HPLC-MS法测定食品中生物碱的研究
详细信息Study on determination of alkaloids in food by high performance liquid chromatography mass spectrometry
-
摘要: 建立了一种高效液相色谱电喷雾质谱（HPLC-ESI-MS）法同时测定食品中六种生物碱的方法。采用ZORBAX SB-C8（2.1mm×150mm,3.5μm）色谱柱,乙腈（A）和pH5的4mmol/L乙酸铵溶液（B）为流动相,梯度洗脱使所有分析物均达到基线分离。采用ESI+一级质谱扫描模式得到甜菜碱、胆碱、苦参碱、阿托品、马钱子碱和乌头碱的定性离子,分别为m/z118.2、104.2、249.5、290.3、395.4和646.4,结合质谱保留时间检测六种生物碱。结果表明,采用1.0mg/mL混合标准溶液,准确性好,RSD<0.59%。该方法应用于检测实际样品荒漠肉苁蓉、山药、宁夏枸杞,添加回收率分别为81.7%112.9%、80.8%117.5%、96.9%119.3%,说明建立的方法可以快速准确的检测实际样品中的生物碱成分。Abstract: An high-performance liquid chromatographic electrospray ionization mass spectrometry (HPLC-ESI-MS) method was developed for the identification of 6 alkaloids in food. A mixture of acetonitrile (A) and pH5 4mmol/L ammonium acetate aqueous solution (B) were used as the mobile phase for the chro-matographic separation on ZORBAX SB-C8 (2.1mm×150mm, 3.5μm) column in the gradient elution mode. Under positive electrospray ionization mode, the protonated molecular[M+H]+ions for betaine (m/z 118.2) , choline (m/z 104.2) , matrine (m/z 249.5) , atropine (m/z 290.3) , brucine (m/z 395.4) and aconitine (m/z 646.4) and retain time were obtained as qualitative analysis. The experiment results indicated that RSD of the precision was less than 0.59% for adding 1.0mg/mL of spike standard. This method was used in the actual sample Herba Cistanche, Rhizoma Dioscoreae, Lycium bar-barum L testing and the average extraction recoveries were in the range of 81.7%112.9%, 80.8%117.5%, 96.9%119.3%. A simple, rapid and accurate identification of 6 alkaloids was successfully achieved using the method.
-
[1] 李媛, 宋媛媛, 张洪泉.肉苁蓉的化学成分及药理作用研究进展[J].中国野生植物资源, 2010, 29 (1) :7-11. [2] 袁书林.山药的化学成分和生物活性作用研究进展[J].食品研究与开发, 2008, 29 (3) :176-179. [3] 张英, 唐玉峰, 白杰.宁夏枸杞营养成分分析及其应用研究进展[J].保鲜与加工, 2009 (4) :9-12. [4] 谈永霞, 王鸣刚, 张继.枸杞和宁夏枸杞叶片主要活性成分含量比较研究[J].食品科学, 2011, 31 (1) :29-32. [5] 李英, 刘志河, 刘建祥, 等.松花粉中胆碱的提取及测定研究[J].光谱实验室, 2006, 1 (1) :44-46.. [6] 王晓菁, 吴燕, 王黎明.固相萃取-高效液相色谱法测定枸杞中甜菜碱[J].食品科学, 2010, 31 (8) :199-201. [7] 李媛媛, 关树文, 王伟, 等.高效液相色谱法测定婴幼儿配方乳粉中的胆碱[J].食品科技, 2009, 34 (10) :263-265. [8] 龚立冬, 曹玉华, 侯建霞.高效液相色谱-蒸发光散射测定肉苁蓉中的甜菜碱[J].色谱, 2007, 25 (2) :280-281. [9] 张雪琴, 周欣, 王道平, 等.液相色谱-电喷雾质谱联用研究不同产地吴茱萸中的生物碱成分[J].分析化学, 2005, 33 (2) :241-244. [10] 王柯, 郑荣, 简龙海, 等.火锅调料中5种生物碱成分的液相色谱-串联质谱测定法[J].中国卫生检验杂志, 2011, 21 (2) :363-365. [11] 沈燕, 韩超, 刘翠平, 等.高效液相色谱-串联质谱法同时测定夏天无中的4种生物碱[J].色谱, 2011, 29 (2) :176-179.
计量
- 文章访问数:
- HTML全文浏览量:
- PDF下载量:
下载:
