目的建立超高效液相色谱-四极杆飞行时间质谱快速筛查和确证草鱼中39种糖皮质激素残留的方法。方法样品加入饱和氯化钠溶液后用乙腈涡旋提取,提取液经酸性氧化铝柱净化,以0.1%(V/V)甲酸水溶液和0.1%(V/V)甲酸乙腈溶液为流动相进行梯度洗脱,经Phenomenex Kinetex C18柱(100 mm×2.1mm, 2.6μm)分离。采用电喷雾离子源,正离子扫描和信息依懒性扫描(information dependent acquisition,IDA)模式进行分析,外标法进行定量。结果 39种糖皮质激素在1~100μg/L浓度范围内线性关系良好,相关系数r均大于0.998,方法检出限为2μg/kg,定量限为5μg/kg。对草鱼进行3个水平的加标回收试验,回收率为67.7%~126.5%,相对标准偏差为4.52%~14.67%。结论本方法简单、高效、重复性好,适用于草鱼中糖皮质激素的快速筛查和确证。
Objective To establish a rapid method for screening and confirming 39 glucocorticoid residues in Ctenopharyngodon idellus by ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry. Methods The sample was extracted by acetonitrile vortex after adding saturated sodium chloride solution, and the extract was purified by acidic alumina column, then gradient elution was performed using gradient with 0.1%(V/V) formic acid aqueous solution and 0.1%(V/V) formic acid acetonitrile solution as mobile phase, and separated by Phenomenex Kinetex C18 column(100 mm×2.1 mm, 2.6 μm). Electrospray ion source, positive ion scanning and information dependent acquisition(IDA) mode were used for analysis, and external standard method was used for quantitative analysis. Results The linear relationship between 39 glucocorticoids was good in the range of 1-100 g/L,and the correlation coefficient r was greater than 0.998. The detection limit was 2 g/kg and the quantitative limit was 5 g/kg. Three levels of standard addition and recovery tests were carried out on grass carp, with recovery rates of 67.7%-126.5% and relative standard deviations of 4.52%-14.80%. Conclusion This method is simple and sensitive, and is suitable for the analysis of the glucocorticoid in Ctenopharyngodon idellus.
Journal of Food Safety and Quality
high resolution time-of-flight mass spectrometry