18色譜柱(250 mm×4.6 mm,5 μm),流動(dòng)相為乙腈(A)-0.2%甲酸溶液(B)梯度洗脫(0~20 min,20%~40% A;20~30 min,40% A;30~35 min,90% A;35~40 min,20% A),體積流量1.0 mL/min,柱溫30℃,檢測(cè)波長(zhǎng)260 nm。結(jié)果 毛蕊異黃酮葡萄糖苷、大黃素和大黃素甲醚分離度較好,且在各自濃度范圍內(nèi)呈現(xiàn)出良好的線性關(guān)系,r=0.999 2;精密度可靠(RSD為0.63%~0.74%);樣品在12 h內(nèi)穩(wěn)定;方法重復(fù)性良好(RSD為1.39%~2.00%);3種成分的平均加樣回收率分別為100.3%、100.5%、103.2%,RSD均小于2.0%。采用HPLC可準(zhǔn)確有效測(cè)出益腎排毒丸中有效成分的含量。指紋圖譜研究得共有峰32個(gè),指認(rèn)了其中6個(gè)成分,益腎排毒丸各批次間一致性較好,質(zhì)量相對(duì)穩(wěn)定。結(jié)論 該方法簡(jiǎn)便易行、穩(wěn)定可靠,可更好用于益腎排毒丸的質(zhì)量控制。;Objective To establish an RP-HPLC method for simultaneous determination of the contents of three ingredients (calycosin glycoside,emodin,physcion) and fingureprint in Yishen Paidu Pills.Methods The analysis was performed on Agilent TCC18 column (250 mm×4.6 mm,5 μm) with the mobile phase of acetonitrile (A) and 0.2% formic acid (B) in a liner gradient mode as follows:0-20 min,20%-40% A;20-30min,40% A;30-35 min,90% A;35-40 min,20% A.The flow rate was 1.0 mL/min.The column temperature was 30℃ and the detective wavelength was at 260 nm.Results The standard curves of three ingredients showed good linearity in their concentration ranges with r=0.999 2.Precision was reliable (RSD in 0.63%-0.74%).Samples were stable in 12 h and the repeatability of method was excellent (RSD in 1.39%-2.0%).The average recovery of the three ingredients were 100.3%,100.5% and 103.2%,respectively with RSD less than 2.0%.The contents of three ingredients in Yishen Paidu Wan can be determined accurately and effectively by HPLC.Fingerprints study of Yishen Paidu Pills indicated that they have good consistency among different batches and the quality were relatively stable.Conclusion The method is rapid,simple and accurate,and can be better applied for the quality control of Yishen Paidu Pills."/>

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首頁 > 過刊瀏覽>2019年第42卷第4期 >2019,42(4):658-662. DOI:10.7501/j.issn.1674-6376.2019.04.010
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益腎排毒丸中有效成分含量測(cè)定及指紋圖譜研究

Study on determination of active components content and fingerprint of Yishen Paidu Pills

發(fā)布日期:2019-04-12
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