OBJECTIVE: To establish the method for simultaneous determination of 9 components in Huichun yuzi granules. METHODS: LC-MS/MS method was adopted. The determination was performed on Shim-pack XR-ODS C18 column with column temperature of 30 ℃. The sample size was 5 μL, and ion source as electrospray ion source; MRM mode was adopted. The acetonitrile-water was used as mobile phase for ferulic acid, rutin, paeonol, icariin and schisandrin (gradient elution); positive ion mode monitoring was conducted. The methanol-0.1% fomic acid water was used as mobile phase for naringin, verbascoside, amygdalin and protocatechuic acid (gradient elution); negative ion mode monitoring was conducted. RESULTS: The linear ranges of ferulic acid, rutin, paeonol, icariin, schisandrin, naringin, verbascoside, amygdalin and protocatechuic acid were 0.499 5-500, 25-1 000, 0.245 9-250, 5.185 1-1 000, 0.981 9-1 000, 0.248 1-125, 2.510 4-250, 10-2 500, 4.999 7-1 000 ng/mL (r≥0.997 8), respectively. The limits of detection were 0.075, 0.30, 0.072, 0.015, 0.015, 0.075, 0.15, 0.30, 0.15 ng/mL,respectively; the limits of quantitation were 0.25, 1.00, 0.24, 0.51, 0.49, 0.25, 0.50, 0.99, 0.49 ng/mL, respectively. The recoveries rate were 91.39%-103.56% (RSD=1.03%-3.67%, n=6). RSDs of stability test ranged 1.4%-3.4% (n=6) within 48 h at room temperature.CONCLUSIONS: The method is rapid, sensitive and reproducible, and can be used for content determination of 9 components in Huichun yuzi granules. It can be used for quality control of Huichun yuzi granules.
关键词
回春育子颗粒成分液相色谱-串联质谱法质量控制含量测定
Keywords
Huichun yuzi granulesComponentLC-MS/MSQuality controlDetermination of content