| 高效液相色谱-串联质谱法测定虾中万古霉素及去甲万古霉素残留量 |
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| 基金项目:农业行业标准制定和修定农产品质量安全项目(2130109) |
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| 中文摘要: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。 |
| 中文关键词: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) |
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| Determination of Vancomycin and Norvancomycin Residues in Shrimps by High Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| 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. |
| Key Words:vancomycin norvancomycin dedichloro vancomycin shrimps high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) |
| 引用本文：薛婷婷，黄冬梅，严敏鸣，韩峰,王政，史永富,田良良.高效液相色谱-串联质谱法测定虾中万古霉素及去甲万古霉素残留量[J].分析测试学报,2017,36(6):773-777. |
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