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| 超高效液相色谱-串联质谱法测定食品中乳酸链球菌素残留量 |
| Determination of lactostreptococcin residues in food by ultra-high performance liquid chromatography-tandem mass spectrometry |
| 投稿时间：2025-04-14 修订日期：2025-07-05 |
| DOI： |
| 中文关键词: 乳酸链球菌素 残留量 超高效液相色谱-串联质谱法 食品: |
| 英文关键词:Lactistreptococcin Residual amount Ultra high performance liquid chromatography-tandem mass spectrometry food |
| 基金项目:四川省2023年“天府菜油”支持建立科技创新团队奖补项目(No. 2023TFR004) |
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| 中文摘要: |
| 建立一种超高效液相色谱-串联质谱法测定多种食品中乳酸链球菌素(Nisin)残留量的方法。样品用0.1%甲酸溶液+乙腈(80+20)提取、正己烷去脂,以0.1%甲酸溶液和乙腈为流动相梯度洗脱,经ZORBAX Eclipse Plus C18(100 mm×2.1 mm,1.8 μm)色谱柱分离,采用电喷雾离子源、正离子多反应监测模式检测,基质匹配标准曲线外标法定量。结果表明,Nisin A和Nisin Z在0.5 μg/mL~50.0 μg/mL范围内线性关系良好,相关系数大于0.995,检出限和定量限分别为0.15 mg/kg~0.6 mg/kg和0.3mg/kg~1.0 mg/kg,在1.0 mg/kg、5.0 mg/kg、200.0 mg/kg三个加标水平下,回收率在83.4%~112.9%之间,相对标准偏差为1.27%~8.85%。所建立的方法快速高效、重复性好、灵敏度高、定性定量准确,可用于批量食品样品中Nisin A和Nisin Z的测定。 |
| 英文摘要: |
| ABSTRACT:An ultra-high performance liquid chromatography-tandem mass spectrometry method was developed for the determination of Nisin residues in various foods. The samples were extracted with 0.1% formic acid solution + acetonitrile (80+20), delipid with n-hexane, eluted with 0.1% formic acid solution and acetonitrile as mobile phase gradient, and separated by ZORBAX Eclipse Plus C18 (100 mm×2.1 mm, 1.8 μm) column. Electrospray ion source and positive ion multi-reaction monitoring mode were used for detection, and matrix matching standard curve external standard method was used for quantification. The results showed that the linear relationship between Nisin A and Nisin Z was good in the range of 0.5 μg/mL to 50.0 μg/mL, and the correlation coefficient was greater than 0.995. The limits of detection and quantitation were 0.15 mg/kg to 0.6 mg/kg and 0.3mg/kg to 1.0 mg/kg, respectively. The recoveries ranged from 83.4% to 112.9% and the relative standard deviations were 1.27% to 8.85% at the three added levels of 1.0 mg/kg, 5.0 mg/kg and 200.0 mg/kg. The established method is fast, efficient, repeatable, sensitive and accurate, and can be used for the determination of Nisin A and Nisin Z in batch food samples. |
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