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超高效液相色谱-串联质谱法测定原料乳中苯并咪唑类药物
引用本文:方忠意.超高效液相色谱-串联质谱法测定原料乳中苯并咪唑类药物[J].中国兽药杂志,2009,43(5):17-20.
作者姓名:方忠意
作者单位:河南省兽药监察所,郑州,450008
摘    要:建立了超高效液相色谱—串联四级杆质谱法测定原料奶中苯并咪唑类药物残留量的检测方法。原料奶经乙酸乙酯提取,MCX固相萃取柱净化,用UPLC-MS/MS进行检测。色谱条件为:色谱柱为ACQUITYUPLCTMBEHC18柱(2.1 mm×100 mm,1.7μm);流动相为:乙腈-0.1%甲酸水溶液,梯度洗脱,流速为0.3 mL/min。采用ESI正离子模式,多反应监测(MRM)模式检测,外标法定量。本方法检测测苯并咪唑类药物残留的检测限为0.5μg/kg,定量限为1.0μg/kg。

关 键 词:苯并咪唑类药物  超高效液相色谱—串联四级杆质谱  原料奶
收稿时间:2/1/2009 12:00:00 AM
修稿时间:2009/3/23 0:00:00

Determination of benzimidazoles residue in raw milk using ultra performance liquid chromatography-tandem mass spectrometry
fang zhongyi.Determination of benzimidazoles residue in raw milk using ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Veterinary Drug,2009,43(5):17-20.
Authors:fang zhongyi
Institution:Henan provincial supervising agency of veterinary Drugs
Abstract:A method for determination of benzimidazoles residue in raw milk was developed using ultra performance liquid chromatography - tandem mass spectrometry ( UPLC - MS/MS). Ethyl acetate was used to extract the target analyte from raw milk, extraction was degreased and cleaned up with Waters Oasis MCX solid phase extraction (SPE) column for UPLC - MS/MS. The liquid chromatography separation was carried on Cls column (2.1 mm × 100 mm i. d. ,1.7 μm) with acetonitrile and water(added 0.1% formic acid) as mobile phase at a flow rate of 0.3mL/min. The mass spectrometry was performed in multiple reaction monitoring(MRM) mode. The limits of detection (LOD) of the method were 0.5 μg/kg and the limits of quantification (LOQ) were 1.0μg/kg. The method has good repeatability and high sensitivity , and can be applied for the determination of benzimidazoles in raw milk.
Keywords:benzimidazoles  ultra performance liquid chromatography-tandem mass spectrometry  raw milk
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