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目的:建立一种可以同时测定健儿消食口服液中毛蕊异黄酮苷、橙皮苷和黄芩苷含量的高效液相色谱法。方法:样品用甲醇超声提取;采用Agilent ZORBAXSB-C18(150 mm×4.6 mm,3.5μm)色谱柱,以乙腈(A)-1%乙酸溶液为流动相,梯度洗脱(0~10 min,5%A→10%A;10~19 min,10%A→11%A;19~27 min,11%A;27~40 min,11%A→14%A;40~45 min,14%A→15%A;45~60 min,15%A;60~70 min,15%A→17%A;70~80 min,17%A→20%A),流速1.0 m L·min-1,检测波长242nm,柱温30℃,进样量10μL。结果:毛蕊异黄酮苷、橙皮苷和黄芩苷的线性范围分别为0.002 9~0.116 0、0.069 2~2.760、0.475~19.000μg;平均加样回收率(n=6)分别为95.3%、99.0%、97.0%,RSD分别为1.5%、1.6%、1.1%。20批样品中毛蕊异黄酮苷、橙皮苷和黄芩苷含量测定结果为:毛蕊异黄酮苷的含量范围为0.007 9~0.024 8 mg·m L-1,橙皮苷的含量范围为0.217~0.376 mg·m L-1,黄芩苷的含量范围为1.310~2.587 mg·m L-1。结论:经方法学验证,本法可测定制剂中毛蕊异黄酮苷、橙皮苷和黄苓苷的含量。
OBJECTIVE: To establish a high performance liquid chromatography (HPLC) method that can simultaneously determine the content of calycosin, hesperidin and baicalin in Jian’er Xiaoshi oral liquid. METHODS: The samples were extracted with methanol by ultrasonic wave. The mobile phase was eluted with acetonitrile (A) -1% acetic acid (0-10 min, 5%) using Agilent ZORBAXSB-C18 column (150 mm × 4.6 mm, % A → 10% A; 10-19 min, 10% A → 11% A; 19-27 min, 11% A; 27-40 min, 11% A → 14% A; 40-45 min, 14% A 15 to 60 min, 15% A to 60 to 70 min, 15 to 17% A, 70 to 80 min, 17% A to 20% A) at a flow rate of 1.0 m L · min- Detection wavelength 242nm, column temperature 30 ℃, injection volume 10μL. Results: The linear range of curcuma longa isoflavone glycosides, hesperidin and baicalin were 0.002 9 ~ 0.116 0, 0.069 2 ~ 2.760 and 0.475 ~ 19.000 μg, respectively. The average recoveries (n = 6) were 95.3% and 99.0% , 97.0%, RSD respectively 1.5%, 1.6%, 1.1%. The results of determination of the content of calycosin, hesperidin and baicalin in 20 batches of samples were as follows: the content of calycosin in the range of 0.007 9 to 0.024 8 mg · m L -1 and the content of hesperidin in the range of 0.217 to 0.376 mg · m L-1, baicalin content ranged from 1.310 to 2.587 mg · m L-1. Conclusion: This method can be used to verify the content of calycosin, hesperidin and yanglin in the preparation by the methodological verification.