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 performance liquid chromatography-tandem mass spectrometry

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 performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 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残留量的方法。方法 样品用0.1%甲酸溶液+乙腈(80:20, V:V)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)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 乳酸链球菌素A和乳酸链球菌素Z在0.5~50.0 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0.05~0.30 mg/kg和0.15~1.00 mg/kg, 在1.0、5.0、200.0 mg/kg 3个加标水平下, 回收率为88.8%~106.2%, 相对标准偏差为1.32%~8.85%。结论 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乳酸链球菌素A和乳酸链球菌素Z的测定。

英文摘要:

      Objective To develop an ultra performance liquid chromatography-tandem mass spectrometry method for the determination of Nisin residues in various foods. Methods The samples were extracted with 0.1% formic acid solution+acetonitrile (80:20, V:V), 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). 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. Results The linear relationship between Nisin A and Nisin Z was good in the range of 0.5 to 50.0 μg/mL, and the correlation coefficient was greater than 0.995. The limits of detection and quantitation were 0.05 to 0.30 mg/kg and 0.15 to 1.00 mg/kg, respectively. The recoveries ranged from 88.8% to 106.2% and the relative standard deviations were 1.32% to 8.85% at the 3 added levels of 1.0, 5.0 and 200.0 mg/kg. Conclusion 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.