HPLC双波长法同时测定2种枳术丸中8种有效成分的含量

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-C₁₈（4.6 mm×250 mm，5 μm）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1 mL·min^-1，柱温30℃，检测波长283 nm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6 h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 double-wavelength HPLC method for simultaneous determination of eight main compounds in Citrus aurantium L.-Zhizhu pills and C. sinensis Osbeck-Zhizhu pills. Methods: The separation was performed on an Agilent XDB-C₁₈ (4.6 mm×250 mm, 5 μm) column. The mobile phase consisted of 0.01% sodium dihydrogen phosphate water solution(A)-acetonitrile(B) with gradient elute(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) at a flow rate of 1 mL·min^-1. The column temperature was 30℃.. The detection wavelength was 283 nm for narirutin,naringin, hesperidin,neohesperidin and atractylenolide Ⅰ,and 220 nm for atractylenolide Ⅱ,atractylenolide Ⅲ and atractylon. Results: The determination should be completed within 6 h after the sample solution was prepared due to the instability of atractylon. All the compounds had good linearity in the defined ranges and the RSDs of recoveries(99.14%-102.6%) of them were below 3%,respectively. All of the eight compounds were determined in Citrus aurantium L.-Zhizhu pills, while naringin and hesperidin were not detected in C. sinensis Osbeck-Zhizhu pill. Conclusion: The established method can be applied to quality control of Zhizhu pills according to the methodology validation.