超高效液相色谱-串联四极杆质谱联用法同时测定蒙药全石榴、中药石榴皮及新鲜石榴中7种成分  

Simultaneous Quantification of 7 Components in Different Parts of Punica granatum Fruits Using Ultra-High Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry(UPLC-QQQMS)

作　　者：王常喜[1] 岳丽丽[1] 许海燕[1] 乌妮尔 黄燕[1] 张海鹏[1] 高杰[1] 马超美[1] 

机构地区：[1]内蒙古大学生命科学学院,内蒙古呼和浩特010021

出　　处：《食品科学》2016年第4期139-143,共5页Food Science

基　　金：内蒙古大学校级大学生创新创业训练计划资助项目(201414199);高等学校博士学科点专项(#20131501110008)

摘　　要：采用超高效液相色谱-串联四极杆质谱联用法,同时检测蒙药全石榴皮及籽、中药石榴皮、鲜石榴皮及籽中诃子鞣质A、诃子鞣质B、诃子裂酸、五没食子酰葡萄糖、鞣料云实素、诃黎勒酸和没食子酸7种成分。选用表儿茶素-4-乙酰半胱氨酸作为内标。石榴样品经粉碎用甲醇（含内标液）溶液超声提取,采用ZORBAX Eclipse XDB-C_（18）柱（2.1 mm×50 mm,1.8μm）,以甲醇-0.1%甲酸溶液为流动相,梯度洗脱,以电喷雾离子源,采用超高效液相色谱-串联四极杆质谱联用动态多反应监测模式测定。结果表明,7种成分检出限均小于0.013 5μg/m L,定量限均小于0.054 2μg/m L,在0.003 4-13.875 0、0.013 5-13.875 0、0.003 4-13.875 0、0.216 8-55.500 0、0.867 2-55.500 0、0.216 8-55.500 0、0.003 4-13.875 0μg/m L范围内,峰面积与质量浓度呈良好线性关系,相关系数均大于0.99;方法回收率为99.44%-105.54%;其日内及日间精密度实验的相对标准偏差分别为0.11%-0.95%和0.14%-1.21%。该方法灵敏度高、稳定性强、操作简便、快捷、准确,可用于蒙药全石榴、中药石榴皮、鲜石榴及其相关食品药品的质量控制。An ultra-high performance liquid chromatography-triple quadrupole mass spectrometry（UPLC-QQQMS） method was developed and validated to simultaneously determine seven constituents including chebumeinin A,chebumeinin B,chebulic acid,pentagalloyl glucose,corilagin,chebulagic acid and gallic acid in dried whole pomegranate（containing peels and seeds,a traditional Mongolian medicinal material）,dried pomegranate peels（a traditional Chinese medicinal material）,and fresh pomegranate peels and seeds（Punica granatum L.）. 4β-（L-acetylcysteinyl）-epicatechin was used as an internal standard for the quantification. The internal standard was added to methanol before being used to extract samples. The separation was performed on an Agilent ZORBAX Eclipse XDB-C-（18） column（2.1mm×50 mm,1.8 μm） with methanol-0.1% formic acid as the mobile phase at a flow rate of 0.4 m L/min. As a result,the linear ranges of chebumeinin A,chebumeinin B,chebulic acid,pentagalloyl glucose,corilagin,chebulagic acid and gallic acid were 0.003 4–13.875 0,0.013 5–13.875 0,0.003 4–13.875 0,0.216 8–55.500 0,0.867 2–55.500 0,0.216 8–55.500 0,and 0.003 4–13.875 0 μg/m L,respectively,with correlation coefficients higher than 0.99. The average recovery rate of the developed method ranged from 99.44% to 105.54% and the intra-day and inter-day relative standard deviations（RSDs） were 0.11%–0.95% and 0.14%–1.21%,respectively. This method is sensitive,simple,fast,and accurate,and can be used for the quality control of pomegranate for medicinal use and related food products or pharmaceuticals.

关 键 词：石榴 全石榴 石榴皮 超高效液相色谱-串联四极杆质谱联用 同时测定 

分 类 号：R284.1[医药卫生—中药学]