UPLC-MS/MS法同时测定清肝健脾颗粒中19个成分的含量OA

Objective:To establish a UPLC-MS/MS method for the simultaneous determination of 19 components in 11 herbs such as Crataegi fructus and Artemisiae scopariae herba in Qinggan Jianpi granules,and to improve the quality control standard.Methods:The analysis method was performed on a 40 ℃ thermostatic Agilent Eclipse Plus-C18 column(100 mm ×2.1 mm,1.8 μm),with the mobile phase comprising of 0.1％formic acid-0.01 mol·L-1 ammonium formate(A)and acetonitrile(B)(0-20 min,10％→90％B)flow-ing at 0.3 mL·min-1.The MS/MS asystem was operated by Agilent 6460 triple quadrupole system(A.00.06.37),multiple reaction monitoring(MRM)under ESI+and ESI-.Results:The 19 components(Hyperoside,Rutoside,23-Acetate alisol B/C,Luteolin,Polydatin,Sodium Danshensu,Salvianolic Acid B,Tanshinone Ⅱ A,Emodin,Chrysophanol,Rhein,Physcion,Aloe-emodin,Auran-tio-obtusin,Astragaloside Ⅳ,Saikosaponin a/d,2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside)were completely separated within 20 min,linear relationship is good(r2＞0.99),Linear range coverage 0.06-321.55 μg·mL-1,Precision,stability and repeatabili-ty test RSD were＜3.0％.Sample recovery 96.8％-103.7％(RSD ≤2.0％).Content determination of 3 batches of samples shows the content range of each component 0.75-267.7 μg·g-1.Conclusion:This method is accurate,sensitive,detection limit was 0.08 μg·mL-1,repeatability is good,realize multi-component synchronous detection within 20 min,Comprehensively control the quality of herbal medicines,can be used for quality control of Qinggan Jianpi Granules and related compound preparations.