College of Food Science and Engineering, South China University of Technology, Guangzhou, 510640, China.
Guangzhou Quality Supervision and Testing Institute, Guangzhou, 510640, China.
J Chromatogr A. 2019 Jul 5;1596:1-7. doi: 10.1016/j.chroma.2019.02.061. Epub 2019 Feb 27.
The presence of potential carcinogen 4(5)-Methylimidazole (4-MeI) in foods causes much concern, stressing the need of a sensitive determination means. Here, we proposed a high-sensitivity method to determine 4-MeI in biscuits using dansyl chloride derivatization and disperse liquid-liquid micro-extraction (DLLME) followed by a liquid chromatography-ion trap mass spectrometry (LC-IT-MS) analysis. This developed method was subsequently compared to the solid phase extraction combining with liquid chromatography-triple quadrupole mass spectrometry (SPE-LC-QqQ-MS) method. The optimized derivatization conditions were 30 °C and 10 min. Results suggested that the column retention time (RT) was significantly extended, and the MS signal response of 4-MeI-dansyl derivative was also amplified. The developed DLLME-LC-IT-MS method in 4-MeI determination provided satisfactory linearity in a range of 0.5-300 ng/mL (R > 0.9991), inter-day accuracy (87-102%) and precision (%RSD ≤ 13.6%) with the quantification limit of 0.2 ng/mL, which obtained similar results comparing to the conventional SPE-LC-QqQ-MS method.
食品中存在潜在致癌物 4(5)-甲基咪唑(4-MeI)引起了广泛关注,强调了需要一种灵敏的测定方法。在这里,我们提出了一种使用丹磺酰氯衍生化和分散液液微萃取(DLLME)结合液相色谱-离子阱质谱(LC-IT-MS)分析测定饼干中 4-MeI 的高灵敏度方法。该方法随后与固相萃取结合液相色谱-三重四极杆质谱(SPE-LC-QqQ-MS)法进行了比较。优化的衍生化条件为 30°C 和 10 min。结果表明,柱保留时间(RT)显著延长,4-MeI-丹磺酰衍生物的 MS 信号响应也得到增强。开发的 DLLME-LC-IT-MS 方法用于 4-MeI 的测定,在 0.5-300 ng/mL 范围内具有令人满意的线性关系(R > 0.9991)、日内准确度(87-102%)和精密度(%RSD ≤ 13.6%),定量限为 0.2 ng/mL,与传统的 SPE-LC-QqQ-MS 方法得到的结果相似。