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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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
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ISSN2095-0381

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Abstract 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。
AbstractList 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 UPLCTM BEH C18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(r2)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。
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。
Abstract_FL 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 were ranged from 77.2% to 90.2%, with the relative standard deviations (RSDs) less than 10%.Conclusion The proposed method is accurate and sensitive, which can be used for the determination of vancomycin and norvancomycin in animal derived food.
Author 綦艳 李锦清 黄翠莉 周勇 庄艺协
AuthorAffiliation 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
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Author_FL HUANG Cui-Li
ZHUANG Yi-Xie
QI Yan
ZHOU Yong
LI Jin-Qing
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DocumentTitleAlternate Determination of vancomycin and norvancomycin residues in animal derived food by ultra performance liquid chromatography-tandem mass spectrometry
DocumentTitle_FL Determination of vancomycin and norvancomycin residues in animal derived food by ultra performance liquid chromatography-tandem mass spectrometry
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Issue 12
Keywords 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
Language Chinese
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Notes 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
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PublicationTitle 食品安全质量检测学报
PublicationTitleAlternate Journal of Food Safety and Quality
PublicationTitle_FL Journal of Food Safety & Quality
PublicationYear 2016
Publisher 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
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Snippet 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...
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...
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StartPage 4759
SubjectTerms 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
Title 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
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