世界科学技术-中医药现代化
世界科學技術-中醫藥現代化
세계과학기술-중의약현대화
WORLD SCIENCE AND TECHNOLOGY-MODERNIZATION OF TRADITIONAL CHINESE MEDICINE
2013年
8期
1837-1842
,共6页
毋桂花%李莉%王颖莉%张梦萱%张伟
毌桂花%李莉%王穎莉%張夢萱%張偉
무계화%리리%왕영리%장몽훤%장위
鼻敏康%提取工艺%正交试验%黄芪甲苷%HPLC-ELSD
鼻敏康%提取工藝%正交試驗%黃芪甲苷%HPLC-ELSD
비민강%제취공예%정교시험%황기갑감%HPLC-ELSD
Bimink ang%extraction technology%orthogonal experiment%Astragaloside Ⅳ%HPLC-ELSD
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。
目的：優選中藥複方“鼻敏康”的最佳提取工藝併建立黃芪甲苷的HPLC-ELSD含量測定方法。方法：採用加熱迴流法，乙醇為提取溶劑，以浸膏率及黃芪甲苷含量為指標，對乙醇濃度、提取時間、液料比和提取次數進行單因素攷查，優選齣對浸膏率及黃芪甲苷含量較大影響的3箇因素，按照L9（34）安排正交試驗優選複方製劑鼻敏康的提取工藝。黃芪甲苷含量測定採用Diamonstil C18（250 mm×4.6 mm，5μm）色譜柱，流動相為水（A）-乙腈（B）,洗脫梯度：0~45 min，22%B；45~60 min，22%~32%B，流速1.0 mL·min-1，漂移管溫度100℃，載氣為N2，載氣流速2.5 L·min-1，柱溫：30℃。結果：複方製劑鼻敏康最佳提取工藝為8倍量70%乙醇,每次1.5 h，提取3次，結果錶明乙醇濃度和提取次數存在顯著性影響，最終確定提取工藝為8倍量70%乙醇,每次加熱迴流1.5 h，提取2次；黃芪甲苷含量測定線性範圍為0.87~8.72μg，迴歸方程 Y=1.5454X+5.8759，r =0.9997，平均收率95.05%，RSD值為2.64%。結論：優選的提取工藝穩定閤理可行，適用于工業生產。
목적：우선중약복방“비민강”적최가제취공예병건립황기갑감적HPLC-ELSD함량측정방법。방법：채용가열회류법，을순위제취용제，이침고솔급황기갑감함량위지표，대을순농도、제취시간、액료비화제취차수진행단인소고사，우선출대침고솔급황기갑감함량교대영향적3개인소，안조L9（34）안배정교시험우선복방제제비민강적제취공예。황기갑감함량측정채용Diamonstil C18（250 mm×4.6 mm，5μm）색보주，류동상위수（A）-을정（B）,세탈제도：0~45 min，22%B；45~60 min，22%~32%B，류속1.0 mL·min-1，표이관온도100℃，재기위N2，재기류속2.5 L·min-1，주온：30℃。결과：복방제제비민강최가제취공예위8배량70%을순,매차1.5 h，제취3차，결과표명을순농도화제취차수존재현저성영향，최종학정제취공예위8배량70%을순,매차가열회류1.5 h，제취2차；황기갑감함량측정선성범위위0.87~8.72μg，회귀방정 Y=1.5454X+5.8759，r =0.9997，평균수솔95.05%，RSD치위2.64%。결론：우선적제취공예은정합리가행，괄용우공업생산。
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.
