作　　者： ; ; ; ; ; ; ;

机构地区： 深圳市中医院

出　　处： 《中国实验方剂学杂志》 2018年第19期73-78,共6页

摘　　要： 目的：建立高效液相色谱-串联质谱法同时测定小儿安神补脑颗粒中8个成分的含量测定方法。方法：采用Agilent TC-C18色谱柱（4.6 mm×250 mm,5μm）;流动相乙腈（A）-10 mol·L-1乙酸铵（B）水溶液,梯度洗脱;进样量10μL。质谱条件采用电喷雾离子源,正负离子同时检测,扫描方式为选择离子扫描模式。结果：甘草苷,毛蕊异黄酮葡萄糖苷,甘草酸铵,柚皮苷,3,6＇-二芥子酰基蔗糖,橙皮苷,新橙皮苷和黄芪甲苷线性范围分别在0.019 5～2.5 mg·L-1（r=0.999 1）,0.078 1～5 mg·L-1（r=0.999 2）,0.078 1～5 mg·L-1（r=0.999 8）,0.312 5～50 mg·L-1（r=0.999 9）,0.019 5～2.5 mg·L-1（r=0.999 2）,0.078 1～10 mg·L-1（r=0.999 0）,0.312 5～20 mg·L-1（r=0.999 4）,0.019 5～1.25 mg·L-1（r=0.999 0）;精密度、稳定性、重复性试验的RSD均〈2%;平均回收率在95.07%～97.79%,RSD均〈2%;甘草苷,毛蕊异黄酮葡萄糖苷,甘草酸铵,柚皮苷,3,6＇-二芥子酰基蔗糖,橙皮苷,新橙皮苷和黄芪甲苷样品含量测定结果依次为187.5～188.1,330.0～331.0,312.1～319.5,1 509.0～1 510.2,172.2～173.0,180.0～181.0,639.0～639.8,37.5～38.2μg·g-1。结论：该方法简单、准确、灵敏、重复性好,可用于小儿安神补脑颗粒的质量评价与控制。 Objective： To establish a high performance liquid chromatography-mass spectrometry（ HPLCMS） method for simultaneously determining eight components in Xiaoer Anshen Bunao granule. Method： Agilent TC-C18（ 4. 6 mm × 250 mm,5 μm） column was adopted with acetonitrile-10 mol·L-1 ammonium acetate solution as the mobile phase for gradient elution,and the injection volume was 10 μL. Electrospray ionization（ ESI） was used in both positive and negative modes, and the selected ion monitoring（ SIM） were used for scanning.Result： Liquiritin,calycosin-7-O-β-D-glucoside,ammonium glycyrrhizinate,naringin,3,6＇-disinapoyl sucrose,hesperidin,neohesperidin, astragaloside Ⅳ showed a good linearity in the ranges of 0. 019 5-2. 5 mg·L-1（ r = 0. 999 1）,0. 078 1-5 mg·L-1（ r = 0. 999 2）,0. 078 1-5 mg·L-1（ r = 0. 999 8）,0. 390 6-50 mg·L-1（ r = 0. 999 9）,0. 019 5-2. 5 mg·L-1（ r = 0. 999 2）,0. 078 1-10 mg·L-1（ r = 0. 999 0）,0. 312 5-20 mg·L-1（ r = 0. 999 4）,0. 019 5-1. 25 mg·L-1（ r = 0. 999 0）,respectively. Relative standard deviations（ RSDs） of precision,stability and reproducibility were all less than 2. 0%. The recoveries for the eight analytes were between 94. 67% and 97. 79%,with RSD less than 2. 0%. The contents of liquiritin,calycosin-7-O-β-Dglucoside, ammonium glycyrrhizinate, naringin, 3, 6＇-disinapoyl sucrose, hesperidin, neohesperidin, and astragaloside Ⅳ were 187. 5-188. 1,330. 0-331. 0,312. 1-319. 5,1 509. 0-1 510. 2,172. 2-173. 0,180. 0-181. 0,639. 0-639. 8, and 37. 5-38. 2 μg·g-1,respectively. Conclusion： This method is simple,accurate,sensitive and repeatable,which can be used for identification,quality evaluation of Xiaoer Anshen Bunao granule.

关 键 词： 小儿安神补脑颗粒 甘草苷 毛蕊异黄酮葡萄糖苷 甘草酸铵 柚皮苷 二芥子酰基蔗糖 橙皮苷 新橙皮苷 黄芪甲苷

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