HPLC波长切换法测定麦味地黄胶囊中5种有效成分的含量

Simultaneous determination of five constituents in Maiwei Dihuang capsules by HPLC with wavelength switching

目的:建立HPLC波长切换法同时测定麦味地黄胶囊中5-羟甲基糠醛、莫诺苷、马钱苷、丹皮酚、五味子醇甲5种化学成分的含量。方法:采用Agela Venusil MP C_(18)(2)(4.6 mm×250 mm,5μm)色谱柱,以乙腈(A)-0.2%磷酸溶液(B)为流动相,梯度洗脱(0~15 min,3%A;15~40 min,3%A→10%A;40~50 min,10%A→15%A;50~70 min,15%A→40%A;70~90 min,40%A),流速1.0 mL·min^(-1),柱温40℃,波长切换(0~30 min,在284 nm波长下检测5-羟甲基糠醛;30~70 min,在240 nm波长下检测莫诺苷和马钱苷;70~80 min,在274 nm波长下检测丹皮酚;80~90 min,在216 nm波长下检测五味子醇甲)。结果:5-羟甲基糠醛、莫诺苷、马钱苷、丹皮酚、五味子醇甲的线性范围分别为0.08~2.26μg(r=0.999 9)、0.02~0.63μg(r=0.999 9)、0.02~0.62μg(r=1.000)、0.05~1.49μg(r=1.000)、0.008~0.24μg(r=0.999 9),平均回收率(n=6)分别为96.8%(RSD=0.65%)、96.3%(RSD=0.61%)、97.7%(RSD=0.32%)、97.7%(RSD=1.4%)、100.6%(RSD=1.9%)。10批样品的含量测定结果分别为5-羟甲基糠醛3.194~10.27 mg·g^(-1),莫诺苷0.473 2~0.800 4 mg·g^(-1),马钱苷0.736 0~1.226 mg·g^(-1),丹皮酚1.562~2.499 mg·g^(-1),五味子醇甲0.035 22~0.143 7 mg·g^(-1)。结论:该方法合理可行,重复性好,可用于麦味地黄胶囊的质量控制。

Objective： To develop simultaneous determination method of 5-hydroxymethyl-2 furaldehyde, morroniside, loganin, paeonol and schisandrin in Maiwei Dihuang capsules by HPLC combined with wavelength switching technology. Methods： The Agela Venusil MP C18 （ 2 ）column （ 4.6 mm × 250 mm, 5 μm ）was adopted. The mobile phase was acetonitrile （A）-0.2% aqueous phosphoric acid （B）with gradient elution （0-15 min, 3%A; 15-40 min, 3%A → 10%A; 40-50 min, 10%A → 15%A; 50-70 min, 15%A → 40%A; 70-90 min,40%A ） at a flow rate of 1.0 mL· min-1. The column temperature was 40 ℃. The detection wavelength was set at 284 nm for 5-hydroxymethyl-2 furaldehyde in the first 30 min, then switched to 240 nm for morroniside and loganin between 30 and 70 min, then switched to 274 nm for paeonol between 70 and 80 min and switched to 216 nm for schisandrin between 80 and 90 rain. Results： The linear ranges of 5-hydroxymethyl-2 furaldehyde, morroniside, loganin, paeonol and schisandrin fell within the ranges of 0.08-2.26 μg （ r =0.999 9 ）, 0.02-0.63 μg （ r=-0.999 9 ）, 0.02-0.62 μg （ r = 1.000 ）, 0.05-1.49 μg （ r=1.000 ） and 0.008-0.24 μg （ r =0.999 9 ）. respectively. The average recoveries （ n=6 ） were 96.8% （ RSD=0.65% ）, 96.3% （ RSD=0.61% ）, 97.7% （ RSD=0.32% ）, 97.7% （ RSD=1.4% ） and 100.6% （ RSD=1.9% ） respectively. The content ranges of the above constituents were 3.194-10.27 mg·g-1, 0.473 2-0.800 4 mg· g-1, 0.736 0- 1.226 mg· g-1, 1.562-2.499 mg·g-1 and 0.035 22-0.143 7 m·g-1 g , respectavely. Conclusion： The proposed methods were reasonable, feasible and reproducible, which could be used for the quality control of Maiwei Dihuang capsules.