UPLC法测定生、制白术配伍枳术丸中10种成分

Determination of ten constituents in raw and processed Atractylodes macrocephala compatible Zhizhu Pills by UPLC

目的建立UPLC法测定生、制白术配伍枳术丸中橙皮苷、柚皮苷、芸香柚皮苷、柚皮素、橙皮素、辛弗林、荷叶碱、白术内酯Ⅱ、白术内酯Ⅰ、白术内酯Ⅲ中的含有量。方法枳术丸甲醇提取物的分析采用ACQUITY UPLC HSS T3色谱柱(2. 1 mm×100 mm,1. 8μm);流动相0. 1%甲酸-0. 1%甲酸乙腈,梯度洗脱;体积流量0. 4 m L/min;柱温30℃;283 nm波长下测定橙皮苷、柚皮苷、芸香柚皮苷、柚皮素、橙皮素、辛弗林、荷叶碱、白术内酯Ⅱ;220 nm波长下测定白术内酯Ⅰ、白术内酯Ⅲ。结果 10种成分在各自范围内线性关系良好(r>0. 999 0),平均加样回收率97. 5%~100. 6%,RSD 1. 89%~3. 16%。结论该方法准确稳定,重复性好,可用于枳术丸的质量控制。

AIM To establish a UPLC method for the content determination of hesperidin, naringin,narirutin,naringenin,hesperetin,synephrine,nuciferine,atractylenolide Ⅱ,atractylenolide Ⅰ and atractylenolide Ⅲin raw and processed Atractylodes macrocephala Koidz. compatible Zhizhu Pills. METHODS The analysis of methanol extract of Zhizhu Pills was performed on a 30 ℃ thermostatic ACQUITY UPLC HSS T3 column(2. 1 mm×100 mm,1. 8 μm),with the mobile phase comprising of 0. 1% formic acid-0. 1% formic acid flowing at 0. 4 m L/min in a gradient elution manner,and the detection wavelengths of hesperidin,naringin,narirutin,naringenin,hesperetin,synephrine,nuciferine,atractylenolide Ⅱ and the detection wavelengths of atractylenolideⅠ,atractylenolide Ⅲ were set at 283,220 nm. RESULTS Ten constituents showed good linear relationships within their own ranges( r > 0. 999 0),whose average recoveries were 97. 5%-100. 6%, with the RSDs of1. 89%-3. 16%. CONCLUSION This accurate,stable and reproducible method can be used for the quality control of Zhizhu Pills.