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目的:建立艾可清胶囊中毛冬青皂苷甲的硅胶薄层色谱(TLC)鉴别方法和高效液相色谱-蒸发光散射(HPLC-ELSD)检测的含量测定方法。方法:自药材中分离鉴定毛冬青皂苷甲;确定TLC条件;采用ODS色谱柱(4.6 mm×250 mm,5μm)及保护柱,以甲醇-0.2%冰醋酸(67∶33)为流动相,ELSD检测器,漂移管温度95℃,载气流速2.5 L.min-1,柱温30℃,流速1.0 mL.min-1作为HPLC条件。结果:设立的TLC条件可以从复方制剂中检出毛冬青皂苷甲;建立的HPLC含量测定方法,毛冬青皂苷甲在1.92～9.60μg呈良好线性关系(r=0.999 5),平均回收率为99.85%,RSD 1.04%。结论:建立的毛冬青皂苷甲的硅胶TLC鉴别方法和HPLC-ELSD含量测定方法具有操作快捷、方法准确的特点,可作为毛冬青药材及其复方制剂的质量控制方法。
OBJECTIVE: To establish TLC identification method and HPLC-ELSD method for determination of Maoqingqing saponin in Ai Keqing Capsule. METHODS: Maodong saponin A was isolated and identified from medicinal materials. The TLC conditions were determined. ODS column (4.6 mm × 250 mm, 5 μm) and protective column were used with methanol-0.2% glacial acetic acid (67:33) The detector, drift tube temperature 95 ℃, carrier gas flow rate 2.5 L.min-1, column temperature 30 ℃, flow rate 1.0 mL · min-1 as HPLC conditions. Results: The TLC conditions were established to detect Mao Dongqing saponin A from the compound preparation. The established HPLC method showed that Mao Dong Qing saponin A had a good linear relationship (r = 0.999 5) with an average recovery of 99.85 %, RSD 1.04%. CONCLUSION: The method of TLC identification and HPLC-ELSD determination of Mao hollysin saponin A has the advantages of quick operation and accurate method, which can be used as the quality control method of Mao Dong Qing medicine and its compound preparation.