超高效液相色谱-串联质谱法测定动物源性食品中万古霉素和去甲万古霉素的残留量

Determination of vancomycin and norvancomycin residues in animal derived food by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  固相萃取  万古霉素  去甲万古霉素

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  solid-phase extraction  vancomycin  norvancomycin

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定动物源性食品中万古霉素和去甲万古霉素的残留量。方法 样品经甲醇-水溶液提取, 二氯甲烷去除脂肪等杂质, 经Strata-X-C SPE小柱净化, ACQUITY UPLCTM BEH C18色谱柱分离, 以乙腈和0.1 %甲酸-水(V:V)作为流动相进行梯度洗脱。质谱采用电喷雾离子源在多反应监测模式下进行测定, 以外标法定量。结果 万古霉素和去甲万古霉素在4~5000 μg/L浓度范围内线性关系良好, 相关系数(r2)均大于0.99。方法检出限分别为0.5 μg/kg和0.8 μg/kg。在5、20和50 μg/kg 3个水平上的加标回收率为77.2 %~90.2 %, 相对标准偏差均小于10 %。结论 该方法准确灵敏, 适用于动物源性食品中万古霉素和去甲万古霉素残留量的测定。

英文摘要:

      Objective To establish a method for the simultaneous determination of vancomycin and norvancomycin residues in animal derived food by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted by a mixed solution of methanol and water, removed impurities such as fat with methylene chloride, and further purified by Strata-X-C solid-phase extraction (SPE). The target compounds were separated by ACQUITY UPLCTM BEH C18 column with acetonitrile and 0.1%formic acid-water solution(V:V) as mobile phases for gradient elution. The mass spectrometry was carried out by means of multiple reaction monitoring (MRM) in electrospray ionization mode (ESI) with external standard for quantification. Results Vancomycin and norvancomycin had good linear relationships in the range of 4~5000 μg/L with r2>0.99. The limits of detection of vancomycin and norvancomycin were respectively 0.5 and 0.8 μg/kg. The average recoveries of the two target compounds spiked at 5, 20 and 50 μg/kg were ranged from 77.2% to 90.2%, with the relative standard deviations (RSDs) less than 10%. Conclusion The proposed method is accurate and sensitive, which can be used for the determination of vancomycin and norvancomycin in animal derived food.