[關(guān)鍵詞]
[摘要]
目的 建立HPLC法同時(shí)測定參烏益腎片中β-蛻皮甾酮、25R-牛膝甾酮、25S-牛膝甾酮、大車前苷、毛蕊花糖苷、異毛蕊花糖苷、木通苯乙醇苷B和2,3,5,4′-四羥基二苯乙烯-2-O-β-D-葡萄糖苷8種成分,聯(lián)合化學(xué)計(jì)量學(xué)方法對參烏益腎片的產(chǎn)品質(zhì)量進(jìn)行綜合評價(jià)。方法 采用Sepax Bio-C18色譜柱(250 mm×4.6 mm,5 μm);以乙腈–0.1%甲酸進(jìn)行梯度洗脫;檢測波長分別為250 nm(0~20 min測定β-蛻皮甾酮、25R-牛膝甾酮和25S-牛膝甾酮)、330 nm(20~60 min測定大車前苷、毛蕊花糖苷、異毛蕊花糖苷、木通苯乙醇苷B和2,3,5,4′-四羥基二苯乙烯-2-O-β-D-葡萄糖苷);柱溫30℃;體積流量1.0 mL/min;進(jìn)樣量10 μL。采用聚類分析、主成分分析和偏最小二乘法–判別分析法對8種指標(biāo)成分檢測結(jié)果相關(guān)性進(jìn)行分析評價(jià)。結(jié)果 β-蛻皮甾酮、25R-牛膝甾酮、25S-牛膝甾酮、大車前苷、毛蕊花糖苷、異毛蕊花糖苷、木通苯乙醇苷B和2,3,5,4′-四羥基二苯乙烯-2-O-β-D-葡萄糖苷分別在1.47~36.75、0.66~16.50、0.74~18.50、5.80~145.00、15.77~394.25、4.58~114.50、1.29~32.25、8.78~219.50 μg/mL有良好的線性關(guān)系;平均回收率分別為97.78%、96.90%、97.96%、99.67%、100.01%、99.54%、98.03%、100.11%,RSD值分別為1.17%、0.82%、1.48%、0.93%、0.77%、0.69%、1.13%、0.65%。成分8(2,3,5,4′-四羥基二苯乙烯-2-O-β-D-葡萄糖苷VIP=1.503)、成分4(大車前苷AVIP=1.404)、成分5(毛蕊花糖苷VIP=1.274)、成分1(β-蛻皮甾酮VIP=1.030)是影響參烏益腎片樣品質(zhì)量的關(guān)鍵成分。結(jié)論 建立的方法簡便快捷、準(zhǔn)確可靠,可用于參烏益腎片中多指標(biāo)成分的質(zhì)量綜合評價(jià)模式。
[Key word]
[Abstract]
Objective To establish an HPLC method for simultaneous determination of β-ecdysterone, 25R-inokosterone, 25S- inokosterone, plantamajoside, verbascoside, isoacteoside, calceolarioside B, and 2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside, and to evaluate the comprehensive quality of Shenwu Yishen Tablets by chemometrics analysis. Methods The separation was carried out on Sepax Bio-C18 column (250 mm×4.6 mm, 5 μm). The mobile phase consisted of acetonitrile - 0.1% formic acid with gradient elution. The detection wavelengths were set at 250 nm for β-ecdysterone, 25R-inokosterone, and 25S-inokosterone, and 330 nm for plantamajoside, verbascoside, isoacteoside, calceolarioside B, and 2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside. Temperature of column was set at 30 ℃, the flow rate was 1.0 mL/min, and the volume of injection was 10 μL. The chemometrics method was used to analyze and evaluate the correlation of the detection results of eight index components. Results There were good linear relationships of β-ecdysterone, 25R-inokosterone, 25S-inokosterone, plantamajoside, verbascoside, isoacteoside, calceolarioside B, and 2,3,5,4'- tetrahydroxystilbene-2-O-β-D-glucoside within the ranges of 1.47 — 36.75, 0.66 — 16.50, 0.74 — 18.50, 5.80 — 145.00, 15.77 — 394.25, 4.58 — 114.50, 1.29 — 32.25, and 8.78 — 219.50 μg/mL, whose average recoveries and RSD were 97.78% (1.17%), 96.90% (0.82%), 97.96% (1.48%), 99.67% (0.93%), 100.01% (0.77%), 99.54% (0.69%), 98.03% (1.13%), and 100.11% (0.65%), respectively. Through chemometrics analysis, 2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside(VIP = 1.503), plantamajoside (VIP = 1.404), verbascoside (VIP = 1.274), and β-ecdysterone (VIP = 1.030) were the differential markers affecting the quality of Shenwuyishen Tablets. Conclusion The method is simple and accurate, which can be used for quality evaluation of multiple index components in Shenwu Yishen Tablets.
[中圖分類號(hào)]
R286.02
[基金項(xiàng)目]
北京市中醫(yī)管理局第二批中藥骨干人才培養(yǎng)項(xiàng)目(京中醫(yī)科字[2018]213號(hào))