Determination of Five Peptide Antibiotics in Pork by HPLC－MS/MS Based on Pass-through Solid Phase Extraction

LIU Zhen; WANG Yu-mei; HU Wen-yan

doi:10.19969/j.fxcsxb.22103102

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Determination of Five Peptide Antibiotics in Pork by HPLC－MS/MS Based on Pass-through Solid Phase Extraction

Scientific Papers | 更新时间：2023-02-28

- Determination of Five Peptide Antibiotics in Pork by HPLC－MS/MS Based on Pass-through Solid Phase Extraction
- Journal of Instrumental Analysis Vol. 42, Issue 2, Pages: 197-203(2023)
- 作者机构：
  
  南京市食品药品监督检验院，江苏南京 211198
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22103102
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刘真,王玉梅,胡文彦.基于通过式固相萃取净化的液相色谱－串联质谱法测定猪肉中5种肽类抗生素[J].分析测试学报,2023,42(02):197-203.

LIU Zhen,WANG Yu-mei,HU Wen-yan.Determination of Five Peptide Antibiotics in Pork by HPLC－MS/MS Based on Pass-through Solid Phase Extraction[J].Journal of Instrumental Analysis,2023,42(02):197-203.
刘真,王玉梅,胡文彦.基于通过式固相萃取净化的液相色谱－串联质谱法测定猪肉中5种肽类抗生素[J].分析测试学报,2023,42(02):197-203. DOI： 10.19969/j.fxcsxb.22103102.

LIU Zhen,WANG Yu-mei,HU Wen-yan.Determination of Five Peptide Antibiotics in Pork by HPLC－MS/MS Based on Pass-through Solid Phase Extraction[J].Journal of Instrumental Analysis,2023,42(02):197-203. DOI： 10.19969/j.fxcsxb.22103102.

摘要

建立了一种基于免活化通过式固相萃取净化技术的液相色谱－串联质谱法（HPLC－MS/MS）用于测定猪肉中5种肽类抗生素（达托霉素、万古霉素、去甲万古霉素、维吉尼亚霉素M1、维吉尼亚霉素S1）。猪肉采用甲醇－2%甲酸（体积比为5∶2）进行提取，经免活化的Captiva EMR－Lipid固相萃取小柱净化后，以Phenomenex Kinetex F5（2.1 mm×100 mm，2.6 μm）色谱柱分离，0.1%甲酸乙腈溶液和0.1%甲酸梯度洗脱。采用电喷雾离子源正离子模式扫描，多反应模式（MRM）监测目标物，内标法定量。结果表明，猪肉中达托霉素在2 ~ 200 ng/mL范围内，万古霉素及去甲万古霉素在5 ~ 500 ng/mL范围内，维吉尼亚霉素M1及维吉尼亚霉素S1在1 ~ 100 ng/mL范围内均呈良好线性关系，相关系数（,r,2,）均大于0.99，5种肽类抗生素的检出限为3 ~ 7.5 μg/kg，定量下限为5 ~ 25 μg/kg。在25、50、250 μg/kg 3个加标水平下的平均回收率为80.2% ~ 102%，日内相对标准偏差（Intra-RSD）为1.3% ~ 7.4%，日间相对标准偏差（Inter-RSD）为2.6% ~ 8.5%。该方法基于Captiva EMR－Lipid固相萃取小柱免活化净化，前处理简便，回收率好，重复性佳，适用于猪肉中5种肽类抗生素的同时检测。

Abstract

A high performance liquid chromatography－tandem mass spectrometric（HPLC－MS/MS） method was developed for the determination of five peptide antibiotics，i.e．daptomycin，vancomycin，norvancomycin，virginiamycin M1 and virginiamycin S1 in pork based on a purification technique with non-activation pass-through solid phase extraction（SPE） column．The pork samples were extracted with methanol－2% formic acid（5∶2，by volume），and purified with a non-activation Captiva EMR－Lipid SPE column．The separation was carried out on a Phenomenex Kinetex F5（2.1 mm × 100 mm，2.6 μm） column by gradient elution，with 0.1% formic acid acetonitrile solution and 0.1% formic acid as mobile phases．The target substances were analyzed in electrospray ion source positive ion mode under multi-reaction monitoring（MRM） mode，and quantified by the internal standard method．Results showed that the calibration curves of five peptide antibiotics in pork were linear（,r,2,>, 0.99） in the range of 2－200 ng/mL for daptomycin，5－500 ng/mL for vancomycin and norvancomycin，and 1－100 ng/mL for virginiamycin M1 and virginiamycin S1．The limits of detection were in the range of 3－7.5 μg/kg，and the limits of quantitation were in the range of 5－25 μg/kg．The recoveries of five peptide antibiotics from negative pork samples at three spiked levels of 25，50，250 μg/kg ranged from 80.2% to 102%，with intra-RSDs and inter-RSDs of 1.3%－7.4% and 2.6%－8.5%，respectively．With the characteristics of simple pretreatment，good recovery and repeatability，this method based on Captiva EMR-lipid SPE column is suitable for the simultaneous analysis of 5 peptide antibiotics in pork.

关键词

肽类抗生素液相色谱－串联质谱法（HPLC－MS/MS）猪肉通过式固相萃取

Keywords

peptide antibioticsliquid chromatography－tandem mass spectrometry（HPLC－MS/MS）porkpass-through solid phase extraction

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