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 |
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Main Author | |
Format | Journal Article |
Language | Chinese |
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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Subjects | |
Online Access | Get full text |
ISSN | 2095-0381 |
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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。 |
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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 |
AuthorAffiliation_xml | – name: 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 |
Author_FL | HUANG Cui-Li ZHUANG Yi-Xie QI Yan ZHOU Yong LI Jin-Qing |
Author_FL_xml | – sequence: 1 fullname: QI Yan – sequence: 2 fullname: LI Jin-Qing – sequence: 3 fullname: HUANG Cui-Li – sequence: 4 fullname: ZHOU Yong – sequence: 5 fullname: ZHUANG Yi-Xie |
Author_xml | – sequence: 1 fullname: 綦艳 李锦清 黄翠莉 周勇 庄艺协 |
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Copyright | Copyright © Wanfang Data Co. Ltd. All Rights Reserved. |
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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 |
EndPage | 4765 |
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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 |
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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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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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