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分散固相萃取-高效液相色谱-串联质谱法测定水产品中19种喹诺酮类兽药残留
引用本文:曹军.分散固相萃取-高效液相色谱-串联质谱法测定水产品中19种喹诺酮类兽药残留[J].中国兽药杂志,2011,45(7):21-25.
作者姓名:曹军
作者单位:1. 盐城出入境检验检疫局,江苏盐城,224002
2. 南通市水产品检测中心,江苏南通,226006
基金项目:国家质检总局科研计划项目(No.2010IK186)
摘    要:建立了高效液相色谱-电喷雾串联质谱联用测定水产品中19种喹诺酮类兽药残留的方法。采用酸化乙腈溶液进行提取,用固相填料进行分散固相萃取净化。以甲醇和0.1%甲酸溶液作为流动相,C18作为分析色谱柱,采用梯度洗脱方式进行液相色谱分离,选择离子反应监测模式检测19种喹诺酮类药物,内标方法定量。在2.0~100.0μg/L范围内,19种喹诺酮类药物的线性相关系数均大于0.99。通过添加回收试验,方法的定量限(S/N=10)为1.0μg/kg,3个添加水平中,小龙虾的回收率为70.5%~112.6%,相对标准偏差为3.5%~8.9%,鮰鱼的回收率为70.2%~113.8%,相对标准偏差为4.5%~8.9%。

关 键 词:分散固相萃取  高效液相色谱/串联质谱法  水产品  喹诺酮类兽药
收稿时间:2011/3/18 0:00:00
修稿时间:6/7/2011 12:00:00 AM

Simultaneous determination of 19 quinolones residues in aquatic product Using DSPE and high performance liquid chromatography-tandem mass spectrometry
cao jun.Simultaneous determination of 19 quinolones residues in aquatic product Using DSPE and high performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Veterinary Drug,2011,45(7):21-25.
Authors:cao jun
Institution:YanCheng Entry-Exit Inspection and Quarantine Bureau
Abstract:A method for the simultaneous analysis of 19 quinolones residues in aquatic product was developed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The treated samples were extracted using buffered acetonitrile and cleaned up using Dispersive SPE(DSPE).The HPLC separation was performed on a C18 column with a linear gradient elution program of methanol and 0.1% formic acid solution as the mobile phase.Selective reaction monitoring(SRM) was used for the selective detection of 19 q...
Keywords:Dispersive-Solid Phase Extraction (DSPE)  HPLC-MS/MS  aquatic product  quinolones
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