摘要
目的:运用超高效液相色谱-飞行时间质谱联用(UPLC-Q-TOF-MS)技术法,对复方益肝灵片中的化学成分进行快速鉴定及定量分析。方法:采用Waters XBridge BEH C_(18)色谱柱(50 mm×2.1 mm,1.7μm),以0.1%甲酸水-甲醇梯度洗脱,体积流量0.3 mL·min^(-1);进样量1μL。质谱采用电喷雾离子源(ESI),正负离子模式下同时采集,通过精确质量数、二级质谱碎片信息和保留时间,参照文献和对照品对化合物进行鉴定;通过Product Ion扫描模式对9种成分进行定量。结果:结合参考文献和对照品信息,共鉴定化合物29个,其中22个化合物来源于五味子,7个化合物来源于水飞蓟素。定量分析方法显示,9种成分在限定质量浓度范围内线性关系良好;加样回收率在96.0%~101.1%,RSD≤3.4%。结论:建立了UPLC-Q-TOF-MS法对复方益肝灵片的成分进行快速分析,为其质量控制及药效机制的阐明提供理论参考。
OBJECTIVE To identify and quantify the chemical constituents of compound Yiganling tablets by UPLC-Q-TOF-MS.METHODS Compound Yiganling tablet was analyzed by UPLC-Q-TOF-MS under the both negative and positive ion modes. The chromatographic separation was performed on Waters XBridge BEH C18 column（50 mm × 2. 1 mm,1. 7 μm） by using a mobile phase consisted of methanol and 0. 1% formic acid water at the flow rate of 0. 3 mL·min^-1 for gradient elution and the injection volume was1 μL. Quantization was performed by MS/MS using product ion scan mode. RESULTS Twenty-nine compounds were identified. The quantization method performed for analyzing nine compounds in compound Yiganling tablet was systematically validated. The regression equations showing good linear relationships between peak areas and contents of compounds were obtained. The average recoveries of the compounds ranged from 96. 0% to 101. 1% and the RSD was less than 3. 4%. CONCLUSION The developed method is sensitive,accurate and rapid,and can be used for simultaneous qualitative and quantitative analysis of the chemical constituents of compound Yiganling tablets.
作者
李颖
吴茵
李亚静
李倩
王祁民
董占军
LI Ying;WU Yin;LI Ya-jing;LI Qian;WANG Qi-min;DONG Zhan-jun(Graduate School of Hebei Medical University,Hebei Shijiazhuang 050051,China;Department of Pharmacy,Hebei General Hospital,Hebei Shijiazhuang 050017,China)
出处
《中国医院药学杂志》
CAS
北大核心
2018年第17期1801-1807,共7页
Chinese Journal of Hospital Pharmacy
