高效液相色谱-串联质谱法测定畜禽产品中倍他米松和地塞米松的残留量

Determination of betamethasone and dexamethasone residues in livestock and poultry products by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  畜禽产品  糖皮质激素  QuEChERS  高效液相色谱-串联质谱法

英文关键词:livestock and poultry products  glucocorticoids  QuEChERS  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法检测3种不同基质的畜禽产品中糖皮质激素(glucocorticoids, GCs)(倍他米松和地塞米松)残留量的方法。方法 样品采用乙酸乙酯提取, 通过QuEChERS净化方式, 后过0.22 μm有机微孔滤膜, 在正离子模式下采用多反应监测(multiple reaction monitoring, MRM)模式, 以0.1%甲酸水溶液和乙腈作为流动相, 经高效液相色谱-串联质谱仪进行定性定量分析。结果 在0~100 μg/L的质量浓度范围内, 线性关系良好, 相关系数大于0.9994, 回收率在79.3%~105.8%之间, 相对标准偏差(relative standard deviations, RSDs)在1.4%~9.4%之间。倍他米松的检出限(limits of detection, LODs)为4.4~4.8 μg/kg, 定量限(limits of quantitation, LOQs)为14.6~15.9 μg/kg; 地塞米松的LODs为2.7~3.4 μg/kg, LOQs为8.9~11.2 μg/kg。结论 该方法具有较高的灵敏度和准确性, 适用于测定畜禽产品中糖皮质激素类药物的残留量。

英文摘要:

      Objective To establish a method for the determination of glucocorticoids (GCs) (betamethasone and dexamethasone) in livestock and poultry products with 3 kinds of different substrates by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with ethyl acetate and purified by QuEChERS, filtered by 0.22 μm organic microporous membrane. The target analytes were subjected to qualitative and quantitative analysis by high performance liquid chromatography-tandem mass spectrometry under positive ion mode with multiple reaction monitoring (MRM) pattern, using a mobile phase consisting of 0.1% formic acid aqueous solution and acetonitrile. Results The calibration curve showed a good linear from concentration 0–100 μg/L and the correlation coefficient was greater than 0.9994. The recoveries were from 79.3% to 105.8%, and the relative standard deviations (RSDs) were between 1.4% and 9.4%. The limits of detection (LODs) and limits of quantification (LOQs) of betamethasone were 4.4–4.8 μg/kg and 14.6–15.9 μg/kg respectively. The LODs and LOQs of dexamethasone were 2.7–3.4 μg/kg and 8.9–11.2 μg/kg, respectively. Conclusion The method is suitable for the determination of glucocorticoid residues in livestock and poultry products with its high sensitivity and accuracy.