同时测定人血浆中柚皮苷、柚皮素质量浓度的HPLC-MS/MS方法学  

HPLC-MS/MS method for simultaneous determination of naringin and naringenin in human plasma

作　　者：曾璇[1] 苏薇薇[1] 白杨[1] 彭维[1] 姚宏亮[1] ZENG Xuan SU Weiwei BAI Yang PENG Wei YAO Hongliang(School of Life Sciences, Sun Yat-sen University ,Guangdong Engineering ＆ Technology Research Center for Quality and Efficacy Re-evaluation of Post-market Traditional Chinese Medicine, Guangzhou 510275, China)

机构地区：[1]中山大学生命科学学院∥广东省中药上市后质量与药效再评价工程技术研究中心,广东广州510275

出　　处：《中山大学学报（自然科学版）》2017年第1期125-130,共6页Acta Scientiarum Naturalium Universitatis Sunyatseni

基　　金：国家"重大新药创制"科技重大专项课题(2015ZX09101014);广东省应用型科技研发专项资金项目(2015B020234004)

摘　　要：采用HPLC-MS/MS建立了同时测定人血浆中柚皮苷、柚皮素质量浓度的方法。以异槲皮苷为内标,血浆样品经乙酸乙酯萃取后,以Agilent Poroshell 120 EC-C18(3.0 mm×30 mm,2.7μm)为色谱柱,甲醇-水(体积比45∶55,均含φ=0.1%甲酸)为流动相,流速为0.4 m L·min-1;采用电喷雾负离子(ESI-)、多反应离子检测(MRM)模式检测,用于定量分析的离子对分别为柚皮苷m/z 579.1/270.8、柚皮素m/z 270.9/150.7、异槲皮苷(内标)m/z 463.1/299.8。经方法学验证,柚皮苷、柚皮素分别在0.251 0~100.4、0.503 0~201.2ng·m L-1质量浓度范围内线性关系良好,批间、批内精密度均符合要求,提取回收率高。结果表明,HPLC-MS/MS法灵敏度好、准确性高、重现性好,适用于测定人血浆中柚皮苷、柚皮素质量浓度。The aim of the study was to establish an HPLC-MS/MS method for simultaneous determination of naringin and naringenin in human plasma.Naringin and naringenin were extracted from plasma by eth-yl acetate,then determined by HPLC-MS/MS taking isoquercitrin as internal standard （IS）.Chromato-graphic separation was carried out on a Agilent Poroshell 1 20 EC-C1 8 column （3.0 mm ×30 mm,2.7μm）.The mobile phase was composed of solvent A （0.1% formic acid,V/V）and B （methanol with 0.1%formic acid,V/V）.The flow rate was 0.4 mL·min-1 .Electrospray ionization （ESI）source was applied and operated in multiple reaction monitoring （MRM）mode with the transitions of m/z 579.1 /270.8,m/z 270.9/1 50.7,m/z 463.1 /299.8 for naringin,naringenin and IS,respectively.The method was validated over the concentration range of 0.251 0 -1 00.4 ng·mL-1 for naringin,and 0.503 0 -201.2 ng·mL-1 for naringenin,respectively.The intra-and inter-run precisions were within the accept-able range,and the extraction recoveries were satisfactory.The established method is highly sensitive,accurate and reproducible,which can be applied for the simultaneous determination of naringin and nar-ingenin in human plasma.

关 键 词：人血浆 柚皮苷 柚皮素 HPLC—MS/MS 

分 类 号：R965[医药卫生—药理学]