, WANG Mengli, XIE Hongying, FENG Ya’nan, XU Xiaoping
    (West China School of Pharmacy,Sichuan University,Chengdu 610041,China)
    Abstract: Simultaneously determination of the 5 platycosides in Platycodon radix with HPLC-ELSD method. Gradient elution (0-15 min, 20%-22%A; 15-60 min, 22%A; 60-65 min, 22%-30%A; 65-70 min, 30%-20%A) is carried out under the following conditions: ODS 250 silica gel as solid phase (250 mm×4.6 mm×5 μm), acetonitrile - 0.2% methanoic acid as mobile phase A, and water as mobile phase B; the test products are ultrasonically extracted with 50% methanol (ν/ν) for 30 min, filtered and dried by distillation before further dilution with 50% methanol (ν/ν) to a 5 mL volumetric flask; and the drift tube is set at 75 ℃ and the nitrogen flow rate 2.5 L/min. The composition concentration shows a good linear relationship with the peak area when deapioplatycoside E, platycoside E, platycodin D3, deapioplatycodin D and platycodin D are 0.64-6.4 μg, 1.22-12.2 μg, 1.08-10.8 μg, 0.74-7.4 μg and 1.7-17 μg respectively. The average recoveries of the five ingredients are 101.1%, 99.9%, 100.4%, 100.7% and 101.6% respectively. All the RSDs are lower than 5%. The method is simple, accurate and efficient, suitable for the quality control of Platycodon  radix.
    Keywords: Platycodon radix; Platycoside; HPLC-ELSD; gradient elution
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