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  

Determination of Ginkgolic Acids in Yinxingye Tablet by Ultrahigh Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry

作　　者：刘丽娜[1] 李耀磊[1] 金红宇[1] 昝珂[1] 马双成[1] LIU Li-na;LI Yao-lei;JIN Hong-yu;ZAN Ke;MA Shuang-cheng(National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]中国食品药品检定研究院,北京100050

出　　处：《中国药学杂志》2021年第20期1684-1689,共6页Chinese Pharmaceutical Journal

基　　金：国家“重大新药创制”科技重大专项资助(2018ZX09303-024)。

摘　　要：目的建立了利用超高效液相色谱-三重四极杆串联质谱测定银杏叶片中银杏酸的分析方法。方法样品经体积分数80%甲醇超声提取后,采用waters Acquity UPLC BEH C_(18)(2.1 mm×5 mm,1.7μm),以甲醇-0.1%甲酸为流动相,流速为0.4 mL·min^(-1),柱温为30℃;采用电喷雾离子源,负离子模式下,以多反应监测方式(MRM)检测。结果银杏酸C13∶0、C15∶1、C17∶1、C17∶2及C15∶0在1~200 ng·mL^(-1)范围内呈良好的线性关系,相关系数均大于0.9985。在4、40、80 ng·mL^(-1)加标水平下的平均加样回收率为81.57%~101.45%,相对标准偏差为4.66%~11.39%,检出限为0.40~0.44 pg,定量限为1.00~1.11 pg。结论建立的检测方法可应用于银杏叶片中银杏酸的测定。73批银杏叶片中有1批超出限度要求,整体风险较低。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 C_(18) column(2.1 mm×5 mm,1.7μm)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 0.9985.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.

关 键 词：超高效液相色谱-三重四极杆串联质谱 银杏酸 银杏叶片 银杏叶制剂 

分 类 号：R917[医药卫生—药物分析学]