RP-HPLC法同时测定半夏药材中4种有机酸的含量  

Simultaneous determination of four organic acids in Pinelliae Rhizoma by RP-HPLC

作　　者：孙全[1] 张景勍[1] 傅亚[2] 秦少容[3] 何丹[1] 

机构地区：[1]重庆医科大学药学院,重庆400016 [2]重庆科技学院化学化工学院,重庆401331 [3]太极集团重庆涪陵制药厂有限公司,重庆408000

出　　处：《药物分析杂志》2015年第6期1062-1066,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：国家科技支撑计划(2011BAI13B03)

摘　　要：目的：采用RP-HPLC法同时测定半夏药材中草酸（oxalic acid,OA）、柠檬酸（citric acid,CA）、苹果酸（malic acid,MA）、琥珀酸（succinic acid,SA）的含量。方法：采用Gemini-C18（4.6 mm×250 mm,5μm）色谱柱,以0.03 mol·L-1磷酸二氢铵缓冲液（以磷酸调节p H=2.0）-甲醇（97∶3）为流动相,流速0.8 m L·min-1,柱温30℃,检测波长210 nm。结果：草酸、柠檬酸、苹果酸和琥珀酸的线性方程分别为Y=1.194×104X＋1.938×103（r=0.999 5）,Y=291X＋263（r=0.999 6）,Y=7.446×103X＋260（r=0.999 9）,Y=2.332×103X-1.727×103（r=0.999 6）,它们的质量浓度分别在2.28-36.48、12.32-197.1、2.62-41.86、12.56-201.0μg·m L-1范围内线性关系良好,低、中、高浓度平均加样回收率（n=9）在96.9%与98.0%之间。10个不同产地半夏4种有机酸的总含量在0.295%-2.086%之间。结论：10个不同产地半夏4种有机酸总含量以四川西昌最高,四川遂宁最低,该方法经方法学验证,可为半夏药材的质量控制提供参考。Objective：To establish a RP-HPLC method for simultaneous determination of oxalic acid,citric acid,malic acid and succinic acid in Pinelliae Rhizoma.Methods：The separation was performed on a Gemini-C18 analytical column（4.6 mm × 250 mm,5 μm） with 0.03 mol·L-1ammonium dihydrogen phosphate buffer solution（adjusted p H to 2.0 with phosphoric acid）-methanol（97∶ 3） as the mobile phase at a flow rate of 0.8 m L·min-1.The detection wavelength was 210 nm and the column temperature was 30 ℃.Results：The regression equations of oxalic acid,citric acid,malic acid and succinic acid were as follows：Y = 1.194 × 104 X ＋ 1.938 × 103（r = 0.9995）,Y = 291 X ＋ 263（r = 0.999 6）,Y = 7.446 × 103 X ＋ 260（r = 0.999 9）,Y = 2.332 × 103X-1.727 × 103（r =0.999 6）.Linear ranges of oxalic acid,citric acid,malic acid and succinic acid were 2.28-36.48 μg·m L-1,12.32-197.1 μg·m L-1,2.62-41.86 μg·m L-1,12.56-201.0 μg·m L-1,respectively.Their average recoveries（n = 9） at low,medium and high concentrations fell between 96.9% and 98.0%,the total content of the four organic acids from 10 different origins ranged from 0.295% to 2.086%.Conclusion：The total content of the four organic acids in samples from Xichang district,Sichuan province was the highest and that from Suining district,Sichuan province was the lowest.By the methodology validation,the RP-HPLC method was proved to be applicable as a standard for the quality control of Pinelliae Rhizoma.

关 键 词：半夏 草酸 柠檬酸 苹果酸 琥珀酸 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]