亲水作用色谱-质谱法同时检测鱼肉中 链霉素和双氢链霉素残留

Simultaneous determination of streptomycin and dihydrostreptomycin residues in fish using hydrophilic interaction liquid chromatography coupled with electrospray ionization tandem mass spectrometry

中文关键词:  链霉素  双氢链霉素  亲水作用色谱  质谱法  鱼肉

英文关键词:streptomycin  dihydrostreptomycin  hydrophilic interaction liquid chromatography  electrospray ionization tandem mass spectrometry  fish

中文摘要:

      目的 建立一种亲水作用色谱串联质谱技术同时检测鱼肉中链霉素和双氢链霉素残留的分析方法。方法 以鱼肉为原料, 样品经磷酸盐缓冲溶液提取, 固相萃取柱净化后, 采用亲水作用色谱柱分离, 在正离子模式下以电喷雾电离串联质谱进行测定, 外标法定量。结果 链霉素和双氢链霉素在2.0?50 μg/L质量浓度范围内线性关系良好, 在10、20、50 μg/kg三个加标水平下, 方法的回收率为80.2%?97.1%, 相对标准偏差为3.3%?7.2%。结论 该方法简便、快速、实用、准确, 各项技术指标满足国内外法规的要求, 可用于鱼肉中链霉素和双氢链霉素残留的确证检测。

英文摘要:

      Objective To establish a method for determination of streptomycin and dihydrostreptomycin residues in fish by hydrophilic interaction liquid chromatography coupled with electrospray ionization tandem mass spectrometry. Methods Streptomycin and dihydrostreptomycin were extracted from samples with phosphate buffer solution, and then detected by HPLC-MS/MS in positive mode with external standard method after being cleaned up with ion exchange SPE column. Results The method showed a good linear-ity over the range of 2.0~50 μg/L for streptomycin and dihydrostreptomycin residues. The recoveries were from 80.2% to 97.1% at three spiked level of 10, 20, and 50 μg/kg with relative standard deviation of 3.3%?7.2%. Conclusion The method is simple, rapid, and accurate, and its performance can meet the re-quirements of the domestic and international legislation. It is suitable for the detection of streptomycin and dihydrostreptomycin residues in fish.