液相色谱–串联质谱法检测猪肉中5种磺胺类药物残留

Simultaneous determination of 5 kinds of sulfonamides residues in pork by liquid chromatography-tandem mass spectrometry

中文关键词:  液相色谱–串联质谱法  猪肉  磺胺类药物  兽药残留

英文关键词:liquid chromatography-tandem mass spectrometry  pork  sulfonamides  residues

中文摘要:

      目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)测定猪肉组织中5种磺胺类药物残留的方法。方法 猪肉样品中的残留药物经乙腈提取后用正己烷去除脂肪, 经氮吹浓缩后用初始流动相溶解定容。用Shim-pack GIST C18色谱柱(150 mm×2.1 mm, 5 μm)分离, 以0.1%甲酸-水溶液和0.1%甲酸-0.1%乙腈溶液为流动相进行梯度洗脱, 质谱采用多反应监测模式对5种磺胺类药物的定量离子和定性离子进行监测, 以外标法定量。结果 本方法在6.5 min内完成5种目标化合物的分离分析。5种磺胺类药物在0.5~50 μg/kg范围内线性关系良好, 相关系数r2为0.9980~0.9999, 在5、10、20 μg/L添加水平的回收率为(59.96?1.71)%~(96.09?0.54)%,日内相对标准偏差(relative standard deviation, RSD)为1.32%~2.99%, 日间RSD为0.41%~0.94%(n=5), 方法定量限均小于5 μg/kg。结论 该方法操作快速、灵敏、准确, 可用于猪肉组织中5种磺胺类药物的残留检测。

英文摘要:

      Objective To established a method for simultaneous determination of 5 kinds of sulfonamides residues in pork by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The residues in the pork sample were extracted with acetonitrile and the fat was removed with n-hexane, the sample was concentrated by nitrogen blowing, and dissolved to volume with initial mobile phase. The liquid was performed on a Shim-pack GIST C18 chromatographic column (150 mm×2.1 mm, 5 μm) with gradient elution of 0.1% formic acid-water solution and 0.1% formic acid-acetonitrile solution. The mass spectrometry was carried out with multiple reaction monitoring to monitor the quantitative ions and qualitative ions of 5 kinds of sulfonamides, and quantified by external standard solution. Results This method completed the separation analysis of 5 target compounds within 6.5 min. Five kind of sulfonamides showed good linear relationships in the concentration range of 0.5-50 μg/kg with the correlation coefficients of 0.9980-0.9999. The recoveries at 3 spiked levels (5, 10, and 20 μg/L) were (59.96?1.71)%- (96.09?0.54)%, with intra-day relative standard deviation (RSD) of 1.32%-2.99%, and intraday RSD of 0.41%-0.94% (n=5). The limits of quantitation for 5 kinds of sulfonamides were less than 5 μg/kg. Conclusion The method is rapid, sensitive and accurate, which is suitable for the determination of 5 kind of sulfonamides in pork tissues.