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目的:建立HPLC双波长法同时测定酸橙枳术丸和甜橙枳术丸中多成分的含量,为质量评价提供依据。方法:采用Agilent XDB-C(18)(4.6 mm×250 mm,5μm)色谱柱,以0.01%磷酸二氢钠水溶液(A)-乙腈(B)为流动相,梯度洗脱(0~5 min,5%B;5~7 min,5%B→10%B;7~10 min,10%B→16%B;10~25 min,16%B→18%B;25~42 min,18%B→35%B;42~55 min,35%B→58%B;55~65 min,58%B;65~75 min,58%B→100%B;75~85 min,100%B),流速1mL·min~(-1),柱温30℃,检测波长283nm测定芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷和白术内酯Ⅰ含量,220 nm测定白术内酯Ⅱ、白术内酯Ⅲ和苍术酮含量。结果:苍术酮不稳定,制备的供试品溶液应避光放置,并在制备后6h内完成检测;各成分在一定范围内线性关系良好;平均回收率介于99.14%~102.6%,RSD均小于3%。酸橙枳术丸中检测到8种待测成分,而甜橙枳术丸中没有检测到柚皮苷与新橙皮苷。结论:经方法学验证,本方法可为枳术丸质量控制提供依据。
OBJECTIVE: To establish a dual-wavelength HPLC method for the simultaneous determination of multi-component content of Zhisheng Zhizhu Pill and Sweet Orange Zhizhu Pills, and to provide basis for quality evaluation. METHODS: The mobile phase was eluted with gradient elution (0 ~ 5 min) using an Agilent XDB-C (18) (4.6 mm × 250 mm, 5 μm) column with 0.01% sodium dihydrogen phosphate (A) , 5% B; 5 to 7 min, 5% B to 10% B; 7 to 10 min, 10% B to 16% B; 10 to 25 min, 16% B to 18% B; % B → 35% B; 42-55 min 35% B → 58% B 55-65 min 58% B 65-75 min 58% B → 100% B 75-85 min 100% B ), flow rate 1mL · min ~ (-1), column temperature 30 ℃, measured narirutin, naringin, hesperidin, neohesperidin and atractylenolide ⅰ in the detection wavelength 283nm, 220 nm measured Atractylodes Ester Ⅱ, atractylodes lactone Ⅲ and atractyloside content. Results: The atractylodes macrocephala Ketone was unstable. The prepared test solution should be protected from light and tested within 6 hours after preparation. The linearity of each component was good within a certain range. The average recoveries ranged from 99.14% to 102.6% Less than 3%. There were 8 kinds of test components detected in the orange Zhizhu pill, but no naringin and neohesperidin were detected in the sweet orange Zhizhu pill. Conclusion: This method can provide the basis for the quality control of Zhizhu Pill by methodological verification.