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| 超高效液相色谱-串联质谱法结合多功能净化柱测定干海参中50种抗生素残留 |
| Determination of 50 kinds of antibiotic residues in dried sea cucumbers by multifunctional purification column with ultra performance liquid chromatography-tandem mass spectrometry |
| 投稿时间：2025-04-10 修订日期：2025-06-20 |
| DOI： |
| 中文关键词: 多功能净化柱 超高效液相色谱-串联质谱法 干海参 抗生素残留 |
| 英文关键词:multifunctional purification column ultra performance liquid chromatography-tandem mass spectrometry dried sea cucumbers antibiotic residues |
| 基金项目:江苏省市场监督管理局技术能力提升项目（NL2021047）；连云港市科技计划项目（SF2331） |
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| 中文摘要: |
| 目的 建立多功能净化柱净化结合超高效液相色谱-串联质谱法同时检测干海参中50种抗生素的分析方法。方法 样品经50%乙腈水溶液提取,多层复合净化柱净化,采用Waters ACQUITY UPLC HSS T3(100 mm×2.1 mm,1.7 μm)色谱柱分离,以乙腈和 0.1%甲酸水(含5 mmol/L乙酸铵)作为流动相洗脱,质谱采用电喷雾正离子模式扫描及多反应监测采集方式(MRM)监测,外标法定量。结果 50种抗生素在0.1-100.0 ng/mL浓度范围内线性关系良好,相关系数均大于0.99,方法检出限在0.5-2.0 μg/kg之间,定量限在1.0-5.0 μg/kg之间。考察基质空白在3个不同浓度时加标试验,定量限浓度平均回收率为54.8%～120.0%,相对标准偏差(RSD, n=6)为0.08%～9.15%。结论 该方法操作简便、灵敏度高、精密度好,适用于干海参中多种抗生素的快速筛查以及定性定量分析检测。 |
| 英文摘要: |
| Objective To establish a method for simultaneous determination of 50 kinds of antibiotics in dried sea cucumbers by multifunctional purification column combined with ultra performance liquid chromatography-tandem mass spectrometry. Methods The sample was extracted with 50% acetonitrile aqueous solution. After purification by multifunctional purification column, 50 kinds of antibiotics were separated using Waters ACQUITY UPLC HSS T3(100 mm×2.1 mm,1.7 μm) column with acetonitrile and 0.1% formic acid aqueous solution (include 5mmol/L ammonium acetate) as mobile phase. The mass spectrum was performed by electrospray positive ion mode scanning and multi-reaction monitoring acquisition (MRM), and quantified by external standard method. Results The results showed that 50 kinds of antibiotics exhibited good linearity in the range of 0.1–100.0 ng/mL, and the correlation coefficients were all greater than 0.99. The detection limit of the method was 0.5–2.0 μg/kg, the quantitation limit was 1.0-5.0 μg/kg. Recovery tests were carried out at three levels in the blank matrix, the average recoveries of the detection limit were in the range of 54.8%-120.0%, and all the relative standard deviations (RSD, n=6) were 0.08%-9.15%. Conclusion This method is easy and simple to handle, has high sensitivity and good accuracy, it can be applied to rapid screening and qualitative and quantitative detection of multiple antibiotics in dried sea cucumbers. |
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