超高效液相色谱—串联质谱法测定牛奶中9种磺胺类药物残留量
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- 英文论文题名：Determination of nine Sulfonamides in milk by UPLC-MS/MS
- 论文作者：陈娟 ; 吴春燕 ; 李莉 ; 马岩 ; 杨俊华 ; 史宁花 ; 陈建蓉 ; 陈海燕
- 年：2016
- 作者机构：宁夏兽药饲料监察所;
- 论文关键词：磺胺类药物 ; 牛奶 ; 残留 ; 超高效液相色谱-串联质谱法
- 英文论文关键词：Sulfonamides ; milk ; residues ; UPLC-MS/MS
- 会议召开时间：2016-09-18
- 会议录名称：中国畜牧兽医学会动物药品学分会第五届全国会员代表大会暨2016年学术年会论文集
- 语种：中文
- 分类号：S859.84;O657.63
- 学会代码：ZGXJ
- 会议名称：中国畜牧兽医学会动物药品学分会第五届全国会员代表大会暨2016年学术年会
- 会议地点：中国四川成都
- 主办单位：中国畜牧兽医学会动物药品学分会
- 学会名称：中国畜牧兽医学会
- 页数：5
- 文件大小：545k
- 原文格式：O
- 会议级别：全国
摘要
建立了牛奶中9种磺胺类药物残留检测的超高效液相色谱—串联质谱方法(UUPLC-MS/MS)。样品用乙腈提取,吹干后用20%乙腈溶解,供超高效液相色谱—串联质谱法分析。液相色谱条件为:色谱柱为WatersBEH C18柱(50mm×2.1mm,1.7μm);流动相为乙腈-0.1%甲酸水溶液,梯度洗脱;柱温为40℃;流速为0.3mL/min;进样量:2νL。质谱条件为:电喷雾离子源(ESI~+),多反应监测(MRM)方式采集,外标法定量。结果表明:在0.625-50μg/L的系列浓度范围内,9种磺胺类药物药物的相关系数R~2>0.996;方法检测限为5μg/L,定量限为10μg/L;从10、50、100μg/三个添加浓度检测结果可以看出,方法的平均回收率在85.7—106.6%,,批内、批间RSD均<15%。本方法简便快捷,定性、定量准确,结果重复性好,灵敏度高,可以满足兽药残留分析的要求。
A UPLC-MS/MS method was established for the determination of nine Sulfonamides in milk.The samples were extracted by acetonitril,dissolved by 5%acetonitril after evaporation and determined on UPLC-MS/MS.UPLC condition:the chromatography column was Waters BEH C18 column of 50mm×2.1mm,1.7μm,mobile phase was acetonitril and water;column temprerature was 40℃;flow rate was 0.3 mL/min;injetion volume was 2μL.Mass spectrometry condition:ESI~+ and MRM mode.The calibration curves were good linear between the peak areas and concentrations from 0.625-50μg/L,the correlation coefficient R~2>0.996.The detection limit of the method was 5μg/L,and the limit of quantification was 10μg/L.The average recoveries from spiked milk at the three concentrations of 10、50、100μg/L ranged from 85.7%-106.6%,and intra-and inter-batch variation coefficients were less than 15%.The method was simple and rapid,and it was satisfied to detect veterinary drug residues in animal derived food.
A UPLC-MS/MS method was established for the determination of nine Sulfonamides in milk.The samples were extracted by acetonitril,dissolved by 5%acetonitril after evaporation and determined on UPLC-MS/MS.UPLC condition:the chromatography column was Waters BEH C18 column of 50mm×2.1mm,1.7μm,mobile phase was acetonitril and water;column temprerature was 40℃;flow rate was 0.3 mL/min;injetion volume was 2μL.Mass spectrometry condition:ESI~+ and MRM mode.The calibration curves were good linear between the peak areas and concentrations from 0.625-50μg/L,the correlation coefficient R~2>0.996.The detection limit of the method was 5μg/L,and the limit of quantification was 10μg/L.The average recoveries from spiked milk at the three concentrations of 10、50、100μg/L ranged from 85.7%-106.6%,and intra-and inter-batch variation coefficients were less than 15%.The method was simple and rapid,and it was satisfied to detect veterinary drug residues in animal derived food.
引文
[1]中华人民共和国国家标准农业部781号公告-12-2006[S].
[2]胡海燕,徐倩,孙雷,等潴肉和牛奶中10种磺胺类药物残留检测超高效液相色谱法研究[J].中国兽药杂志,2009,43(8):1-4.
[3]吴银良,赵莉,刘勇军,等.固相萃取-高效液色谱法同时测定牛奶中残留的9种磺胺药物[J].色谱,2008,25(5):728-731.
[2]胡海燕,徐倩,孙雷,等潴肉和牛奶中10种磺胺类药物残留检测超高效液相色谱法研究[J].中国兽药杂志,2009,43(8):1-4.
[3]吴银良,赵莉,刘勇军,等.固相萃取-高效液色谱法同时测定牛奶中残留的9种磺胺药物[J].色谱,2008,25(5):728-731.