Abstract：OBJECTIVE To develop a sensitive ultrahigh performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS) method for simultaneous determination of ginkgolic acids in Yinxingye tablet. METHODS The samples were extracted with 80% methanol. UPLC-MS/MS was performed on an Acquity UPLC BEH C18 column (2.1 mm×5 mm,1.7 μm) with mobile phase consisting of methanol and 0.1% aqueous formic acid. The flow rate was controlled at 0.4 mL·min-1, and the column temperature was set at 30 ℃. A mass spectrometer equipped with electrospray ionization source was used as detector operated in negative ion mode. Multiple reaction monitoring (MRM) was performed. RESULTS Ginkgo acids C13∶0, C15∶1, C17∶1, C17∶2, and C15∶0 possessed good linear correlation in the concentration ranged from 1 to 200 ng·mL-1, with correlation coefficients higher than 0.998 5. The recoveries ranged from 81.57％ to 101.45％ at the spiked levels of 4,40 and 80 ng·ml-1, with RSDs ranging from 4.66% to 11.39%. The limits of detection and quantification were 0. 40-0. 44 pg and 1.00-1.11 pg, respectively. CONCLUSION The established method can be used to simultaneously determine five ginkgolic acids in Yinxingye tablet. Among 73 batches of Yinxingye tablet, 1 batch exceeded the required limit, and the overall quality risk is low.
刘丽娜, 李耀磊, 金红宇, 昝珂, 马双成. 超高效液相色谱-三重四极杆串联质谱测定银杏叶片中5种微量银杏酸含量研究[J]. 中国药学杂志, 2021, 56(20): 1684-1689.
LIU Li-na, LI Yao-lei, JIN Hong-yu, ZAN Ke, MA Shuang-cheng. Determination of Ginkgolic Acids in Yinxingye Tablet by Ultrahigh Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry. Chinese Pharmaceutical Journal, 2021, 56(20): 1684-1689.
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