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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 establish a HPLC wavelength-switching method for the simultaneous determination of 5 chemical constituents of 5-hydroxymethylfurfural, morroniside, loganin, paeonol and schisandrin in the Granule of Maweidihuang Capsules. Methods: The chromatographic column was developed on a Agela Venusil MP C_ (18) (2) (4.6 mm × 250 mm, 5 μm) column with a mobile phase of acetonitrile-A0.2% phosphoric acid (B) , 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 set at 40 ℃ and the wavelength was switched between 0 and 30 min. The detection of morroniside and loganin; 70 ~ 80 min, detection of paeonol at 274 nm wavelength; 80 ~ 90 min, detection of schisandrin at 216 nm wavelength). Results: The linear ranges of 5-hydroxymethylfurfural, morroniside, loganin, paeonol and schisandrin were 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) and 0.008-0.24μg (r = 0.999 9) .The average recoveries were 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%). The results of 10 batches of samples were as follows: 5-hydroxymethylfurfural 3.194-10.27 mg · g -1, morroniside 0.473 2-0.800 4 mg · g -1, loganin 0.736 0 ~ 1.226 mg · g -1, paeonol 1.562 ~ 2.499 mg · g -1, and Schizandrol A 0.035 22 ~ 0.143 7 mg · g -1. Conclusion: This method is reasonable and feasible with good reproducibility and can be used for the quality control of the Granula flavonoids capsule.