RP-HPLC-ECD测定通脉颗粒中3种化合物

RP-HPLC-ECD determination of 3 compounds in Tongmai granules

目的:建立测定通脉颗粒中原儿茶醛、阿魏酸和黄芩苷的 RP-HPLC-ECD 分析方法。方法:采用 RP-HPLC-ECD 检测法,以 Zorbax SB—C_(18)(150 mm×4.6 mm,5.0 μm)为色谱柱,甲醇(A)、2%醋酸(B)为流动相,梯度洗脱,流速为1.0 mL·min^(-1);电化学检测器的工作电位为0.9 V;柱温为30℃。结果:原儿茶醛、阿魏酸和黄芩苷的线性范围分别为0.138～12.4μg·mL^(-1)(r=0.9999),0.130～11.7μg·mL^(-1)(r=0.9992)和0.192～240μg·mL^(-1)(r=0.9998);平均加样回收率(n=6)分别为97.4%(RSD=0.8%),98.7%(RSD=2.3%)和97.9%(RSD=2.9%)。结论:该法快速、灵敏、准确,可为通脉颗粒的质量控制提供科学依据。

Objectlve：To establish a reversed phase high performance liquid chromatography electrochemical detection （RP-HPLC -ECD） method for determination of protocatechuic aldehyde,ferulic acid and baicalin in Tongmai granules. Method：RP-HPLC- ECD was used. The separation was performed on Zorbax SB -C18 （150 mm ×4. 6 mm,5.0 μm） column by gradient elution with methanol and 2% acetic acid as mobile phase at a flow rate of 1.0 mL. min ^- 1. The detection was done at 0. 9 V, and column temperature is 30 ℃. Results： The linear ranges were 0. 138 - 12.4 μg. mL^-1 （r =0. 9999） for protocatechuic aldehyde,0. 130 - 11.7 μg . mL^-1 （r =0. 9992） for ferulic acid and 0. 192 - 240 μg . mL^- 1 （ r = 0. 9998 ） for baicalin respectively. The recoveries （ n = 6 ） were 97.4% （ RSD = 0. 8% ）, 98.7% （ RSD = 2. 3% ） and 97.9% （ RSD = 2. 9% ）, respectively. Conclusion： The method is rapid, sensitive and accurate. It may provide a scientific basis for quality control of Tongmai granules.