分散固相萃取-超高效液相色谱-串联质谱法测定饲料中的多肽类抗生素OACSTPCD
Determination of polypeptide antibiotics in feed by dispersive solid-phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry
试验基于分散固相萃取净化结合超高效液相色谱-串联质谱法,建立一种同时测定饲料中16种多肽类抗生素(PPTs)的定量分析方法.样品经1%三氯乙酸(aq)-甲醇溶液提取,十八烷基硅胶(C18)分散固相萃取净化后上机测定.在电喷雾正电离模式下,使用多反应监测(MRM)模式,基质匹配校正曲线定量.结果显示,PPTs在相应的浓度范围内线性关系良好,相关系数(R2)大于0.99,检出限为0.4~12.1 μg/kg,定量限为1.4~40.4μg/kg.PPTs在饲料中的平均回收率(n=6)为80.0%~114.4%,相对标准偏差(RSD)为2.33%~9.51%.研究表明,该方法操作简单、准确可靠、灵敏度高、分析时间短且重现性高,可广泛应用于饲料中16种PPTs的快速筛查和常规监测.
A quantitative method for the simultaneous determination of 16 peptide antibiotics(PPTs)in feed was established based on dispersed solid-phase extraction and purification combined with ultra-performance liquid chromatography-tandem mass spectrometry.The samples were extracted by 1%trichloroacetic acid(aq)-methanol solution,and purified by dispersed solid-phase extraction of octadecyl silica gel(C18)before being measured on the machine.In electrospray positive ionization mode,multiple reaction monitoring(MRM)mode was used to quantify the matrix-matched correction curve.The results showed that the linear relationship of PPTs is good in the corresponding concentration range,the correlation coefficient(R2)was larger than 0.99,the detection limit was 0.4~12.1 μg/kg,and the quantification limit was 1.4~40.4 μg/kg.The average recovery rate(n=6)and relative standard deviation(RSD)of PPTs in feed were 80.0%~114.4%,and the relative standard deviation(RSD)was 2.33%~9.51%.The results show that the method is simple,accurate and reliable,with high sensitivity,short analysis time and high reproducibility,and can be widely used in the rapid screening and routine monitoring of 16 PPTs in feed.
黄燕;李燕妹;陈言凯;梁敏;冯丽凤;陈何燊;林浩学;蔡小明
福建省产品质量检验研究院国家加工食品质量检验检测中心(福州),福建福州 350000
畜牧业
超高效液相色谱-串联质谱多肽类抗生素饲料分散固相萃取
ultra-performance liquid chromatography-tandem mass spectrometrypeptide antibioticsfeeddispersive solid-phase extraction
《饲料研究》 2024 (005)
109-116 / 8
福建省产品质量检验研究院科研项目(项目编号:KY202115A)
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