LC-MS/MS法同时测定回春育子颗粒中9种成分的含量  

Simultaneous Determination of 9 Components in Huichun yuzi Granules by LC-MS/MS

作　　者：薛刚强[1] 曹宝帅 高淑丽[1] 张健 潘新艳[4] XUE Gangqiang;CAO Baoshuai;GAO Shuli;ZHANG Jian;PAN Xinyan(Dept. of Reparation, Shijiazhuang Fourth Hospital, Shijiazhuang 050011, China;Hengshui Food and Drug Inspection and Testing Center, Hebei Hengshui 053000, China;Dept. of TCM, Shijiazhuang Fourth Hospital, Shijiazhuang 050011, China;Dept. of Medical Administration, Hebei Provincial People＇s Hospital, Shijiazhuang 050051, China)

机构地区：[1]石家庄市第四医院制剂科,石家庄050011 [2]衡水市食品药品检验检测中心,河北衡水053000 [3]石家庄市第四医院中医科,石家庄050011 [4]河北省人民医院医务处,石家庄050051

出　　处：《中国药房》2018年第9期1213-1217,共5页China Pharmacy

基　　金：河北省医学科学研究课题计划项目(No.20130293)

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5μL,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/m L(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/m L,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/m L;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。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/m L（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/m L,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/m L,respectively. The recoveries rate were91.39%-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 

分 类 号：R927.2[医药卫生—药学]