Determination of Vancomycin and Norvancomycin Residues in Shrimps by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2017,36(6):773-777.
Determination of Vancomycin and Norvancomycin Residues in Shrimps by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2017,36(6):773-777.DOI:
建立了虾中万古霉素和去甲万古霉素残留量的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经0.1%甲酸-乙腈(9∶1,体积比)混合溶液提取,乙腈饱和的正己烷除脂,PCX结合Florisil固相萃取柱进行净化后,以乙腈和0.1%甲酸溶液为流动相,经CAPCELL PAK MG-C18色谱柱分离后,采用高效液相色谱-串联质谱在多反应离子监测(MRM)模式进行测定,以双去氯万古霉素作为内标物,内标法定量。结果表明:万古霉素和去甲万古霉素在2~250 ng/mL范围内呈良好的线性关系,相关系数(r2)均大于0.99。在5,25,50 μg/kg加标水平下,万古霉素和去甲万古霉素的平均回收率为87.2%~102%,相对标准偏差为1.3%~8.7%。方法的检出限(LOD)为2.0 μg/kg,定量下限(LOQ)为5.0 μg/kg。该方法灵敏、准确,重复性好,适用于虾类中万古霉素及去甲万古霉素残留量的测定。
Abstract
A new method for the determination of vancomycin and norvancomycin residues in shrimps by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was established.Samples were extracted with 0.1% formic acid-acetonitrile solution,defatted with n hexane saturated with acetonitrile and purified with PCX and Florisil solid phase extraction column.The separation of two targets was carried out on a CAPCELL PAK MG-C18 column by gradient elution with 0.1% formic acid-acetonitrile as mobile phase.The identification of two analytes was performed in multi-reaction monitoring(MRM),and the quantification was carried out by the internal standard method.Dedichloro vancomycin was used as an internal standard.The calibration curves showed good linearities in the range of 2-250 ng/mL with correlation coefficients(r2) greater than 0.99.The detection limits(LOD) of this method were both 2.0 μg/kg,and the limits of quantitation(LOQ) were 5.0 μg/kg.The recoveries of the target compounds at spiked levels of 5,25,50 μg/kg were in the range of 87.2%-102%,with relative standard deviations(RSDs) of 1.3%-8.7%.The results indicated that this method had high sensitivity,accuracy and good reproducibility.It was suitable for the simultaneous determination of ancomycin and norvancomycin residues in shrimps.
关键词
万古霉素去甲万古霉素双去氯万古霉素虾高效液相色谱-串联质谱(HPLC-MS/MS)
Keywords
vancomycinnorvancomycindedichloro vancomycinshrimpshigh performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)