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Chromatographic separation was accomplished on a BEH C18 column(2.1 mm×100 mm,1.7 μm chromatographic column) . The mass spectrometer conducted real-time detection through the positive ion multiple reaction monitoring(MRM)mode and completed quantitative analysis by external standard method combined with the matrix-matched standard curve.[Result] Within the concentration range of 1~80 ng/mL,the four nitroimidazole drugs had a good linearity,with correlation coefficients(r)were all greater than 0.998.The average recovery rate was 83.2%~106.8% at three spiked levels(1.0 μg/kg,2.0 μg/kg and 10.0 μg/kg),the relative standard deviation(RSD)was 1.8%~20.1%.The detection limit of the method 1 μg/kg.[Conclusion] This method is simple to operate,sensitive and accurate,and is suitable for the detection of nitroimidazole drugs(metronidazole,tinidazole,dimedinidazole,ronidazole) residues in goat milk., authors=YI Hongbo, YANG Jian*, ZHANG Lijun, LU Gang, DONG Liya, YANG Ying, LI Zhenxia, authorsList=YI Hongbo, YANG Jian, ZHANG Lijun, LU Gang, DONG Liya, YANG Ying, LI Zhenxia, authorCompany=Inner Mongolia Mengniu Dairy Industrial Co.,Ltd.,Hohhot Inner Mongolia 011500, correspAuthors=null, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1321421076110889454, articleId=1321421074332504556, tenantId=1146029695717560320, journalId=1296801528146919473, language=CN, title=超高效液相色谱-串联质谱法检测羊奶中硝基咪唑类药物残留量研究, columnId=1297134032135938673, journalTitle=中国乳业, columnName=质量安全, runingTitle=null, highlight=null, articleAbstract=[目的]研发一项采用超高效液相色谱-串联质谱(UHPLC-MS/MS)技术精确检测羊奶中硝基咪唑类药物(包含甲硝唑、地美硝唑、洛硝哒唑及替硝唑等)残留量的方法。[方法]采用乙腈与柠檬酸缓冲液提取羊奶样品,随后用MCX阳离子交换固相萃取柱和PEP-2聚合物固相萃取柱净化处理。氮吹洗脱液至近干后,用含0.1%甲酸的水甲醇溶液定容至1 mL,用流相0.1%甲酸水溶液和乙腈渐变洗脱,色谱分离采用BEH C18柱(2.1 mm×100 mm,1.7 μm)。质谱仪通过正离子多反应监测(MRM)模式实时检测,并运用外标法结合基质匹配标准曲线完成定量分析。[结果]在1~80 ng/mL浓度范围内,4 种硝基咪唑类药物残留量具有较好的线性关系,相关系数(r)均大于0.998;平均回收率在3 个加标水平下(1 μg/kg、2 μg/kg和10 μg/kg)为83.2%~106.8%,相对标准偏差为1.8%~20.1%,方法检出限为1 μg/kg。[结论]该方法操作简单、灵敏、准确,适用于羊奶中硝基咪唑类药物残留量的检测。, authors=仪虹伯, 杨戬*, 张利俊, 逯刚, 董立雅, 杨颖, 李振侠, authorsList=仪虹伯, 杨戬, 张利俊, 逯刚, 董立雅, 杨颖, 李振侠, authorCompany=内蒙古蒙牛乳业集团股份有限公司,内蒙古呼和浩特 011500, correspAuthors=*杨戬(1992-),男,内蒙古呼和浩特人,本科,工程师,研究方向为乳品快速检测技术开发及应用。, authorNote=仪虹伯(1988-),女,内蒙古呼和浩特人,蒙古族,硕士,工程师,研究方向为乳品检验技术;张利俊(1985-),男,内蒙古呼和浩特人,本科,工程师,研究方向为乳品检验技术;逯刚(1978-),男,内蒙古呼和浩特人,硕士,高级工程师,研究方向为食品质量安全研究;董立雅(1987-),女,北京人,硕士,工程师,研究方向为食品质量安全研究;杨颖(1986-),女,内蒙古扎兰屯人,本科,中级工程师,研究方向为食品安全和追溯系统;李振侠(1997-),女,内蒙古包头人,本科,助理工程师,研究方向为乳品检测。, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=S/uBMPPCR3AATi+mjgQKUQ==, pdfFileSize=2130801, pdfExtLink=null, richHtmlUrl=null, 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[11] 张丽媛,周剑,王敏,等.液相色谱-串联质谱法测定鸡肉和鸡蛋中3 种硝基咪唑类药物[J].食品安全质量检测学报,2019,10(14):4508-4514.
[12] 汤水粉,钱卓真,位绍红,等.高效液相色谱-串联质谱法测定水产品中硝基咪唑类药物残留量[J].渔业研究,2022,44(1):60-68.
[13] 马华威,赖艳玲,韦志.羊乳发展前景及广西羊乳产业发展潜力[J].中国乳业,2016(2):34-37.
[14] 金嫘,白丽娟,彭小雨,等.采用电子鼻检测羊奶中的牛奶掺入[J].食品与发酵工业,2015,41(4):165-168.
[15] 董梅,李璐,罗叶丽,等.UPLC-MS/MS测定羊奶中氯霉素、甲砜霉素、氟苯尼考[J].食品工业,2022,43(9):297-300.
[16] 杨霄,万译文,黄华伟,等.分散固相萃取-超高效液相色谱-串联质谱法测定水产品中5 种硝基咪唑类和6 种苯二氮卓类药物[J].色谱,2022,40(7):625-633.
[17] 中华人民共和国国家质量监督检验检疫总局.SN/T2624—2010 动物源性食品中多种碱性药物残留量的检测方法液相色谱-质谱/质谱法[S].
[18] 徐媛原,张微,张杨,等.超高效液相色谱-串联质谱法测定水产品中硝基咪唑类药物及其代谢物[J].饲料博览,2022(5):59-63.
[19] 朱姗姗,吴澎,徐双双,等.基于色谱-质谱法分析食品中硝基咪唑类药物残留的研究进展[J].食品工业科技,2020,41(22):326-334.
[20] 中华人民共和国国家质量监督检验检疫总局.GB/T 27417—2017 合格评定化学分析方法确认和验证指南[S].)
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中国乳业 | 质量安全 2025,(8): 88-93
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中国乳业 |质量安全 2025 , (8) : 88 -93
超高效液相色谱-串联质谱法检测羊奶中硝基咪唑类药物残留量研究
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仪虹伯, 杨戬*, 张利俊, 逯刚, 董立雅, 杨颖, 李振侠
作者信息
    内蒙古蒙牛乳业集团股份有限公司,内蒙古呼和浩特 011500
通讯作者:
*杨戬(1992-),男,内蒙古呼和浩特人,本科,工程师,研究方向为乳品快速检测技术开发及应用。
作者简介:
仪虹伯(1988-),女,内蒙古呼和浩特人,蒙古族,硕士,工程师,研究方向为乳品检验技术;张利俊(1985-),男,内蒙古呼和浩特人,本科,工程师,研究方向为乳品检验技术;逯刚(1978-),男,内蒙古呼和浩特人,硕士,高级工程师,研究方向为食品质量安全研究;董立雅(1987-),女,北京人,硕士,工程师,研究方向为食品质量安全研究;杨颖(1986-),女,内蒙古扎兰屯人,本科,中级工程师,研究方向为食品安全和追溯系统;李振侠(1997-),女,内蒙古包头人,本科,助理工程师,研究方向为乳品检测。
Study on the Detection of Nitroimidazole Drug Residues in Goat Milk by Ultra-performance Liquid Chromatography-tandem Mass Spectrometry in Series
  • YI Hongbo, YANG Jian*, ZHANG Lijun, LU Gang, DONG Liya, YANG Ying, LI Zhenxia
  • Affiliations
      Inner Mongolia Mengniu Dairy Industrial Co.,Ltd.,Hohhot Inner Mongolia 011500
    doi: 10.12377/1671-4393.25.08.14
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    [目的]研发一项采用超高效液相色谱-串联质谱(UHPLC-MS/MS)技术精确检测羊奶中硝基咪唑类药物(包含甲硝唑、地美硝唑、洛硝哒唑及替硝唑等)残留量的方法。[方法]采用乙腈与柠檬酸缓冲液提取羊奶样品,随后用MCX阳离子交换固相萃取柱和PEP-2聚合物固相萃取柱净化处理。氮吹洗脱液至近干后,用含0.1%甲酸的水甲醇溶液定容至1 mL,用流相0.1%甲酸水溶液和乙腈渐变洗脱,色谱分离采用BEH C18柱(2.1 mm×100 mm,1.7 μm)。质谱仪通过正离子多反应监测(MRM)模式实时检测,并运用外标法结合基质匹配标准曲线完成定量分析。[结果]在1~80 ng/mL浓度范围内,4 种硝基咪唑类药物残留量具有较好的线性关系,相关系数(r)均大于0.998;平均回收率在3 个加标水平下(1 μg/kg、2 μg/kg和10 μg/kg)为83.2%~106.8%,相对标准偏差为1.8%~20.1%,方法检出限为1 μg/kg。[结论]该方法操作简单、灵敏、准确,适用于羊奶中硝基咪唑类药物残留量的检测。
    羊奶  /  硝基咪唑类药物  /  超高效液相色谱-串联质谱法
    [Objective] Develop a technology for the precise detection of nitroimidazole drug residues in goat milk using ultra-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS),including metronidazole,dimetridazole,ronidazole and tinidazole,etc.[Method] The Goat milk samples were extracted with acetonitrile and citric acid buffer solution,and then purified by MCX cation exchange solid-phase extraction column and PEP-2 polymer solid-phase extraction column.After the nitrogen purge eluent was nearly dry,it was made up to 1 mL with a water-methanol containing 0.1% formic acid, and eluted gradually with 0.1% formic acid aqueous solution and acetonitrile in the flow phase. Chromatographic separation was accomplished on a BEH C18 column(2.1 mm×100 mm,1.7 μm chromatographic column) . The mass spectrometer conducted real-time detection through the positive ion multiple reaction monitoring(MRM)mode and completed quantitative analysis by external standard method combined with the matrix-matched standard curve.[Result] Within the concentration range of 1~80 ng/mL,the four nitroimidazole drugs had a good linearity,with correlation coefficients(r)were all greater than 0.998.The average recovery rate was 83.2%~106.8% at three spiked levels(1.0 μg/kg,2.0 μg/kg and 10.0 μg/kg),the relative standard deviation(RSD)was 1.8%~20.1%.The detection limit of the method 1 μg/kg.[Conclusion] This method is simple to operate,sensitive and accurate,and is suitable for the detection of nitroimidazole drugs(metronidazole,tinidazole,dimedinidazole,ronidazole) residues in goat milk.
    goat milk  /  nitroimidazole drug  /  ultra-performance liquid chromatography-tandem mass spectrometry
    仪虹伯, 杨戬, 张利俊, 逯刚, 董立雅, 杨颖, 李振侠. 超高效液相色谱-串联质谱法检测羊奶中硝基咪唑类药物残留量研究. 中国乳业, 2025 , (8) : 88 -93 . DOI: 10.12377/1671-4393.25.08.14
    YI Hongbo, YANG Jian, ZHANG Lijun, LU Gang, DONG Liya, YANG Ying, LI Zhenxia. Study on the Detection of Nitroimidazole Drug Residues in Goat Milk by Ultra-performance Liquid Chromatography-tandem Mass Spectrometry in Series[J]. China Dairy, 2025 , (8) : 88 -93 . DOI: 10.12377/1671-4393.25.08.14

      国家重点研发计划项目(2022YFD1301005)

    参考文献 引证文献
    排序方式:
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    [11] 张丽媛,周剑,王敏,等.液相色谱-串联质谱法测定鸡肉和鸡蛋中3 种硝基咪唑类药物[J].食品安全质量检测学报,2019,10(14):4508-4514.
    [12] 汤水粉,钱卓真,位绍红,等.高效液相色谱-串联质谱法测定水产品中硝基咪唑类药物残留量[J].渔业研究,2022,44(1):60-68.
    [13] 马华威,赖艳玲,韦志.羊乳发展前景及广西羊乳产业发展潜力[J].中国乳业,2016(2):34-37.
    [14] 金嫘,白丽娟,彭小雨,等.采用电子鼻检测羊奶中的牛奶掺入[J].食品与发酵工业,2015,41(4):165-168.
    [15] 董梅,李璐,罗叶丽,等.UPLC-MS/MS测定羊奶中氯霉素、甲砜霉素、氟苯尼考[J].食品工业,2022,43(9):297-300.
    [16] 杨霄,万译文,黄华伟,等.分散固相萃取-超高效液相色谱-串联质谱法测定水产品中5 种硝基咪唑类和6 种苯二氮卓类药物[J].色谱,2022,40(7):625-633.
    [17] 中华人民共和国国家质量监督检验检疫总局.SN/T2624—2010 动物源性食品中多种碱性药物残留量的检测方法液相色谱-质谱/质谱法[S].
    [18] 徐媛原,张微,张杨,等.超高效液相色谱-串联质谱法测定水产品中硝基咪唑类药物及其代谢物[J].饲料博览,2022(5):59-63.
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    [20] 中华人民共和国国家质量监督检验检疫总局.GB/T 27417—2017 合格评定化学分析方法确认和验证指南[S].
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    2种不同金属材料的力学参数
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    Number of
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    Number of
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    Percentage of
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    种数
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    占总种数比例
    Percentage of total
    species (%)
    鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
    小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
    多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
    红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
    小菇属 Mycena 11 5.26
    光柄菇属 Pluteus 5 2.39
    红菇属 Russula 17 8.13
    栓菌属 Trametes 5 2.39
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