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-食品安全质量检测学报-CSCIED科技核心评价数据库-手机版

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

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DOI	10.19812/j.cnki.jfsq11-5956/ts.20250210001
刊名	食品安全质量检测学报 Journal of Food Safety and Quality
年，卷(期)	2025, 16(12)
作者	谢蔓莉, 褚能明, 杨晓霞, 舒晓, 张雪梅, 孟霞, 杨俊英*,
作者单位	重庆市农业科学院农业质量标准与检测技术研究所
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。
Abstract	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.
关键词	畜禽产品；糖皮质激素；QuEChERS；高效液相色谱-串联质谱法
KeyWord	livestock and poultry products; glucocorticoids; QuEChERS; high performance liquid chromatography-tandem mass spectrometry
基金项目
页码	224-230

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引用本文

谢蔓莉, 褚能明, 杨晓霞, 舒晓, 张雪梅, 孟霞, 杨俊英*. 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 [J]. 食品安全质量检测学报. 2025; 16; (12). 224 - 230.

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陈**郑州大学****** 已认证✔

2025-11-06 02:12:30

本文建立了基于乙酸乙酯萃取–QuEChERS净化–HPLC-MS/MS（ESI+，MRM）的畜禽产品中倍他米松与地塞米松残留测定方法。线性良好（0–100 μg/L，r＞0.9994），三类基质的加标回收率与RSD(79.3%–105.8%，1.4%–9.4%)符合常规残留分析要求；LOD/LOQ（倍他米松4.4–4.8/14.6–15.9 μg/kg；地塞米松2.7–3.4/8.9–11.2 μg/kg）显示方法具备较好灵敏度与适用性。整体思路清晰、流程简便，具备实验室常规监测的可操作性。主要亮点 1. 同步覆盖三种不同基质，方法的通用性较好。 2. 将QuEChERS用于糖皮质激素前处理，兼顾效率与成本。 3. 方法学验证指标全面，满足快速筛查与定量的基本需求。

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