摘要
目的采用UPLC-Q-TOF-MS/MS技术对玉蝴蝶祛斑膏的中间体及单药味进行化学成分鉴定及综合分析,并对其化学成分进行药味归属,为建立玉蝴蝶祛斑膏特征图谱奠定基础。方法以phenomenex Luna Omega Polar C18(2.1 mm×100 mm,1.6μm)为色谱柱,以0.2%乙酸水溶液为流动相A,乙腈为流动相B,梯度洗脱(0~1 min,12%~17%B;1~5 min,17%~28%B;5~10 min,28%~90%B;10~11 min,90%~100%B;11~14 min,100%B);检测波长为300 nm;柱温为25℃,流速为0.25 mL·min^(-1)。并采用G6530C型Q-TOF-MS,质谱检测分别在正、负离子模式下进行,干燥气温度:350℃,干燥气流速:10L·min^(-1),雾化气压力:35 psi,鞘气温度:350℃,鞘气流速:12 L·min^(-1),毛细管电压:4000 V(正模式)和3500 V(负模式),一级质谱选用MS模式,质量扫描范围:100~1500m/z。二级质谱选用Auto-MS/MS模式,质量扫描范围:100~1000 m/z,碰撞电压:10、15、20、30 eV。所得数据由Agilent MassHunter软件采集。数据处理采用Agilent软件Qualitative Navigator(B.08.00)和Qualitative Workflows(B.08.00)。对玉蝴蝶祛斑膏及单药味进行UPLCUV和UPLC-TOF-MS分析,在正负离子模式下采集数据。结果在正负离子模式条件下共鉴定和推测出19个化合物,结合质谱碎片信息对各色谱峰进行指认和归属。其中5个化合物归属到柿叶,14个化合物归属到木蝴蝶,5个化合物归属到菟丝子;结合文献报道和对照品对比,鉴定出15个化合物,主要为黄酮类化合物,其中包括黄芩苷、木蝴蝶苷B、金丝桃苷、芹菜素等。结论本研究比较全面地阐明了玉蝴蝶祛斑膏的化学组成,对玉蝴蝶祛斑膏的鉴别和质量评价研究有重要的参考价值。
Objective To identify and comprehensively analyze the chemical components in Yuhudie macula-removing cream and single pharmaceutical flavor,and to classify the chemical components based on the pharmaceutical flavor,to lay the foundation for the establishment of characteristic map of Yuhudie macula-removing cream by UPLC-Q-TOF-MS/MS.Methods The separation was conducted with phenomenex Luna Omega Polar C18(2.1 mm×100 mm,1.6μm)column,with 0.2%acetic acid aqueous solution as the mobile phase A,acetonitrile as the mobile phase B,and gradient elution(0~1 min,12%~17%B;1~5 min,17%~28%B;5~10 min,28%~90%B;10~11 min,90%~100%B;11~14 min,100%B).The detection wavelength was 300 nm.The column temperature was 25℃and the flow rate was 0.25 mL·min^(-1).G6530C Q-TOF-MS was used to detect the mass spectrum in the positive and negative ion modes.The drying temperature was 350℃,the drying gas flow rate was 10 L·min^(-1),the atomizing gas pressure was 35 psi.The sheath temperature was 350℃,the sheath gas flow rate was 12 L·min^(-1),the capillary voltage were 4000 V(positive mode)and 3500 V(negative mode).MS mode was selected for primary mass spectrometry,with the mass scanning ranged 100 to 1500 m/z.Auto-MS/MS mode was used for secondary mass spectrometry,with a mass scanning range of 100~1000 m/z and collision voltage of 10,15,20 and 30 eV.The data were collected with Agilent MassHunter software.Agilent software Qualitative Navigator(B.08.00)and Qualitative Workflows(B.08.00)were used for the data processing.UPLC-UV and UPLC-TOF-MS analysis were conducted on Yuhudie macula-removing cream and single medicine flavor.The data were collected under the positive and negative ion mode.Results Totally 19 compounds were identified under the condition of positive and negative ion mode,and the chromatographic peaks were identified and attributed according to the mass spectrum fragment information:5 compounds were attributed to Shiye,14 to Muhudie,and 5 to Tusizi.According to literature reports and comparison of control products,15 com
作者
张云
茅向军
詹学雄
张丽艳
陈碧强
于婷
范志梁
唐海姣
王宗权
ZHANG Yun;MAO Xiang-jun;ZHAN Xue-xiong;ZHANG Li-yan;CHEN Bi-qiang;YU Ting;FAN Zhi-liang;TANG Hai-jiao;WANG Zong-quan(Guizhou University of Traditional Chinese Medicine,Guiyang 550025;Increase(Hengqin)Pharmaceutical Institute Company Limited,Zhuhai Guangdong 519031;Fujian Huitian Biological Pharmacy Company Limited,Sanming Fujian 365001)
出处
《中南药学》
CAS
2023年第12期3226-3233,共8页
Central South Pharmacy
基金
广东省科技计划项目(No.2021A0505080007)。
关键词
玉蝴蝶祛斑膏
高效液相-质谱联用
化学成分
木蝴蝶苷B
Yuhudie macula-removing cream
high performance liquid chromatography-mass spectrometry
chemical constituent
baicalin-7-diglucoside
