QuEChERS-超高效液相色谱-串联质谱法测定动物源性食品中8种糖皮质激素残留量

Determination of 8 kinds of glucocorticoids residues in food of animal origin by QuEChERs-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  动物源性  QuEChERS  糖皮质激素  超高效液相色谱-串联质谱法

英文关键词:animal origin  QuEChERS  glucocorticoids  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-串联质谱法测定动物源性食品中8种糖皮质激素残留量的方法。方法 称取猪肉、牛肉、鸡蛋适量样品, 加入1%甲酸-乙腈及兽药残留专用QuRChERS提取包提取、兽药残留专用QuRChERS净化管进行净化。提取液在40 ℃水浴下氮气吹干后, 加入20%乙腈水溶液定容, 以0.5 mmol/L乙酸铵溶液(含0.1%甲酸)-乙腈为流动相梯度洗脱, 经Poroshell 120 EC-C18 (50 mm×2.1 mm, 1.9 μm)色谱柱分离, 多反应监测(multiple reaction monitoring, MRM)模式测定。结果 8种糖皮质激素在0.5~50.0 ng/mL范围内线性关系良好, 相关系数大于0.99, 方法检出限为0.02~0.20 μg/kg, 定量限为0.04~0.80 μg/kg, 回收率范围均在60%~120%, 变异系数小于15%。结论 该方法简单方便快捷, 减少处理步骤及缩短前处理时间, 检测结果稳定, 准确性高, 满足大批量样品的糖皮质激素残留量检测需求。

英文摘要:

      Objective To establish a method for the determination of 8 kinds of glucocorticoids residues in food of animal origin by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry. Methods Appropriate samples of pork, beef and eggs were taken, and purified by adding 1% formic acid-acetonitrile and QuRChERS purification kit for animal residues and QuRChERS purification tube for animal residues. After drying with nitrogen in a water bath at 40 ℃, the extract was added to 20% acetonitrile solution at constant volume and eluted with 0.5 mmol/L ammonium acetate solution (containing 0.1% formic acid) and acetonitrile as mobile phase gradient, separated by Poroshell 120 EC-C18 (50 mm×2.1 mm, 1.9 μm) column and determined by multiple reaction monitoring (MRM) mode. Results The 8 kinds of glucocorticoids had good linear relationships in the range of 0.5–50.0 ng/mL, and the correlation coefficient was greater than 0.99. The limits of detection were 0.02–0.20 μg/kg, and the limits of quantitation were 0.04–0.80 μg/kg. The recoveries were all in the range of 60%–120%, and the coefficient of variation was less than 15%. Conclusion The method is simple, convenient and fast, reduces the processing steps and the pretreatment time, the detection result is stable and the accuracy is high, and it can meet the requirements of the detection of glucocorticoid residue in a large number of samples.