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

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 UPLC~（TM） BEH C_（18）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4~5000μg/L浓度范围内线性关系良好,相关系数（...

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Bibliographic Details
Published in食品安全质量检测学报 Vol. 7; no. 12; pp. 4759 - 4765
Main Author 綦艳 李锦清 黄翠莉 周勇 庄艺协
Format Journal Article
LanguageChinese
Published 广东产品质量监督检验研究院，国家食品质量监督检验中心 广东，佛山 528300 2016
Subjects
万古霉素
去甲万古霉素
固相萃取
超高效液相色谱-串联质谱法
万古霉素
去甲万古霉素
norvancomycin
超高效液相色谱-串联质谱法
ultra performance liquid chromatography-tandem mass spectrometry
solid-phase extraction
固相萃取
vancomycin
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ISSN2095-0381

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Summary: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 UPLC~（TM） BEH C_（18）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4~5000μg/L浓度范围内线性关系良好,相关系数（r~2）均大于0.99。方法检出限分别为0.5μg/kg和0.8μg/kg。在5、20和50μg/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。
Bibliography: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 4~5000μg/L withr2〉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 50μg/kg we
ISSN:2095-0381