HPLC法测定白术饮片中多种化学成分的含量

Simultaneous determination of multiple components in decoction pieces of Atractylodes Macrocephala by HPLC

目的:建立4种白术饮片(白术、麸炒白术、土白术、焦白术)中白术内酯Ⅰ、Ⅱ、Ⅲ及苍术酮的"一测多评"含量测定方法。方法:采用Kromasil 100-5C_(18)色谱柱(4.6 mm×250 mm,5μm);以乙腈(A)-水(B)为流动相,梯度洗脱,流速1.0 mL·min^(-1),按照4个对照品出峰次序采用220、276、200 nm梯度波长检测,以丹皮酚为参照物,确定了白术内酯Ⅰ、Ⅱ、Ⅲ及苍术酮的相对于丹皮酚的相对校正因子,利用相对校正因子计算4种成分的含量,实现一测多评;同时采用外标法测定4种成分的含量,并比较两者差异,验证一测多评方法的可行性。结果:在一定线性范围内,各成分相对校正因子在不同实验条件下重现性良好,一测多评法计算值与外标法实测值之间无明显差异,两者相对偏差在0.05%~0.48%之间。结论:该方法简便,测定结果准确,解决了白术中所含脂溶性成分稳定性差,对照品价格昂贵难题,对不同白术饮片的评价提供了可行的方法和依据。

Objective： To determine atractylenolide Ⅰ , atractylenolide Ⅱ , atractylenolide m and atractylone in 4 kinds of decoction pieces of Atractylodes Macrocephala by single maker （ QAMS ） method. Methods： The Kromasil 100-5C18 column （ 4.6 mm × 250 mm, 5 μm ） was adopted . The mobile phase was consisted of acetonitrile （ A ） -water （ B ） with gradient elution at a flow rate of 1.0 mL · min-1. The detection wavelength was set at 220, 276 and 200 nm with gradient wavelength by the peak order. Paeonol was used as an internal reference standard and the relative correction factors （ RCFs ） of atractylenolide Ⅰ , atractylenolide Ⅱ , tractylenolide Ⅲ and atractylone to paeonol were calculated. Their contents in Atractylodes Macrocephala were determined by the external standard method （ ESM ） and QAMS method, respectively. The QAMS method was validated through comparison with the results obtained from the ESM method. Results： Within a certain range of linearity, each component＇s relative correcting factor was reproducible under different experimental conditions. The method of QAMS and external standard method for four components was established in Atractylodes Macrocephala and. There were no significant differences between the results of the two methods, and the standard deviation was between 0.05% and 0.48%. Conclusion： The method was simple and accurate, and solved the problem of unstable and expensive reference substances, thus providing feasible method and basis for quality evaluation of different decoction pieces of Atractylodes Macrocephala.