史颖珠,侯建波,谢文,钱艳,黄超群,张雅琴,刘翠平,张辉.液相色谱-串联质谱法测定山银花中有机酸和黄酮类化合物的含量[J].,2021,37(3):275-285.
液相色谱-串联质谱法测定山银花中有机酸和黄酮类化合物的含量
Simultaneous Determination of Organic Acids and Flavonoids in Lonicerae flos by Liquid Chromatography-Tandem Mass Spectrometry
投稿时间:2020-08-13  
DOI:10.13982/j.mfst.1673-9078.2021.3.0814
中文关键词:  山银花  有机酸  黄酮  液相色谱-串联质谱法
英文关键词:Lonicerae flos  organic acid  flavonoids  high performance liquid chromatography with tandem mass spectrometry
作者简介:史颖珠(1986-),女,高级工程师,研究方向:食品中药物残留检测 通讯作者:侯建波(1983-),男,博士,高级工程师,研究方向:食品质量安全检测研究
基金项目:国家重点研发计划项目(2017YFF0211000)
作者单位
史颖珠 (1.浙江大学生物系统工程与食品科学学院,浙江杭州 310058) 
侯建波 (2.杭州海关技术中心,浙江杭州 310016)(3.浙江省检验检疫科学技术研究院,浙江杭州 310016) 
谢文 (2.杭州海关技术中心,浙江杭州 310016)(3.浙江省检验检疫科学技术研究院,浙江杭州 310016) 
钱艳 (3.浙江省检验检疫科学技术研究院,浙江杭州 310016) 
黄超群 (2.杭州海关技术中心,浙江杭州 310016)(3.浙江省检验检疫科学技术研究院,浙江杭州 310016) 
张雅琴 (3.浙江省检验检疫科学技术研究院,浙江杭州 310016) 
刘翠平 (2.杭州海关技术中心,浙江杭州 310016) 
张辉 (1.浙江大学生物系统工程与食品科学学院,浙江杭州 310058) 
AuthorInstitution
SHI Ying-zhu (1.The College of Biosystems Engineering and Food Science of Zhejiang University, Hangzhou 310058, China) 
HOU Jian-bo (2.The Technic Center of Hangzhou Customs, Hangzhou 310016, China) (3.Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou 310016, China) 
XIE Wen (2.The Technic Center of Hangzhou Customs, Hangzhou 310016, China) (3.Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou 310016, China) 
QIAN Yan (3.Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou 310016, China) 
HUANG Chao-qun (2.The Technic Center of Hangzhou Customs, Hangzhou 310016, China) (3.Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou 310016, China) 
ZHANG Ya-qin (3.Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou 310016, China) 
LIU Cui-ping (2.The Technic Center of Hangzhou Customs, Hangzhou 310016, China) 
ZHANG Hui (1.The College of Biosystems Engineering and Food Science of Zhejiang University, Hangzhou 310058, China) 
摘要点击次数: 24
全文下载次数: 16
中文摘要:
      本文通过甲醇溶液超声提取,HLB固相萃取柱净化,液相色谱-串联质谱法检测,建立了山银花中4种有机酸(绿原酸、咖啡酸、异绿原酸A和异绿原酸C)和14种黄酮类化合物(槲皮素、芦丁、木犀草素、木犀草苷、山奈酚、紫云英苷、芹菜素、野漆树苷、黄芩素、黄芩苷、槲皮素-3-甲基醚、香叶木素、白杨素和山奈素)含量测定的方法。山银花样品经50%的甲醇溶液超声提取40分钟,HLB固相萃取柱净化,采用Mightysil RP-18色谱柱分离,液相色谱-串联质谱法进行检测(电喷雾离子源,多反应监测模式,负离子扫描),外标法定量进行测定。方法定量限(以S/N大于10计)0.005 g/kg-0.05 g/kg,配制0.05、0.10、0.20、0.50和1.00 g/kg线性工作曲线,线性相关系数大于0.993。在山银花样品中进行添加回收试验(添加水平绿原酸10.0、20.0和40.0 g/kg,咖啡酸1.0、2.0和4.0 g/kg,异绿原酸A和异绿原酸C 5.0、10.0和20.0 g/kg,其他化合物0.05、0.10和0.20 g/kg),方法总体回收率69.2%~116%,相对标准偏差3.3%~12.0%。方法实现了山银花中多种主要有机酸和黄酮类化合物含量的同时测定。
英文摘要:
      In this paper, an analytical method for the determination of 4 organic acids (chlorogenic acid, caffeic acid, isochlorogenic acid A and isochlorogenic acid C) and 14 flavonoids (quercetin, rutin, luteolin, cynaroside, kaempferol, astragalin, apigenin, rhoifolin, baicalein, baicalin, quercetin-3-methylether, diosmetin, chrysin and kaempferide) in Lonicerae flos were developed and validated by solid phase extraction and liquid chromatography with tandem mass spectrometry (LC-MS/MS). In Lonicerae flos samples, the organic acids and flavonoids were extracted by methanol solution (concentration: 50%), ultrasonication for 40 min, and cleaned up with HLB column by solid phase extraction. The methanol eluent was ?ltered through nylon membrane and analysis by LC-MS/MS. The solution was separated by Mightysil RP-18 column (150 mm × 4.6 mm (i.d), 3 μm) and the quantitative detection was performed on LC-MS/MS by multiple reaction monitoring (MRM) mode under negative electrospray ionization (ESI-). External standard method was used for quantitation analysis. The limits of quantification (LOQs, S/N>10) were 0.005 g/kg~0.05 g/kg. Single-laboratory method validation data were determined, the calibration standard curves concentrations were 0.05~1.00 g/kg and the correlation coefficient of calibration standard curves was more than 0.993. The recoveries were found in the range of 69.2%~116% and the relative standard deviations were 3.3%~12.0% at the respiked levels (10.0, 20.0 and 40.0 g/kg for chlorogenic acid; 1.0, 2.0 and 4.0 g/kg for caffeic acid; 5.00, 10.0 and 20.0 g/kg for isochlorogenic acid A and isochlorogenic acid C; 0.05, 0.10 and 0.20 g/kg for other compounds). This method was suitable for simultaneous determination and confirmation of 4 organic acid and 14 flavonoids in Lonicerae flos. Key words: Lonicerae flos; organic acid; flavonoids; high performance liquid chromatography with tandem mass spectrometry of quantification (LOQs, S/N>10) were 0.005 g/kg~0.05 g/kg. Single-laboratory method validation data were determined, the calibration standard curves concentrations were 0.05~1.00 g/kg and the correlation coefficient of calibration standard curves was more than 0.993. The recoveries were found in the range of 69.2%~116% and the relative standard deviations were 3.3%~12.0% at the respiked levels (10.0, 20.0 and 40.0 g/kg for chlorogenic acid; 1.0, 2.0 and 4.0 g/kg for caffeic acid; 5.00, 10.0 and 20.0 g/kg for isochlorogenic acid A and isochlorogenic acid C; 0.05, 0.10 and 0.20 g/kg for other compounds). This method was suitable for simultaneous determination and confirmation of 4 organic acid and 14 flavonoids in Lonicerae flos.
查看全文  查看/发表评论  下载PDF阅读器
关闭