摘要
目的建立桂附地黄丸中马钱苷、芍药苷、丹皮酚和没食子酸含量同时测定的高效液相色谱法。方法采用Phenmenex Synergri FusionRP80A色谱柱(250nm×4.6nm,4μm);流动相为乙腈-0.05%磷酸溶液,梯度洗脱,体积流量为1mL·min-1,检测波长为234nm和274nm,柱温为30℃。结果马钱苷、芍药苷、丹皮酚和没食子酸的线性范围分别为5.3408~48.0672μg·mL-1(r=0.9999),4.8256~43.4303μg·mL-1(r=0.9996),10.8134~97.3206μg·mL-1(r=0.9999),4.1240~37.116μg·mL-1(r=0.9999)。平均加样回收率分别为马钱苷100.7%,RSD=0.85%(n=6);芍药苷101.1%,RSD=I.98%(n=6);丹皮酚98.9%,RSD=0.55%(n=6);没食子酸99.8%,RSD=1.25%(n=6)。结论该方法操作简便、准确,重复性好,可用于桂附地黄丸的质量控制。
Objective To develop a simple high performance liquid chromatography (HPLC) method for the determination of loganin, paeoniflorin, paeonol and gallic acid in Guifu Dihuang pills. Methods The HPLC method was validated on Phenmenex SynergTi Fusion-RP column (250 nm × 4.6 nm, 4μm) with a mobile phase of acetonitrile -0.05 % phosphoric acid at a flow rate of 1 mL/min and a column temperature of 30 ℃. The detection wavelengths were set at 234 nm and 274 nm. Results The calibration curve of the loganin, paeoniflorin, paeonol and gallic acid showed good linearity relationship in the range of 5.3408- 48.0672 μg·mL-1 (r=0. 9999), 4.8256 - 43.4303 p,g'mL-1 ( r=0.9996 ), 10.8134 - 97.3206 μg·mL-1 ( r=0.9999 ), 4.1240-37.1160 μg·mL-1 (r=0.9999), respectively. The average recovery was 100.7 % for loganin, 101.1% for paeoniflorin, 98.9 % for paeonol and 99.8 % for gallic acid, and the standard deviations were 0.85 %, 1.98 %, 0.55 % and 1.25 %, respectively(n=6). Conclusion The developed method is simple and rapid with excellent specificity, accuracy and precision, which can be used for the quality control of Guifu Dihuang Pills.
出处
《中药新药与临床药理》
CAS
CSCD
北大核心
2014年第2期201-204,共4页
Traditional Chinese Drug Research and Clinical Pharmacology
基金
广东省211工程三期重点学科建设项目[粤发改社(2009)972号]
广东省自然科学基金(9451040701002867)