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D_3、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×5μm,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30min,过滤蒸干后以50%甲醇（ν/ν）定容至5m L容量瓶中;漂移管温度为75℃,氮气流量为2.5L/min。去芹糖桔梗皂苷E、桔梗皂苷E、桔梗皂苷D_3、去芹糖桔梗皂苷D、桔梗皂苷D分别在0.64~6.4μg、1.22~12.2μg、1.08~10.8μg、0.74~7.4μg,1.7~17μg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。
Simultaneously determination of the 5 platycosides in Platycodon radix with HPLC-ELSD method. Gradient elution （0-15rain, 20%-22%A; 15-60min, 22%A; 60-65min, 22%-30%A; 65-70 min, 30%-20%A） is carried out under the following conditions： ODS 250 silica gel as solid phase （250mm×4.6mm×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 （v/v） for 30min, filtered and dried by distillation before further dilution with 50% methanol （v/v） 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 0.64-6.4μg, 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.
出处
《中国测试》
CAS
北大核心
2016年第1期49-52,共4页
China Measurement & Test
