UPLC法测定宣木瓜中齐墩果酸、熊果酸
Detecting Oleanolic and Ursolic Acid with UPLC in Chaenomelis Fructus from Xuancheng
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摘要: 目的 对高效液相色谱法(HPLC)进行转换并优化,建立超高效液相色谱法(UPLC)测定宣木瓜中齐墩果酸(OA)和熊果酸(UA)含量,并与HPLC测定法相比较。方法 UPLC采用ACQUITY UPLCTM BEH C18色谱柱(100 mm×2.1 mm, 1.7 μm),流动相:甲醇-水-冰乙酸-三乙胺(254∶46∶0.1∶0.05);流速:0.3 mL/min,检测波长:210 nm,柱温:25 ℃,进样体积:1 μL;HPLC色谱柱为Shim-pack CLC-ODS(M) (250 mm×4.6 mm,5 μm),流动相:甲醇-水-冰乙酸-三乙胺(265∶35∶0.10∶0.05);流速:0.6 mL/min;柱温及检测波长同UPLC;进样体积:20 μL。结果 2种方法测定不同采收期宣木瓜中OA和UA含量,结果基本一致;UPLC法分析时间短,溶剂消耗少,检测灵敏度高。结论 UPLC法可替代HPLC法测定宣木瓜药材中OA和UA含量。Abstract: OBJECTIVE To transform and develop high performance liquid chromatograph(HPLC), to establish ultra performance liquid chromatography (UPLC) for determinating the contents of oleanolicacid (OA) and ursolicacid (UA) in Chaenomelis Fructus and to compare UPLC with HPLC.METHODS In the UPLC, ACQUITY UPLC TM BEHC18 column(100 mm×2.1 mm, 1.7 μm) was adopted, and the column temperature was 25℃.The mobile phase consisted of methanol-water-glacial acetic acid-triethylamine (254∶46∶0.1∶0.05) with a flow rate of 0.3mL/min.The detection wave length was 210nm, and injection volume was 1 μL in UPLC system. A Shim-pack CLC-ODS(M) column (250mm×4.6mm,5μm) was utilized in HPLC system, and a mixture of methanol-water-glacial acetic acid-triethylamine (265∶35∶0.1∶0.05) was regarded as mobile phase with a flow rate of 0.6mL/min.The Injection volume of HPLC was 20μL.RESULTS The content of oleanolicacid (OA) and ursolicacid (UA) in Chaenomelis Fructus of different picking time detected by HPLC was almost as same as that by UPLC. Compared with HPLC, UPLC provided shorter analysis time, cost less solvent consumption with better sensitivity.CONCLUSION UPLC may replace HPLC for the determination of OA and UA in Chaenomelis Fructus.