HPLC-MS/MS法同时测定骨疏康颗粒及骨疏康胶囊中6个成分的含量

目的：建立高效液相色谱-串联质谱法测定骨疏康颗粒及骨疏康胶囊中6个成分（淫羊藿苷、毛蕊异黄酮葡萄糖苷、丹参酮Ⅱ_A、柚皮苷、黄芪甲苷、毛蕊花糖苷）的含量。方法：采用XTerra C₁₈色谱柱（2.1 mm×150 mm，3.5 μm）分离，以0.1%甲酸水溶液-乙腈作为流动相进行洗脱，采用电喷雾离子源（ESI），正负离子同时检测方式，多反应监测（MRM）模式进行定性和定量分析。结果：6个成分线性相关系数均>0.998 9，平均回收率为94.2%~104.4%，RSD（n=6）为3.4%~6.5%，精密度、稳定性、重复性试验的RSD（n=6）均小于5.8%。颗粒剂及胶囊剂各3批样品中淫羊藿苷、毛蕊异黄酮葡萄糖苷、丹参酮Ⅱ_A、柚皮苷、黄芪甲苷、毛蕊花糖苷的含量结果依次分别为2.011~2.034、0.058 61~0.061 82、0.084 59~0.087 54、0.102 7~0.106 2、0.053 42~0.058 91、0.042 81~0.045 18 mg·g^-1和9.384~9.530、0.577 2~0.611 8、0.684 5~0.715 7、1.699~1.777、0.624 3~0.636 3、0.320 7~0.324 6 mg·g^-1。结论：所建立方法可为骨疏康胶囊及骨疏康颗粒的质量控制提供依据。

Objective:To establish an HPLC-MS/MS method for the determination of icariin,calycosin-7-glucoside,tanshinone Ⅱ_A,naringin,astragaloside IV and acteoside in Gushukang granula and Gushukang capsules.Methods:The chromatographic separation was performed on an XTerra C₁₈ column(2.1 mm×150 mm,3.5 μm)by using elution with acetonitrile and water(containing 0.1% formic acid)as mobile phase.The MS analysis worked in ESI positive and negative modes.Qualitative and quantitative analysis were carried out in multiple reaction monitoring(MRM)model.Results:The correlative coefficients of six components were above 0.998 9.The average recoveries were 94.2%-104.4% and the RSDs ranged from 3.4% to 6.5%(n=6).Precision,stability and repeatability tests RSDs were less than 5.8%(n=6).The contents of icariin,calycosin-7-glucoside, tanshinone Ⅱ_A,naringin,astragaloside IV and acteoside in granula were 2.011-2.034 mg·g^-1,0.058 61-0.061 82 mg·g^-1,0.084 59-0.087 54 mg·g^-1,0.102 7-0.106 2 mg·g^-1,0.053 42-0.058 91 mg·g^-1, 0.042 81-0.045 18 mg·g^-1,and those in capsule weres 9.384-9.530 mg·g^-1,0.577 2-0.611 8 mg·g^-1,0.684 5-0.715 7 mg·g^-1,1.699-1.777 mg·g^-1,0.624 3-0.636 3 mg·g^-1 and 0.320 7-0.324 6 mg·g^-1,respectively.Conclusion:The method can be used for the quality control of Gushukang granula and Gushukang capsule.

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