摘要
目的建立高效液相色谱法同时测定枳术丸中白术内酯Ⅰ等4种成分的含量。方法采用反相高效液相方法分离检测柚皮苷、橙皮苷及新橙皮苷和白术内酯Ⅰ。色谱柱:symmtryC18(250mm×4.6mm,5μm);以甲醇-0.1%磷酸溶液(梯度洗脱)为流动相;测定波长:283nm和224nm;流速:1.0mL·min-1;柱温:30℃;进样量:10μL。结果测定3批枳术丸中,柚皮苷、橙皮苷、新橙皮苷及白术内酯Ⅰ含量分别为10.77±0.61、1.16±0.13、9.41±0.09、0.38±0.02mg·g-1,并且4种成分得到完全分离,柚皮苷平均回收率为98.81%(RSD=1.11%,n=6);橙皮苷平均回收率为100.63%(RSD=1.90%,n=6);新橙皮苷平均回收率为99.32%(RSD=1.44%,n=6);白术内酯Ⅰ平均回收率为99.65%(RSD=1.53%,n=6)。结论该方法准确、可靠、重复性好,可作为枳术丸质量控制方法。
Objective To develop a method for simultaneous determination of 4 compounds in Zhizhu Pills by HPLC. Method Reversed-phase HPLC was used to determine the content of the compounds such as hesperidin, naringin, neohesperidin and atractylenolide Ⅰ. The column was symmetry C18（250 mm × 4.6 mm, 5 μm） with temperature of 30 ℃. Methanol - 0. 095 % phosphoric acid solution served as the mobile phase by gradient elution. The wavelength of detection was set at 283 nm and 224 nm. The injection volume was 10 μL and the flow rate was 1.0 mL/min. Results Hesperidin, naringin, neohesperidin and atractylenolide Ⅰ in Zhizhu Pills can he isolated completely. Three batches of samples were determined and the recoveries of naringin, hesperidin, neohesperidin and atractylenolide Ⅰ were 98.81%（RSD=1. 11 %, n=6）, 100.63%（RSD=1.90%, n=6）, 99.32%（RSD=1.44%, n=6） and 99.65 % （RSD = 1.53 % , n = 6） respectively. Conclusion This method is accurate, reliable and with good repro- ducibility. It can he used for the quality control of Zhizhu Pills.
出处
《中药新药与临床药理》
CAS
CSCD
2006年第5期351-354,共4页
Traditional Chinese Drug Research and Clinical Pharmacology
基金
科技部基础性工作专项"中药材标准及中医临床疗效评价标准"(编号:2001DEA20010)
