摘要
建立了液相色谱-四极杆飞行时间质谱(LC-Q-TOF MS)对中华鳖中未知着色剂的快速筛查方法。20个中华鳖样品经过简易的乙腈提取净化后,利用液相色谱-二极管阵列检测器(LC-DAD)对未知着色剂进行定位。选定其中响应最强的样品S7,同时在线获取其在不同洗脱程序下未知着色剂定位时间段的质谱信息,经阴性样品扣除本底后匹配获得一对精确质量数差异在5 mDa以内的特征提取离子(分别为564.397 73 Da和564.395 61 Da)。通过质谱定性分析处理软件对上述特征提取离子对进行分子式生成,确认两者分子式为C40H52O2,推测其同为未知着色剂。结合该未知着色剂的紫外-可见光谱信息与文献资料,推断该化合物可能为角黄素。通过角黄素标准品建立的飞行时间质谱"二级确证谱库"对样品中未知着色剂进行进一步的匹配确证,最终确证其为角黄素。本研究讨论了基于LC-Q-TOF MS方法的化合物筛查策略,实验表明其可快速对中华鳖中的未知着色剂进行筛查和确证。
A method of non-target pigment screening in Chinese softshell turtle has been established by using liquid chromatography coupled to time of flight mass spectrometry（LC-Q-TOF MS）. After being purified by a simple acetonitrile extraction work,the non-target pigment in 20 Chinese softshell turtle samples was detected by liquid chromatography-photodiode array detection（LC-DAD）. The S7 sample,which has a strong spectral response,was chosen to extract the mass spectrometry information of the non-target pigment on different gradient elution conditions. In order to get the characteristic molecular mass ion（564. 397 73 Da and 564. 395 61 Da）of the non-target pigment,qualitative spectral full scan with negative sample was used. The molecular formula generation data and the literature information prompted speculation that the non-target pigment was canthaxanthin with the formula of C40H52O2. By comparing the canthaxanthin standard material MS / MS information,the result was confirmed accurate. A strategy of LC-Q-TOF MS method for the qualitative analysis of unknown compounds is discussed,and the results indicated that the described method can be effectively applied to qualitative analysis for non-target pigment in Chinese softshell turtle.
出处
《色谱》
CAS
CSCD
北大核心
2015年第12期1251-1256,共6页
Chinese Journal of Chromatography
基金
浙江省科技厅公益技术研究农业项目(2013C32062
2015C32029)
浙江省自然科学基金项目(LQ14C190001)
2013年浙江省农业标准化研究项目
关键词
液相色谱-四极杆-飞行时间质谱法
未知物鉴定
着色剂
中华鳖
liquid chromatography-quadrupole time of fight mass spectrometry（LC-Q-TOF MS）
non-target compound identification
pigment
Chinese softshell turtle
