手性流动相高效液相色谱法测定木瓜中齐墩果酸和熊果酸含量  

Content Determination of Oleanolic Acid and Ursolic Acid in Chaenomelis Fructus by HPLC with Chiral Mobile Phase

作　　者：耿仲乐 王静 张峰 GENG Zhongle;WANG Jing;ZHANG Feng(Luohe Drug Testing and Inspection Center,Luohe,Henan,China 462000)

机构地区：[1]河南省漯河市药品检测检验中心,河南漯河462000

出　　处：《中国药业》2024年第13期93-95,共3页China Pharmaceuticals

摘　　要：目的建立同时测定木瓜中齐墩果酸和熊果酸含量的手性流动相高效液相色谱法。方法色谱柱为Shimpack GIST C_(18)柱(250 mm×4.6 mm,5µm),流动相为乙腈-甲醇-含12 mmol/L羟丙基-β-环糊精的0.5%醋酸铵溶液(64∶12∶21,V/V/V),流速为1.0 mL/min,检测波长为210 nm,柱温为18℃,进样量为20µL。结果齐墩果酸和熊果酸的分离度大于1.5;质量浓度分别在0.009~0.182µg/mL、0.016~0.325µg/mL范围内与峰面积积分值线性关系良好(r=0.9998,0.9999,n=6);检测限分别为0.86,0.58µg/mL,定量限分别为2.75,1.86µg/mL;精密度、稳定性、重复性试验结果的RSD均小于2.0%(n=6);加样回收率分别为99.74%,99.22%,RSD分别为1.00%,0.93%(n=6)。3批样品中齐墩果酸和熊果酸的总含量为2.305%~2.357%。结论该改进方法操作简便、结果准确、重复性好,可有效分离并测定木瓜中齐墩果酸和熊果酸的含量,可用于木瓜药材的质量控制。Objective To establish a high-performance liquid chromatography(HPLC)method with chiral mobile phase for simultaneous determination of oleanolic acid and ursolic acid in Chaenomelis Fructus.Methods The chromatographic column was Shimpack GIST C_(18) column(250 mm×4.6 mm,5µm),and the mobile phase was acetonitrile-methanol-0.5%cyclodextrin ammonium acetate solution containing 12 mmol/L hydroxypropyl group-β-cyclodextrin(64∶12∶21,V/V/V),the flow rate was 1.0 mL/min,the detection wavelength was 210 nm,the column temperature was 18℃,and the injection volume was 20µL.Results The separation degree of oleanolic acid and ursolic acid was higher than 1.5,the linear ranges of oleanolic acid and ursolic acid were 0.009-0.182µg/mL and 0.016-0.325µg/mL(r=0.9998,0.9999,n=6),respectively.The limits of detection were 0.86 and 0.58µg/mL,respectively.The limits of quantification were 2.75 and 1.86µg/mL,respectively.The RSDs of precision,stability,and repeatability test results were all lower than 2.0%(n=6).The recoveries of oleanolic acid and ursolic acid were 99.74%and 99.22%,with RSDs of 1.00%and 0.93%(n=6),respectively.The total content of oleanolic acid and ursolic acid in three batches of samples was in the range of 2.305%-2.357%.Conclusion The improved method is simple,accurate,and has good repeatability,it can effectively separate and determine the content of oleanolic acid and ursolic acid in Chaenomelis Fructus,which can be used for the quality control of Chaenomelis Fructus.

关 键 词：木瓜 高效液相色谱法 手性流动相 齐墩果酸 熊果酸 含量测定 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学] R286.0