[关键词]
[摘要]
目的 建立同时测定裸花紫珠中5个有效成分的超高效液相色谱(UPLC)方法。方法 采用Agilent Eclipse XDB-C18色谱柱(100 mm×3.0 mm,1.8 μm),流动相为乙腈(A)-0.1%甲酸水溶液(B),梯度洗脱,体积流量为0.7 mL/min。检测波长350 nm,柱温40 ℃。结果 木犀草苷、毛蕊花糖苷、木犀草素-4'-O-β-D-吡喃葡萄糖苷、木犀草素、5,4'-二羟基-3,7,3'-三甲氧基黄酮分别在2.44~122.0 μg/mL(r=0.999 8)、9.06~453.0 μg/mL(r=0.999 9)、4.42~221.0 μg/mL(r=0.999 9)、3.36~168.0 μg/mL(r=0.999 8)、2.52~126.0 μg/mL(r=0.999 8)内线性关系良好;平均回收率在98.5%~100.8%。结论 所建立的UPLC法简便快速、重复性良好、结果准确可靠,可作为裸花紫珠药材质量标准控制的方法。
[Key word]
[Abstract]
Objective To develop a UPLC method for the stimultaneous determination of five active ingredients in Callicarpa nudiflora. Methods Analysis was performed on an Agilent Eclipse XDB-C18 column (100 mm ×3.0 mm, 1.8 μm) eluted with acetonitrile (A) and 0.1% methanoic acid (B) in a gradient program. The flow rate was 0.7 mL/min, the detection wavelength was 350 nm, and the column temperature was 40 ℃. Results Luteoloside, acteoside, luteolin-4'-O-β-D-glucopyranoside, luteolin, and 5, 4'-dihydroxy-3, 7, 3'-trimethoxyflavone showed a good linearity in the ranges of 2.44-122.0 μg/mL (r = 0.999 8), 9.06-453.0 μg/mL (r = 0.999 9), 4.42-221.0 μg/mL (r = 0.999 9), 3.36-168.0 μg/mL (r = 0.999 8), and 2.52-126.0 μg/mL (r = 0.999 8). The average recoveries, measured at three concentration levels, varied from 98.5%-100.8%. Conclusion The method is simple, accurate, and can be used for the quality control of C. nudiflora.
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[基金项目]
国家自然科学基金资助项目(81373955);中国食品药品检定研究院中青年发展研究基金课题(2013WA9)