LC-MS/MS法同时测定回春育子颗粒中9种成分的含量
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篇名: LC-MS/MS法同时测定回春育子颗粒中9种成分的含量
TITLE:
摘要: 目的:建立同时测定回春育子颗粒中9种成分含量的方法。方法:采用液相色谱-串联质谱(LC-MS/MS)法。色谱柱为Shim-pack XR-ODS C18,柱温为30 ℃,进样量为5 μL,离子源为电喷雾离子源,采用多反应监测(MRM)模式;其中阿魏酸、芦丁、丹皮酚、淫羊藿苷、五味子醇甲以乙腈-水为流动相梯度洗脱,正离子模式监测;柚皮苷、毛蕊花糖苷、苦杏仁苷和原儿茶酸采用甲醇-0.1%甲酸水溶液为流动相梯度洗脱,负离子模式监测。结果:阿魏酸、芦丁、丹皮酚、淫羊藿苷、五味子醇甲、柚皮苷、毛蕊花糖苷、苦杏仁苷和原儿茶酸检测质量浓度的线性范围分别为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),检测限分别为0.075、0.30、0.072、0.015、0.015、0.075、0.15、0.30、0.15 ng/mL,定量限分别为0.25、1.00、0.24、0.51、0.49、0.25、0.50、0.99、0.49 ng/mL;回收率在91.39%~103.56%之间(RSD为1.03%~3.67%,n=6),室温下48 h内稳定性试验的RSD为1.4%~3.4%(n=6)。结论:该方法快速、灵敏,重复性好,可用于回春育子颗粒中9种成分的含量测定,可用于回春育子颗粒的质量控制。
ABSTRACT: 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.
期刊: 2018年第29卷第9期
作者: 薛刚强,曹宝帅,高淑丽,张健,潘新艳
AUTHORS: XUE Gangqiang,CAO Baoshuai,GAO Shuli,ZHANG Jian,PAN Xinyan
关键字: 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 granules; Component; LC-MS/MS; Quality control; Determination of content
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