目的:优选中药复方“鼻敏康”的最佳提取工艺并建立黄芪甲苷的HPLC-ELSD含量测定方法。方法:采用加热回流法,乙醇为提取溶剂,以浸膏率及黄芪甲苷含量为指标,对乙醇浓度、提取时间、液料比和提取次数进行单因素考查,优选出对浸膏率及黄芪甲苷含量较大影响的3个因素,按照L9(34)安排正交试验优选复方制剂鼻敏康的提取工艺。黄芪甲苷含量测定采用Diamonstil C18(250 mm×4.6 mm,5μm)色谱柱,流动相为水(A)-乙腈(B),洗脱梯度:0-45 min,22%B;45-60 min,22%-32%B,流速1.0 mL·min-1,漂移管温度100℃,载气为N2,载气流速2.5 L·min-1,柱温:30℃。结果:复方制剂鼻敏康最佳提取工艺为8倍量70%乙醇,每次1.5 h,提取3次,结果表明乙醇浓度和提取次数存在显著性影响,最终确定提取工艺为8倍量70%乙醇,每次加热回流1.5 h,提取2次;黄芪甲苷含量测定线性范围为0.87-8.72μg,回归方程 Y=1.5454X+5.8759,r =0.9997,平均收率95.05%,RSD值为2.64%。结论:优选的提取工艺稳定合理可行,适用于工业生产。
This study was aimed to optimize the best extraction technology of traditional Chinese medicine (TCM) Biminkang and establish the HPLC-ELSD method for determination of Astragaloside Ⅳ content. This test used heat-ing reflux which preferred ethanol as solvent extraction, extraction rate as an index to extract. By the single factor ex-periment, three factors which affect extraction rate greater were selected from the solvent concentration, extraction time, liquid ratio and extraction times. And then L9(34) orthogonal test was used to design the extraction technology of compound preparation Biminkang. HPLC-ELSD was performed on Diamonsil C18 column (250 mm í 4.6 mm, 5 μm) with H2O(A)-acetonitrile(B) (0-45 min: 22%B, 45-60 min: 22%-32%B) as mobile phase, flow rate was at 1.0 mL·min-1. The temperature of drift tube was 100℃ and the flow rate of N2 was 2.5 L·min-1. The column temperature was 30℃. The results showed that the best extraction technology of compound preparation Biminkang was liquid-solid ra-tio of 8 mL·g-1, ethanol concentration of 70%, 1.5 h for each extraction time, and extracted for three times. The re-sults showed that the presence of ethanol concentration and extraction times affected significantly. The ultimately de-termined optimal extraction conditions were as follows. The liquid-solid ratio of 8 mL/g, ethanol concentration of 70%, 1.5 h for each extraction time, and extracted for two times. The linear range of Astragaloside Ⅳ content was from 0.87 μg to 8.72 μg. And the regression equation was Y = 1.545 4X + 5.875 9, r = 0.999 7. The average re-covery rate was 95.05%. The RSD was 2.64%. It was concluded that the optimized extraction technology was stable, reasonably practicable, and suitable for industrial production.