分散固相萃取结合液相色谱串联质谱法检测牛可食性组织中吡喹酮残留量
目的 建立分散固相萃取结合液相色谱串联质谱法检测牛肉、牛脂肪、牛肝和牛肾等可食性组织中的吡喹酮残留量的分析方法。方法 取牛组织样品经50%(V:V)乙腈溶液提取, 加入无水硫酸镁和氯化钠进行脱水和盐析, 正己烷脱脂, 高速离心分层后, 取适量乙腈层溶液经0.1%(V:V)甲酸稀释后, 用酸性氧化铝粉末进行样品净化并以10000 r/min离心取上清液, 过0.22 μm滤膜后上机测定。使用反相色谱柱进行分离, 流动相为0.1%甲酸和乙腈溶液, 采用梯度程序进行洗脱, 三重四极杆质谱进行定性定量分析。结果 吡喹酮在2.5~500 μg/kg范围内线性关系良好(r>0.995), 方法的最低检出限为1 μg/kg, 最低定量限为2.5 μg/kg, 添加回收率在60%~110%, 相对标准偏差(relative standard deviation, RSD)＜10%。结论 该方法具有较好的准确度与精密度, 适用于牛可食性组织中吡喹酮残留量的测定。
Objective To establish a method for determination of praziquantel residues in edible bovine tissues such as muscle, fat, liver and kidney by dispersive solid phase extraction combined with liquid chromatography tandem mass spectrometry. Methods Bovine tissue samples were extracted with 50% (V:V) acetonitrile solution, and dehydrated and salted out with anhydrous magnesium sulfate and sodium chloride, and degreased by n-hexane. After high speed centrifugation, the extract was diluted by the 0.1% (V:V) formic acid and purified by the acid alumina powder. After 10000 r/min centrifugation, the extract was filtered by 0.22 μm film and then detected. The targets was separated by the gradient elution with a reverse phase column as the stationary phase and 0.1% formic acid with acetonitrile as the mobile phase. Triple quadrupole mass spectrometry was used for qualitative and quantitative analysis. Results Praziquantel had good linear relationships in the range of 2.5-500 μg/kg, and the correlation coefficients were all above 0.995. The limit of detection of the method was 1 μg/kg and the minimum limit of quantitative was 2.5 μg/kg. The recovery were between 60% and 110%, with the relative standard deviation (RSD) were lower than 10%. Conclusion This method has good accuracy and precision, which is suitable for the determination of praziquantel residues in edible bovine tissues.
标题：分散固相萃取结合液相色谱串联质谱法检测牛可食性组织中吡喹酮残留量
英文标题：Determination of praziquantel in edible bovine tissues by dispersive solid phase extraction combined with liquid chromatography-tandem mass spectrometry
作者：
吴剑平 上海市兽药饲料检测所
张婧 上海市兽药饲料检测所
贡松松 上海市兽药饲料检测所
严凤 上海市兽药饲料检测所
潘娟 上海市兽药饲料检测所
黄士新 上海市兽药饲料检测所
中文关键词:吡喹酮,分散固相萃取,液相色谱串联质谱法,
英文关键词:praziquantel,dispersive solid phase extraction,liquid chromatography tandem mass spectrometry,
发表日期：2019-01-15
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