Lin Fei-Fei, Xie Wen-Bing, Yu Jie, Xu Wei-Guo, Niu Feng-Lan
School of Public Health, Jilin University, Changchun 130021, China.
Zhongguo Zhong Yao Za Zhi. 2013 May;38(10):1518-20.
To develop an HPLC method for simultaneous determination of gallic acid and hesperidin in Xiaogu capsule, in order to provide a simple, rapid and accurate method for quality control of the compound preparation of traditional Chinese medicine.
Xiaogu capsule was extracted with methanol heating reflux method. Synergi 4 mu Hydro-RP 80A (4.6 mm x 250 mm, 5 microm) was adopted as the chromatographic column, with acetonitrile--0.04 mol x L(-1) phosphate monobasic sodium solution (20: 80) as the mobile phase. The flow rate was 1.0 mL x min(-1), the detection wavelength was 283 nm, and the column temperature was 25 degrees C.
Under the conditions, gallic acid and hesperidin reached the baseline resolved peak, with a good linearity within the range of 21.6-216.0 mg x L(-1) (r = 0.999 93) for gallic acid, and 4.5-45.0 mg x L(-1) (r = 0.999 95) for hesperidin, respectively. Their average recoveries (n = 9) were 101.5% (RSD 3.7%) and 94.7% (RSD 2.7%), respectively. The average contents of gallic acid and hesperidin contained in Xiaogu capsule were detected to 5.10% and 0.091 1%, respectively.
The method established in this study can determine the content of gallic acid and hesperidin contained in Xiaogu capsule in a rapid and accurate manner, which provided reference for quality evaluation of the medicine.
建立高效液相色谱法同时测定消骨胶囊中没食子酸和橙皮苷的含量，为该中药复方制剂的质量控制提供简便、快速、准确的方法。
采用甲醇加热回流法提取消骨胶囊。以Synergi 4μm Hydro-RP 80A（4.6mm×250mm，5μm）为色谱柱，乙腈-0.04mol·L⁻¹磷酸二氢钠溶液（20∶80）为流动相。流速为1.0mL·min⁻¹，检测波长为283nm，柱温为25℃。
在此条件下，没食子酸和橙皮苷达到基线分离峰，没食子酸在21.6～216.0mg·L⁻¹范围内线性关系良好（r = 0.999 93），橙皮苷在4.5～45.0mg·L⁻¹范围内线性关系良好（r = 0.999 95）。它们的平均回收率（n = 9）分别为101.5%（RSD 3.7%）和94.7%（RSD 2.7%）。测得消骨胶囊中没食子酸和橙皮苷的平均含量分别为5.10%和0.091 1%。
本研究建立的方法能快速、准确地测定消骨胶囊中没食子酸和橙皮苷的含量，为该药物的质量评价提供了参考。
