HPLC法同时测定凉膈胶囊中4种成分的含量

Simultaneous determinations of 4 constituents in Liangge capsules by HPLC

目的建立同时测定凉膈胶囊中栀子苷、黄芩苷、连翘苷和甘草酸质量分数的高效液相色谱方法。方法采用Kromasil-C18色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈(A)-0.3%(体积分数)H3PO4(B),梯度洗脱:0~12 min,14%A;12~15 min,14%A^20%A;15~35 min,20%A^30%A;35~45 min,30%A^43%A;45~50 min,43%A^43%A;50~55 min,43%A^100%A,55~60 min,100%A,流速为1.0 m L/min,柱温为30℃,检测波长为238 nm。结果栀子苷、黄芩苷、连翘苷、甘草酸4种成分的分离度良好,线性范围分别为0.269 6~2.696μg(r=0.999 6)、0.670 4~6.704μg(r=0.999 6)、0.065 6~0.656μg(r=0.999 6)、0.100 8~1.008μg(r=0.999 9),平均加样回收率(n=6)分别为103.2%(RSD=1.59%)、100.7%(RSD=1.15%)、98.36%(RSD=2.34%)、97.37%(RSD=1.54%)。结论本方法简单、准确、重复性好,可用于同时测定凉膈胶囊中栀子苷、黄芩苷、连翘苷、甘草酸的质量分数。

Objective To develop an HPLC method for the simultaneous determination of gardenoside,baicalin,forsythin and glycyrrhizic acid in Liangge capsules. Methods The sample was separated on a Kromasil C18column（ 4.6 mm× 250 mm,5 μm） with a mobile phase consisting of acetonitrile（ A）- 0.3%phosphoric acid（ B） in the gradient elution as follows： 0- 12 min,14%A; 12- 15 min,14%A- 20%A; 15- 35 min,20%A-30%A; 35- 45 min,30% A- 43% A; 45- 50 min,43% A- 43% A; 50- 55 min,43% A-100%A; 55- 60 min,100%A,at the flow rate of 1.0 m L/min. The column temperature was 30 ℃ and the detection wavelength was 238 nm. Results The calibration curves were linear within the range of 0.269 6-2.696 μg（ r = 0.999 6） for gardenoside,0.670 4- 6.704 μg（ r = 0.999 6） for baicalin,0.065 6- 0.656 μg（ r= 0.999 6） for forsythin,and 0.100 8-1.008 μg（ r = 0.999 9） for glycyrrhizic acid,respectively. The recoveries（ n = 6） of gardenoside,baicalin,forsythin and glycyrrhizic acid were 103.2%（ RSD = 1.59%）,100. 7%（ RSD = 1. 15%）,98. 36%（ RSD = 2. 34%）,and 97. 37%（ RSD = 1. 54%）,respectively.Conclusion The method is simple,accurate,and reproducible for simultaneous determination of gardenoside,baicalin,forsythin and glycyrrhizic acid in Liangge capsules.