CAJ | 학술논문

用超高效合相色谱法( Ultra performance convergence chromatography,UPC2)建立补肾健脑颗粒及各药材提取物的指纹图谱,对补肾健脑颗粒主要色谱峰进行归属分析,并测定有效成分β-蜕皮甾酮和松果菊苷的含量。样品经乙醇提取后,进样1μL,用Waters ACQUITY UPC2TM BEH柱(100 mm×3.0 mm,1.7μm)分离,柱温为40℃,以超临界CO2-0.05% H3 PO4-甲醇溶液为流动相,梯度洗脱,流速为0.8 mL/min。分析补肾健脑颗粒和各药材提取物的UPC2指纹图谱,利用各峰相对保留时间、紫外光谱图及部分对照品归属主峰。结果表明,补肾健脑颗粒UPC2指纹图谱中15个主峰来源明确,其中12号峰为β-蜕皮甾酮,含量为380μg/g,15号峰为松果菊苷,含量为9.562 mg/g。与HPLC和UPLC法相比,本方法简便、快速,精密度高,重现性好。
용초고효합상색보법( Ultra performance convergence chromatography,UPC2)건립보신건뇌과립급각약재제취물적지문도보,대보신건뇌과립주요색보봉진행귀속분석,병측정유효성분β-세피치동화송과국감적함량。양품경을순제취후,진양1μL,용Waters ACQUITY UPC2TM BEH주(100 mm×3.0 mm,1.7μm)분리,주온위40℃,이초림계CO2-0.05% H3 PO4-갑순용액위류동상,제도세탈,류속위0.8 mL/min。분석보신건뇌과립화각약재제취물적UPC2지문도보,이용각봉상대보류시간、자외광보도급부분대조품귀속주봉。결과표명,보신건뇌과립UPC2지문도보중15개주봉래원명학,기중12호봉위β-세피치동,함량위380μg/g,15호봉위송과국감,함량위9.562 mg/g。여HPLC화UPLC법상비,본방법간편、쾌속,정밀도고,중현성호。
An ultra performance convergence chromatographic ( UPC2 ) method was established for the attribution analysis of the main peaks as well as the quantitative determination of echinacoside andβ-ecdyserone in Bushen Jiannao Grains. The samples were extracted with ethanol and separated on Waters ACQUITY UPC2TM BEH column (100 mm × 3. 00 mm, 1. 7 μm), with a gradient supercritical CO2-0. 05%phosphoric acid-methanol solvent system at 40 ℃. The flow rate was 0. 8 mL/min, the detection wavelength was set at 248 nm and the injection volume was 1 μL. Results showed that all the main peaks in the fingerprint were clearly attributed. The peak named 12 wasβ-ecdyserone with the content of 380μg/g and the peak named 15 was echinacoside with the content of 9. 562 mg/g. The method was simple, eco-friendly, accurate and reliable compared with HPLC and UPLC.