摘要
本研究基于超高效液相色谱-四极杆-飞行时间串联质谱(UPLC-Q-TOF MS/MS)技术,结合主成分分析和正交偏最小二乘法-判别分析等多元统计分析,以厄瓜多尔产地可可豆为研究对象,筛选和鉴定可可壳的特征标志物,并利用该特征标志物实现可可粉中可可壳掺入量的定量检测。结果表明,可可粉与可可壳的组分具有较大差异。可可壳的特征标志物为苦木内酯Ⅰ;当可可粉中掺入可可壳的量在1%~50%范围内时,苦木内酯Ⅰ的峰面积与可可壳掺入量之间存在良好的线性关系(相关系数R^(2)>0.999 9),方法的检出限和定量限分别为0.3%和1%。使用该方法进行盲样验证发现,检测含量和实际掺入量基本一致,并对市售样品进行检测,可可壳含量在2.51%~9.03%之间。本方法具有较高的准确性和灵敏度,可用于市售可可粉的掺假鉴别。
An assay combined ultra performance liquid chromatography-quadrupole-time of flight-tandem mass spectrometry(UPLC-Q-TOF MS/MS) with the multivariate statistical analysis methods including principal component analysis and orthogonal partial least squares-discriminate analysis was established for screening and identifying the characteristic markers of cocoa shell relative to cocoa powder, which could be used to quantitatively detect the content of cocoa shell in cocoa powder. The cocoa beans from Ecuador were selected as the research object, and the results showed that there was a great difference between cocoa powder and cocoa shell. One characteristic marker was identified as nigakilactone Ⅰ. There was a good linear relationship between the peak area of nigakilactone Ⅰ and the content of cocoa shell when the content of cocoa shell in cocoa powder was in the range of 1%-50%, the correlation coefficient was greater than 0.999 9. The detection limit and quantitative limit were 0.3% and 1%, respectively. In addition, this method was used for blind sample verification and commercial sample testing. The blind sample verification results showed that the detection content was basically consistent with the actual adulterated content, and the detection content of cocoa shell ranged from 2.51% to 9.03%. This method has high accuracy and high sensitivity, which can be used for identification of commercial cocoa powder adulteration.
作者
张雅莉
韩建勋
宋薇
魏海燕
侯卫静
富玉
付萌
李婷
ZHANG Ya-li;HAN Jian-xun;SONG Wei;WEI Hai-yan;HOU Wei-jing;FU Yu;FU Meng;LI Ting(Pony Testing International Group Co.Ltd,Beijing100095,China;Pony Testing International Group Beijing Academy of Inspection and Certification Co.Ltd,Beijing100095,China)
出处
《质谱学报》
EI
CAS
CSCD
北大核心
2022年第1期121-130,I0006,共11页
Journal of Chinese Mass Spectrometry Society
