School of Public Health, North China University of Science and Technology, Tangshan, Hebei, China.
Hebei Entry-Exit Inspection and Quarantine Bureau, Shijiazhuang, Hebei, China.
J Sep Sci. 2018 Sep;41(17):3432-3440. doi: 10.1002/jssc.201800464. Epub 2018 Aug 6.
We report the fabrication of an anion-exchange monolithic column in a stainless-steel chromatographic column (10 mm × 2.1 mm i.d.) using [2-(acryloyloxy) ethyl]trimethylammonium chloride as the monomer and ethylene dimethacrylate as the crosslinker. The prepared monolith was developed as the adsorbent for the on-line solid-phase extraction of salicylic acid in various animal-origin foodstuffs combined with liquid chromatography and tandem mass spectrometry. The monolith was characterized by using Fourier transform infrared spectroscopy, scanning electron microscopy, nitrogen adsorption analysis, and elemental analysis. Potential factors affecting the on-line solid-phase extraction and liquid chromatography with tandem mass spectrometry analysis were studied in detail. Under the optimized conditions, the total analysis time including cleanup and liquid chromatography with tandem mass spectrometry separation was 17 min. The developed method gave the linear range of 15-750 μg/kg, detection limits (S/N = 3) of 5 μg/kg, and quantification limits (S/N = 10) of 15 μg/kg. The recoveries obtained by spiking 10, 20, and 100 μg/kg of salicylic acid in the animal-origin food samples were in the range of 85.2-98.4%. In addition, the monolith was stable enough for 550 extraction cycles with the precision of peak area ≤11.6%.
我们报告了一种阴离子交换整体柱的制备,该整体柱在不锈钢色谱柱(10mm×2.1mm id)中使用[2-(丙烯酰氧基)乙基]三甲基氯化铵作为单体和乙二醇二甲基丙烯酸酯作为交联剂。制备的整体柱被开发为用于与液相色谱和串联质谱联用的各种动物源性食品中水杨酸的在线固相萃取的吸附剂。通过傅里叶变换红外光谱、扫描电子显微镜、氮气吸附分析和元素分析对整体柱进行了表征。详细研究了影响在线固相萃取和液相色谱-串联质谱分析的潜在因素。在优化条件下,包括净化和液相色谱-串联质谱分离在内的总分析时间为 17 分钟。该方法的线性范围为 15-750μg/kg,检测限(S/N=3)为 5μg/kg,定量限(S/N=10)为 15μg/kg。在动物源性食品样品中添加 10、20 和 100μg/kg 水杨酸的回收率在 85.2-98.4%范围内。此外,整体柱在 550 次萃取循环中具有足够的稳定性,峰面积的精密度≤11.6%。