SPE净化-液质联用测定氨基糖苷类药物残留
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摘要
建立了生鲜乳中新霉素、链霉素、大观霉素、卡那霉素等4种氨基糖苷类抗生素残留的超高效液相色谱-串联质谱(UPLCMS/MS)检测方法。样品经质量分数为5%的三氯乙酸溶液提取,再经弱阳离子固相萃取柱净化;采用CORTECS HILIC液相色谱柱分离,电喷雾串联四级杆质谱检测。对样品的前处理、液相色谱及质谱条件进行了优化。结果表明:4种物质在质量浓度为100～2000μg/L范围内线性良好,方法的检出限在10～20μg/kg之间,加标回收率在74.5%～95.4%之间。该方法灵敏、准确、简单,适合生乳中对这4种氨基糖苷类抗生素的同时检测。
A method of UPLC-MS/MS was developed tu determine four aminglycoside(Neomycin,Streptomycin,Kanamycin,Streptomyces) residues in milk.The sample was extracted by 5% trichloroacetic acid solution and purified by weak cationic solid extraction column.CORTECS HILIC liquid chromatography column was used for separation and electrospray tandem quadruple mass spectrometry detection.The results showed that the linearity of the four substances within the range of 100～2 000 μg/L was good,and the detection limit of the method was between 10～20 μg/kg,and the standard recovery rate was between 74.5%～95.4%.The method is sensitive,accurate and simple,and is suitable for simultaneous detection of these 4 antibiotics in milk.
A method of UPLC-MS/MS was developed tu determine four aminglycoside(Neomycin,Streptomycin,Kanamycin,Streptomyces) residues in milk.The sample was extracted by 5% trichloroacetic acid solution and purified by weak cationic solid extraction column.CORTECS HILIC liquid chromatography column was used for separation and electrospray tandem quadruple mass spectrometry detection.The results showed that the linearity of the four substances within the range of 100～2 000 μg/L was good,and the detection limit of the method was between 10～20 μg/kg,and the standard recovery rate was between 74.5%～95.4%.The method is sensitive,accurate and simple,and is suitable for simultaneous detection of these 4 antibiotics in milk.
引文
[1]李俊锁,邱明月,王超.兽药残留分析[M]上海:上海科学技术出版社.2002.
[2]TANAKA N,HOOPER R.Aminoglycoside Antibiotics[M].Berlin:Springer-Verlag,1982:221.
[3]周自永,王世祥.新编常用药物手册[M].出版.北京:金盾出版社,1994:446.
[4]中华人民共和国农业部公告第235号.
[5]蔡金华,刘雅妮,顾欣,等.链霉素在牛奶中残留的微生物学检测方法[J].中国兽医杂志,2004,38(11):7-9.
[6]黄耀凌,刘智宏,叶妮,等.ELISA法检测牛奶中链霉素残留量[J].中国乳品工业,2007,35(2):54-56.
[7]孙雷,张俪,黄耀凌,等.超高效液相色谱-串联质谱法检测动物源性食品中8种氨基糖苷类药物残留[J].色谱,2012,30(11):1143-1147.
[8]叶磊海,钟世欢,叶佳明,等.LC-MS-MS法同时测定动物肌肉组织和牛奶中10种氨基糖苷类药物的方法优化研究[J].医药化工,2016,42(12):107-108.
[9]杨碧霞,王炼,骆春迎,等.分子印迹固相萃取LC-MS/MS法同时测定蜂蜜中11种氨基糖苷类抗生素[J].现代预防医学,2017,44(7):1285-1289.
[10]中华人民共和国国家标准,GB/T 21323-2007动物组织中氨基糖苷类药物残留的测定高效液相色谱-质谱/质谱法.
[11]龚强,丁利,朱绍华,等.高效液相色谱-串联质谱法检测乳制品中10种氨基糖苷类抗生素残留[J].色谱,2012,30(11):1143-1147.
[12]王帅兵,曲斌,狄世伟,等亲水作用色谱-高分辨质谱测定生鲜牛乳中7种氨基糖苷类药物残留[J].动物医学进展,2017,38(9):67-72.
[13]刘雪红,张秀琴,侯颖,等.超高效液相色谱-串联质谱法检测牛奶中7种氨基糖苷类药物残留[J].中国兽药杂志,2015,49(3):48-52.
[14]戴辉,孟晶,等.基于HPLC-MS检测食品中新霉素和潮霉素B的残留量[J].山西农经,2016,18:97-98.
[2]TANAKA N,HOOPER R.Aminoglycoside Antibiotics[M].Berlin:Springer-Verlag,1982:221.
[3]周自永,王世祥.新编常用药物手册[M].出版.北京:金盾出版社,1994:446.
[4]中华人民共和国农业部公告第235号.
[5]蔡金华,刘雅妮,顾欣,等.链霉素在牛奶中残留的微生物学检测方法[J].中国兽医杂志,2004,38(11):7-9.
[6]黄耀凌,刘智宏,叶妮,等.ELISA法检测牛奶中链霉素残留量[J].中国乳品工业,2007,35(2):54-56.
[7]孙雷,张俪,黄耀凌,等.超高效液相色谱-串联质谱法检测动物源性食品中8种氨基糖苷类药物残留[J].色谱,2012,30(11):1143-1147.
[8]叶磊海,钟世欢,叶佳明,等.LC-MS-MS法同时测定动物肌肉组织和牛奶中10种氨基糖苷类药物的方法优化研究[J].医药化工,2016,42(12):107-108.
[9]杨碧霞,王炼,骆春迎,等.分子印迹固相萃取LC-MS/MS法同时测定蜂蜜中11种氨基糖苷类抗生素[J].现代预防医学,2017,44(7):1285-1289.
[10]中华人民共和国国家标准,GB/T 21323-2007动物组织中氨基糖苷类药物残留的测定高效液相色谱-质谱/质谱法.
[11]龚强,丁利,朱绍华,等.高效液相色谱-串联质谱法检测乳制品中10种氨基糖苷类抗生素残留[J].色谱,2012,30(11):1143-1147.
[12]王帅兵,曲斌,狄世伟,等亲水作用色谱-高分辨质谱测定生鲜牛乳中7种氨基糖苷类药物残留[J].动物医学进展,2017,38(9):67-72.
[13]刘雪红,张秀琴,侯颖,等.超高效液相色谱-串联质谱法检测牛奶中7种氨基糖苷类药物残留[J].中国兽药杂志,2015,49(3):48-52.
[14]戴辉,孟晶,等.基于HPLC-MS检测食品中新霉素和潮霉素B的残留量[J].山西农经,2016,18:97-98.