中成药复方金银花颗粒中黄芩成分的HPLC法测定

Determination of Radix Scutellariae Composition in the Proprietary Chinese Medicine Compound Jinyinhua Granules by HPLC Method

目的:建立高效液相色谱法测定复方金银花颗粒中黄芩苷、黄芩素和汉黄芩素的含量。方法:采用ZORBAX SB-C18色谱柱,流动相为乙腈(A)-0.2%冰醋酸(B)采用梯度洗脱(0~10 min,A 25%;10~20 min,A 25%~40%;20~35 min,A 40%~50%);检测波长:275 nm;流速:1.0 mL·min^(-1)。结果:黄芩苷在4.1~204.5μg·mL^(-1)质量浓度范围内线性关系良好(r=0.9999),平均回收率为99.4%,RSD=0.7%;黄芩素在1.05~52.5μg·mL^(-1)质量浓度范围内线性关系良好(r=0.9999),平均回收率为98.2%,RSD=1.3%;汉黄芩素在0.98~48.8μg·mL^(-1)质量浓度范围内线性关系良好(r=0.9999),平均回收率为98.6%,RSD=0.9%。3批样品检测结果黄芩苷含量为4.08~4.23 mg·mL^(-1)、黄芩素为0.28~0.30mg·mL、汉黄芩素0.14~0.15 mg·mL^(-1)。结论:本法经方法学验证可用于中成药复方金银花颗粒的质量检测。

Objective：To establish a HPLC method for determination of baicalin, baicalein and wogonin in Compound Jinyinhua Granules. Methods：A stable HPLC method was established and the chromatography was accomplished on a ZORBAX SB-C18 column with the mobile phase consisting of acetonitrile （A）-0.2%acetic acid （B） in a gradient mode （0-10 min, A 25%;10-20 min, A 25%-40%;20-35 min, A 40%-50%）;the detection wavelength was 275 nm, and the lfow rate was 1.0 mL＆#183;min-1. Results：The calibration curve of baicalin was linear in the mass concentration range of 4.1-204.5μg＆#183;mL-1 （r=0.9999）, and the average recovery was 99.4%with the corresponding RSD of 1.1%;the calibration curve of baicalein was linear in the mass concentration range of 1.05-52.5μg＆#183;mL-1 （r=0.9999）, and the average recovery was 98.2%with the corresponding RSD of 1.3%;The calibration curve of wogonin was linear in the mass concentration range of 0.98-48.8μg＆#183;mL-1 （r=0.9999）, and the average recovery was 98.6% with the corresponding RSD of 0.9%. Test results for these batches of samples showed that, the content was 4.08-4.23 mg＆#183;g-1 for baicalin, 0.28-0.30 mg＆#183;g-1 for baicalein, and 0.14-0.15 mg＆#183;g-1 for wogonin. Conclusion： In accordance with the requirements of methodology validation, the method can be used for the quality test of Compound Jinyinhua Granules.